GIFT OF TU Craif Western Sar METHODS OF ANALYSIS AND LABORATORY CONTROL OF THE GREAT WESTERN SUGAR COMPANY BY THE CHEMICAL DEPARTMENT OF THE GREAT WESTERN SUGAR COMPANY FIRST EDITION DENVER THE GREAT WESTERN SUGAR COMPANY 1920 * . . . - COPYRIGHT, 1920 BY HE GREAT WESTERN SUGAR COMPANY PRINTED BY PREFACE This book is an outgrowth of a 20-page pamphlet, "Methods of Analysis for Beet Sugar Factories," published in 1903, and reissued in revised form in 1908. With the development of a highly specialized system of chemical control, the need for a more up to date and comprehensive treatise has been increasingly felt. The present book has accordingly been prepared as a handbook and reference book for the laboratories of the Great Western Sugar Company. It has seemed desirable to include not only directions for the process control, but also methods for the analysis of raw materials and for such other analyses as the chemist in our organization is commonly called on to make. This has resulted in the expansion of the book to a considerable size, but at the same time an effort has been made to employ a certain conciseness of treatment and style. Hence very little explanation is ordinarily given of the reasons for various steps or procedures, except where the reason is likely to be obscure or where it is desired to emphasize the im- portance of the matter in the reader's mind. It is expected that the chemist will be able readily to figure out such things for him- self, and to profit if any mental exercise is involved. For the sake of keeping the book within reasonable bounds, directions for purely numerical or statistical calculations have also, with a few excep- tions, been purposely omitted. A great number of chemists of this company, past and pres- ent, too numerous to mention, are responsible for the development of our methods of analysis and laboratory control to their present status. The writer's thanks are due in particular to Mr. P. Roller for assistance in preparing a considerable portion of the manu- script and for having read over the text in its entirety. The following books have been consulted and found especially helpful: Browne's "Handbook of Sugar Analysis," Hillebrand's iii 468640 iv PREFACE "The Analysis of Silicate and Carbonate Rocks" (Bulletin 700 of the U. S. Geological Survey), Scott's "Standard Methods of Chemi- cal Analysis," the "Methods of Analysis" of the Association of Official Agricultural Chemists, and Circular 44, " Polarimetry, " and numerous other publications of the Bureau of Standards. For the methods for the analysis of diatomaceous earth we are indebted to Messrs. S. C. Meredith and P. B. Caster, of the Western Sugar Refining Company. The writer will especially welcome criticisms from any source which will assist him in correcting errors or making improvements in a future edition. S. J. OSBORN General Chemist, The Great Western Sugar Company. Denver, Colorado, July 29, 1920. CONTENTS Chapter Page I. GENERAL METHODS 1 II. REGULAR FACTORY CONTROL 16 III. SULPHATE CONTROL 42 IV. STEFFEN PROCESS CONTROL 47 V. PULP DRYER CONTROL 62 VI. PULP SILO CONTROL 69 1 VII. BOILER HOUSE CONTROL 72 VIII. POTASH CONTROL (BEET CAMPAIGN) 80 IX. POTASH CONTROL (POTASH CAMPAIGN) 82( X. CRUDE POTASH 90 XI. MOLASSES 100 XII. BEET LABORATORY TESTS 102 XIII. ASH ANALYSIS OF SUGAR FACTORY PRODUCTS 107 XIV. SCALES AND DEPOSITS 115 XV. COAL AND COKE 126) XVI. LIMESTONE 133 XVII. WATER 139 XVIII. DIATOMACEOUS EARTH (KIESELGUHR) 147 XIX. SULPHUR : 149 XX. FOODS AND FEEDING STUFFS 151 XXI. COTTON SEED CAKE 157 XXII. SOIL 160 XXIII. APPARATUS 168 XXIV. STANDARDIZATION AND VERIFICATION OF APPARATUS . 179 XXV. REAGENTS 188 XXVI. MISCELLANEOUS ...198 VI CONTENTS Chapter Page XXVII. TABLES 1. Brix, Baume, and Specific Gravity of Sugar Solutions. .201 2. Factors for Calculation of Apparent Purity 214 3. Temperature Corrections for Brix Hydrometers Stand- ard Temperature 20 C 215 3-A. Temperature Corrections for Brix Hydrometers Stand- ard Temperature 20 C. (Condensed Table) 216 4. Temperature Corrections for the Abbe Sugar Refrac- tometer Standard Temperature 20 C 216 5. Approximate Amounts of Basic Lead Acetate Solution (55 Brix) for Various Products 217 6. Polarization Table 200 mm Tube, 1/10 Dilution. (For Pulp and Pulp Water) 218 7. Polarization Table 400 mm Tube, 1/10 Dilution. (For Sewer Water) 218 8. Polarization Table 400 mm Tube, Read Direct. (For Condensed Waters) 219 9. Steffen Polarization Table 220 10. Invert Sugar in Thick Juices, Syrups, and Solid Products 221 11. Invert Sugar in Thin Juices 223 12. Cupric Oxide Table for Obtaining the Percentage of Invert Sugar (10 grams of material) 223 13. Cupric Oxide Table for Obtaining the Percentage of Invert Sugar (5 grams of material) 223 14. CaO by Soap Solution in Thin Juices 224 15. CaO by Soap Solution in Thick Juices, Massecuite, Molasses, etc 226 16. Table for Use in Dry Substance Determinations on Pulp Sold 228 17. B. T. U. Lost in Dry Flue Gas per pound of Coal Con- taining 57% Carbon 229 18. "Moisture Factor" for Computing Loss of Heat in Flue Gas due to Moisture 241 18-A. "Temperature Factor" for Computing Loss of Heat in Flue Gas due to Moisture 242 19. CaO in Milk of Lime of Various Densities 243 20. Equivalents of Normal Solutions 244 21. Percentage of Available Granulated on Dry Substance of Sugar Solutions Molasses Purity of 60 245 22. Percentage of Available Granulated on Total Sugar of Sugar Solutions Molasses Purity of 60 246 23. Standard Beet Extraction 247 24. Standard Steffen Extraction 251 25. Specific Gravity of Various Materials 251 26. International Atomic Weights, 1920 252 INDEX . 253 I. GENERAL METHODS 1. DEGREES BRIX The Brix scale represents the percentage of sugar in a pure sugar solution. The reading of a Brix hydrometer in a solution at the standard temperature (20 C.) is known as the "degrees Brix," or simply the "Brix," which is employed as an approximate meas- ure of the percentage of dry substance. (a) DIRECT METHOD Determine the density of all solutions up to 75 Brix as fol- lows: Transfer the solution to a suitable glass cylinder (hydro- meter jar), and, if necessary, immerse in a cooling bath to reduce the temperature to approximately 20. If air bubbles are present, remove them by the action of a vacuum. Mix the solution in the cylinder to equalize the temperature and immerse a clean, dry hydrometer about one-quarter of an inch below the point where it floats naturally and then allow it to assume its normal position. Read the scale by bringing the eye upon a level with the surface of the solution so that the latter appears as a straight line and not an ellipse, and note where the border line forming the bottom of the meniscus intersects the scale. Dark or opaque solutions may have to be read from above, by estimating the distance of the level of the solution below the top of the meniscus. When the reading is taken, the liquid and hydrometer must be free from air bubbles and at rest, and the hydrometer must not be in contact witli the bottom or walls of the cylinder. Take the temperature of the solution with a thermometer; if it is not exactly 20, apply the correction indicated in Table 3 or 3-A. Hydrometer readings should not be made below 15 or above 25. To insure strict accuracy, the cylinder should be filled so full that the insertion of the hydrometer causes the liquid to overflow. 2 METHODS OP ANALYSIS This minimizes the effect on the reading of the formation of sur- face films of impurities. (b) DOUBLE DILUTION METHOD In the case of molasses, massecuite, etc., weigh out 400 grams in a copper beaker, add about 350 grams of hot water, and stir with a glass rod until completely dissolved. Cool to approximately 20, remove and rinse the rod, make up to 800 grams with water, and mix well. Pour into a glass cylinder, rinsing it first with a little of the solution if the cylinder is wet, and obtain the Brix reading as under (a). Apply the temperature correction, if neces- sary, and then multiply by 2. Other weights may be used if the final dilution is in the same ratio. See under "4. Apparent Purity Determination" regarding the quality of the water used for dilution. 2. DRY SUBSTANCE AND MOISTURE Special directions for particular products will be found under "Sugar," "Dried Pulp," etc. Where this determination is im- portant in itself, other than as an incidental figure for obtaining the true purity, etc., it should not be made on material which has been placed under vacuum for any great length of time, because a considerable increase in concentration sometimes occurs under this condition. (a) BY OVEN DRYING ( 1 ) Apparatus : A double-walled drying oven containing a glycerin solution in the jacket, of such a strength that a tempera- ture of 100-105 is maintained in the interior of the oven. The boiling point is kept constant by means of a reflux condenser. See Chap. XXIII, 7. Aluminum dishes 2 in. diameter by 11/2 i n - high, as described in Chap. XXIII, 6, provided in each case with an aluminum cover and a glass rod of such a length that it will not interfere with the proper position of the cover. A desiccator containing sulphuric acid as the dehydrating agent. The acid should be renewed as soon as it shows any sign of discoloration or loss of absorptive power. Renew the acid at least once a week when the desiccator is in constant use. (2) Reagents: Sea sand prepared as described in Chap. XXV, 17. I. GENERAL METHODS 3 (3) Method: Place 25-30 grams of sea sand in an aluminum dish and dry it, together with the cover and glass rod, in an oven at 100-105 C. for at least one hour. Remove from the oven, put on the cover, and cool in a desiccator. Weigh out, in 'the covered aluminum dish, an amount of the material under examination which is equivalent to approximately one gram of dry substance. Warm the dish on top of the drying oven, remove the cover, and mix the contents well. Warm again, add 1 ml of *hot water and stir until a perfectly homogeneous mixture is obtained. Dry at 100-105 C. for 5-6 hours, replace the cover, cool in the desiccator, and weigh. Repeat the drying for one hour periods until the loss in weight in any period is less than 0.1%. Keep the thermometers in the desiccator and balance case, and do not make the weighings until the difference in tem- perature is 2 degrees or less. Make all determinations in duplicate. The duplicates should ordinarily check within 0.1% ; if they differ by more than 0.2% repeat the determination. Sugar, dried pulp, and filter press cakes are dried directly without the use of sand. (b) BY REFRACTOMETER The Abbe sugar refractometer uses the refractive index as a measure of the percentage of dry substance, and in the case of or- dinary sugar factory products gives results which are close to those found by oven drying. Use the original material in the case of juices, syrups, and molasses, and " double diluted" material in the case of sugar and massecuite. Place 1 or 2 drops on one of the prisms, close quickly, mid circulate water at 20 through the instrument. Read directly from the scale the percentage of dry substance. Multiply the reading by two if "double diluted" material has been used. If the reading is not made at exactly 20, apply the correction indi- cated in Table 4. Check the zero point of the instrument frequently with distilled water. See also Chap. XXIII, 16 and XXIV, 8. 3. SUGAR The polarization (direct polarization) is defined as the per- centage of sugar indicated by the polariscope. *Thin solutions do not require the addition of water. 4 METHODS OF ANALYSIS In the absence of other optically active bodies the polarization represents the true percentage of sugar. In the presence of an- other optically active substance, such as raffinose, the method of double polarization (before and after inversion) is used to. deter- mine the two sugars accurately. The percentage of sugar obtained in this manner is known as the " sugar by inversion." (a) SUGAR BY DIRECT POLARIZATION Weigh out 26 grams (or a *fraction or multiple thereof, de- pending on the nature of the material) in a counterpoised nickel dish, and dissolve in a small amount of water. Use hot water if difficult to dissolve. Rinse into a 100 ml flask and add sufficient basic lead acetate solution to decolorize, avoiding any great excess. (See Table 5.) Where the amount of the lead precipitate is small, as in the case of products of high purity, the addition of a few drops of alumina cream will aid in securing a clear filtrate. Cool to approximately 20 if necessary, and make up to the mark with water, using one or two drops of ether, if necessary, to break the foam. Shake well and filter, rejecting the first portion of the fil- trate and returning the remainder to the filter until it is perfectly clear. Polarize in a 200 mm tube, first rinsing the tube two or three times with the solution. If the normal weight, 100 ml flask, and 200 mm tube have been used, the reading gives directly the percentage of sugar. If the weight, volume, or length of tube differs from these standards, calculate the percentage of sugar proportionally. When great accuracy is required, make up to the mark with water at exactly 20 and polarize in a jacketed tube at the same temperature. For ordinary work it is sufficiently accurate to ap- proximate the above temperature conditions. See also Chap. XXIII, 13, regarding the use of the polariscope. (b) SUGAR BY INVERSION (1) Polarize as above. (2) Weigh out 13 grams of the original material (or 26 grams of the double diluted solution) in a counterpoised nickel dish, dissolve in a small amount of water, and rinse into a thin walled 100 ml Kohlrausch flask, marked at the point at which it holds 75 ml. Add from a pipette 10 ml of hydrochloric acid *In the case of molasses use 13 grams of the original molasses, or 26 grams of the "double diluted" solution. In the case of other products of higher purity use ordinarily 26 gram? of the original material, or 52 grams ot the "double diluted" splution, I. GENERAL METHODS 5 C)f\O (D -^-1.029^see Chap. XXV, 10), make up immediately to the 75 ml mark with water, and mix thoroughly. Place a thermometer in the flask, and immerse in a water bath at 70 with frequent agitation. The solution should reach a temperature of 67 in not more than five minutes, and preferably in 2 3 minutes. When the temperature reaches 67, note the time, and maintain the temperature for exactly five minutes between 67 and 70. Shake the flask occasionally with a rotary motion in order that the tem- perature may be uniform throughout the solution. Then place the riask immediately in a cold water bath and cool as rapidly as pos sible to 20. Remove the thermometer, rinsing the adhering liquid into the flask, and make up to the 100 ml mark with water at ex- actly 20. Next add 2-4 grams of zinc dust, according to the amount of decolorization required, and allow to stand for half an hour, shaking at frequent intervals. Filter and polarize at exactly 20 in a 200 mm jacketed tube. In making the polarization, place the tube in the trough of the polariscope and insert a thermometer graduated in one-tenths of one degree, allowing the bulb to rest against the bottom of the inner tube. Circulate the cooling water at 20 (or at 19-20, but never below 19) until the thermometer indicates that the 20 point has been reached, then remove the thermometer and take a sufficient number of readings with as little delay as possible. If the solution is cooled in this manner, the temperature will not change appreciably during the time that the readings are made. Do not handle the tube during the final adjustment of the tem- perature. All the conditions prescribed must be rigidly followed to ob- tain accurate results. The total volume during inversion must be approximately 75 ml; the hydrochloric acid must be measured accurately and be of the proper strength ; the conditions regarding the temperature and time of heating must be observed; and the solution in the polariscope tube must be cooled in the manner de- scribed in order that the reading may be made at exactly 20 and that this temperature may prevail uniformly throughout the solution. Means should be provided for a sufficient supply of cool- ing water at constant temperature. ^Fultiply the reading by 2, since the half -normal weight has been used. *Mix constantly until the solution has attained a temperature of 67. D METHODS OP ANALYSIS (c) FORMULAS ^(1) Raffinose Formula (For the determination, of sugar in the presence of raffinose) : This formula is generally used in beet sugar work. Let P = direct polarization J = polarization after inversion (expressed as a posi- tive number) S = % sugar by inversion R = raffinose .839 AndR = .54X (P -S) (2) Clerget Formula (For the determination of sugar in the presence of invert sugar) : This formula is not commonly used in beet sugar work, but is given here for the sake of completeness : Let T = temperature at which polarization is made ThcnS 142.66 .5 T Or, if T = 20 100 (P + J) 132.66 4. APPARENT PURITY (a) DEFINITION The "purity" (coefficient of purity) of a juice, syrup, etc., is the percentage of sugar in the total solid matter, and is calcu- lated by multiplying the percentage of sugar by 100 and dividing by the percentage of solids. If the direct polarization is used to represent the percentage of sugar and the degrees Brix to repre- sent the percentage of solids, the result is known as the ' ' apparent ' ' purity. If the ' ' sugar by inversion ' ' is used for the percentage of sugar and the actual dry substance for the percentage of solids, the figure is known as the ' ' true ' ' purity. (b) DETERMINATION If too thick, dilute the material with water to approximately 23 Brix as follows : Put a suitable amount of hot water in a copper can or sample bucket, and add a suitable amount of the juice or syrup; the proportions to be used should be such as will yield a solution of the required density and will be learned by experience. I. GENERAL, METHODS 7 Stir vigorously until completely dissolved and then pour the solu- tion into a cylinder (hydrometer jar). The solution prepared in this manner should have a density of not less than 21 nor more than 24 Brix. If, after cooling as described below, the density is found to be a little too high, add the necessary small amount of cold water, and mix thoroughly by inverting the cylinder at least half a dozen times; only under this condition is it permissible to make any dilutions in cylinders or with the use of cold water, and care should be taken then that a thorough mixture is obtained. " Double diluted" solutions, if available, may be used in place of the original material, but the dilution should be made by mixing with hot water as described above and not in a cylinder. It may be preferable, however, in order to save time, to prepare a sep- arate solution for the apparent purity determination from the original material. Cool in the cylinder under vacuum to remove air bubbles, and obtain the Brix reading as described in section 1, "Degrees Brix," making correction for temperature if necessary. Measure out 100 ml in a 100-110 nil flask, rinsing the latter first with a small portion .. Qse only neutral water for all dilutions. 12 METHODS OF ANALYSTS (a) JUICES Transfer 10 ml with a pipette to a porcelain dish, dilute with neutral water if dark, add a few drops of indicator solution, and add the standard acid until the pink color entirely disappears ; test for the end point by adding a drop of the indicator. If the solution is acid, add an excess of N/28 sodium hydroxide solution, and titrate back to neutrality with the standard acid ; subtract from the number of ml of alkali added the number of ml of acid required. In the case of highly colored products where it is diffi- cult to observe the end reaction, transfer 10 ml to a test tube or a tumbler and dilute with about 50-100 ml of water: fill a second vessel in the same manner. Add phenolphthalein to one and titrate with the standard acid until a color match for the two solutions is obtained. Express the result as "grams of CaO p?r 100 ml," by divulin.^ the number of ml of acid required by 100. Express acidity as negative alkalinity on the same basis. ( b ) MASSECUITE Use 10 ml of the double diluted solution prepared for the Brix determination, titrate as in (a), and multiply the result by 2. (c) STEFFEN LIQUORS Measure out 50 ml with a pipette, add a few drops of indicator, and titrate to neutrality with the standard nitric acid ( 1 ml = .05 g CaO). Express the result as "grams of CaO p?r 100 ml" by dividing the number of ml of acid required by 10. 11. CaO BY TITRATION Use standard nitric acid and sodium hydroxide (1 ml = .0") g CaO), and phenolphthalein indicator. Dilute the weighed sample with 50-100 ml of neutral water in a porcelain casserole, add an excess of the standard acid, and boil for 3-5 minutes to expel all carbon dioxide. (The amount of dilu- tion and time of boiling must be maintained within the p^e^ribod limits in order to drive off all carbon dioxide produced from the decomposition of carbonates and at the same time not to volatilize any nitric acid.) Add a few drops of indicator and titrate to neutrality with the standard alkali. I. GENERAL METHODS 13 If 5 grams of the sample is used for the determination, the number of ml of acid used, less the number of ml of alkali required, gives directly the percentage of calcium oxide. 12. CaO BY SOAP SOLUTION Use a soap solution prepared and standardized as described in Chap. XXV, 21, and adjusted to a strength of 1 ml = .001 g CaO (twenty-eighth normal). (a) DETERMINATION IN THICK JUICE, SYRUPS, MASSECUITE, ETC Use a portion of the 23 Brix solution prepared for the ap- parent purity determination. Transfer 10 ml with a pipette to an 8 oz. glass bottle provided with a ground stopper and marked at the point at which it holds 50 ml. Fill to this mark with water and add a drop of phenolphthalein solution. If the reaction is not alkaline, add N/28 sodium hydroxide a drop at a time until a permanent pink color is produced. Then add the soap solution in small quantities from a burette; after each addition stopper the bottle and shake vigorously. Take as the end point the formation of a fine foam 5 mm in depth which will last five minutes. Make a blank test on each lot of water prepared for dilution, first adding phenolphthalein and then N/28 sodium hydroxide a drop at a time until a permanent pink color is produced. Subtract from the num- ber of ml of soap solution used in the determination the number of ml of soap solution required by 40 ml of the water in the blank test. Obtain the "CaO to 100 Brix" from Table 15. The quality of water used for dilution should be the best available, in order that the correction may be kept as small as possible. The recognition of the end point is a matter of experience. Usually a granular or curdy precipitate is formed at the beginning of the addi- tion of the soap solution; when the amount of this is large, it collects on the surface and may be mistaken for the final foam. As the end point is approached, the precipitate breaks up and yields a uniformly opaque solution. Practice will enable the end point to be recognized immediately by the fact that, as long as the bubbles show any marked sign of break- ing, the amount of soap solution is insufficient. (b) DETERMINATION IN THIN JUICES Determine as in (a), using 20 instead of 10 ml of juice. Cor- rect for the number of ml of soap solution required by 30 ml of the water in the blank test. Obtain the "CaO to 100 Brix" from Table 14. 14 METHODS OF ANALYSIS 13. DETECTION OF SUGAR BY MEANS OF ALPHA- NAPHTHOL Employ the following method for the detection of sugar in condensed waters. Use 6x% inch test tubes graduated at % inch and I 1 /*? inches from the bottom. Fill the tube to the upper mark with the water under examination, add 5-10 drops of alpha-naphthol solution, and mix thoroughly. Cool if the water is hot, then add concentrated sulphuric acid (a 250 ml dispensing burette is convenient), hold- ing the tube in an inclined position so that the acid will run lo the bottom and form a separate layer, and continuing the addition until the acid layer reaches the % inch mark. If a lilac or purple ring appears at the intersection of the two layers during the addition of the acid or immediately thereafter, polarize the water as follows : Cool if the water is hot, filter if necessary, and read directly in a 400 mm tube without the addition of lead acetate. To obtain the percentage of sugar multiply the reading by .13, or use Table 8. If the polariscope reading is less than .2, record as a "heavy trace," which should represent a con- centration of at least 1 part of sugar in 10,000 parts of water. If the color does not appear immediately upon the addition of the acid, roll the test tube once in an upright position between the palms of the hands. If no purple or lilac ring appears within 15 seconds, report sugar as absent. If the characteristic color ap- pears within this time, report as a ' 'light trace, ' ' which should sig- nify that the water contains from 1 part of sugar in 10,000 to 1 part in 100,000. Previous to the campaign and frequently during the campaign, test the stock of alpha-naphthol with freshly prepared sugar solu- tions of known concentration, as follows : Per Cent Sugar Concentration 1.0 1 :100 .1 1 :1000 .01 1 rlOOOO .001 1 :100000 The conditions of the test may be modified accordingly, if necessary. Any alpha-naphthol, however, which is not sufficiently sensitive to give a reaction in a 1 : 100,000 sugar solution after 15 seconds standing should Joe discarded or repurified. Chemists I. GENERAL METHODS 15 should familiarize themselves with the shade of color produced by each of the above standard sugar solutions. The following resume will be found convenient for reference: Approximate Designation Abbreviation Percentage of Sugar Indicated Zero Less than .001% Light Trace L .001 to .010% Heavy Trace H .010 to .026% A figure The percent-age indicated. II. REGULAR FACTORY CONTROL 1. COSSETTES Determine : (a) Sugar every hour. (b) Apparent Purity, every 2 hours. (c) Lixiviated Ash, every 24 hours. SAMPLING Fill a 2-gallon pail by holding it in the stream of cossettes as they fall from the conveyor, or from the slicers. Pay particular attention to securing a sample free from contamination with steam or water. See also below under * ' Tailings. ' ' As a check upon the cossette test, an extra sample should be taken every 2 hours in the same manner as the regular sample, but at a different time, preferably half an hour before or after the time of a regular sample. The sugar should be determined by a different operator from the one who handles the regular samples. PREPARATION OF SAMPLE Grind the entire sample without delay in an Enterprise Meat Chopper No. 41 fitted with a plate containing one-eighth inch per- forations and running at the rate of 300 revolutions per minute. When all the sample has been introduced, return a handful of the ground material to the machine and allow the machine to run until no more material or juice is forced through the perforated plate. Do not add to the sample the small portion of the material remain- ing in the machine. Mix the ground sample thoroughly with the hands, take out a small portion for analysis, and place it in a covered bucket. Use the remainder of the ground sample for the purity determination. After the sample has been ground, open II. REGULAR FACTORY CONTROL 17 the machine and wash it out well with hot water. Be sure that it is dry before it is used again. Use this machine only for grinding cossettes. Obtain the juice for the purity determination as follows : Place a suitable amount of the ground sample in a clean, dry cloth and subject it to a pressure of 240 Ibs. per sq. in. in a hydraulic press. Measure the pressure with a suitable high pressure gage; the gage pressure to be carried depends on the dimensions of the basket and the ram, and is calculated as described in Chap. XXIII, 14. Bring up the pressure gradually and maintain the prescribed pressure until juice ceases to flow. Collect the entire amount of juice ex- pressed and mix it well. Use the press and the cloths exclusively for cossettes, wash them well with hot water after use, and see that they are dry before they are used again. A small drying closet, heated by steam pipes, should be employed for drying cos- sette and pulp cloths. ANALYSIS (a) Sugar: Weigh out 26 grams of the ground cossettes as rapidly as possible, and rinse with a jet of water into a 200.6 ml Kohlrausch flask. Add 6 ml of basic lead acetate solution and sufficient water to make a volume of about 160-170 ml. Digest in a water bath at 80, keeping the body of the flask entirely im- mersed but not in contact with the bottom of the bath. Remove the flask from time to time and mix with a rotary motion. At the end of exactly 30 minutes fill to the mark, or slightly above it, with water at 80 and continue the digestion for exactly 10 minutes longer. Then cool to approximately 20 in a cold water bath and make up to the mark with the necessary small amount of water. Use a few drops of ether to break the foam, adding it either just previous to the second period of digestion or after the solu- tion has been cooled. Shake, filter, and polarize in a 400 mm tube. The reading gives directly the percentage of sugar. In the case of beets of abnormally low purity, 8-10 ml of basic lead acetate solution may be needed for clarification. (b) Apparent Purity: Place the juice in a cylinder under vacuum until all air has been removed and determine as described in the "General Methods," 4 (b). Use a stronger lead solution for clarification, if necessary, and, if this is insufficient, proceed as follows : Transfer 50 ml with a pipette to a 100-110 ml flask, add sufficient basic lead acetate for clarification, and make up to the 18 METHODS OP ANALYSIS 110 ml mark with water. Multiply the polariscope reading by 2 before applying the formula or the table. The use of the last mentioned method should very seldom be necessary, and then only in the case of beets of abnormally low purity. (c) Lixiviated Ash: Weigh out 5-10 grams in a platinum dish from the sample of ground cossettes used for one of the hourly sugar determinations on which the apparent purity is also determined. Follow the "General Methods," 7 (b). TAILINGS If beet tailings are introduced and pass through the automatic scales with the beets, no particular attention need be paid to them, as the cossette samples will, in the long run, include a proportional amount of the tailings. If tailings are introduced which do not pass through the auto- matic scales, they may be handled by one of the following methods : (1) If the tailings are mixed with the cossettes at a reason- ably uniform rate, take the cossette samples as above, so that they will include a proportional amount of the tail- ings. Add the weight of tailings introduced to the weight of beets which passes through the scales. (2) Take the cossette samples at a point where none of the tailings will be included in the sample ; sample the tail- ings also once a shift, grind, and determine the percent- age of sugar as in the case of "Cossettes." Add the "equivalent in beets" of the weight of tailings to the weight of beets which passes through the scales. In either of the preceding two cases determine the amount of tail- ings introduced by actual weighing for a 24 hour period at least once a week. 2. DIFFUSION JUICE Determine every 2 hours : (a) Brix. (b) Apparent Purity. Determine every 24 hours: (c) Lixiviated Ash. II. REGULAR FACTORY CONTROL 19 SAMPLING Take a catch sample from a full measuring tank, or from the pipe line or pump before the juice enters the heaters. ANALYSIS (a) Brix: Follow the " General Methods," I (a). (b) Apparent Purity: Determine as in (b) under "Cos- settes." (c) Lixiviated Ash: Weigh out 7-10 grams of one of the catch samples and proceed as in the " General Methods," 7 (b). SPECIAL DETERMINATIONS (d) Acidity: Measure out 10 ml in a porcelain dish, add two or three times its volume of neutral water to lighten the color, and a few drops of phenolphthalein. Add an excess of standard sodium hydroxide (1 ml = .001 g CaO), then titrate to neutrality with standard sulphuric acid of the same strength. Express the result in grams of CaO per 100 ml. See "General Methods," 10 (a). (e) Invert Sugar: Use one of the samples on which the pre- vious determinations have been made, but do not allow it to stand for any length of time before starting this determination. Follow the "General Methods," 6 (b). 3. PULP AND PULP WATER Determine hourly in a sample from each diffusion battery: (a) Sugar. SAMPLING The workman under the battery should take from each cell dumped a small portion of the mixture of pulp and pulp water, using a long handled dipper. The sample should be taken from the first pulp and water discharged. The individual sample should be transferred at the time to a covered container of the customary type, so arranged that the water will drain into the bottom of the receptacle and not stand in contact with the pulp. PREPARATION OP SAMPLE Grind the entire sample of pulp in an Enterprise Meat Chop- per No. 41 in the same manner as described under "1. Cossettes," 20 METHODS OF ANALYSIS and press in a clean, dry cloth in a suitable hand press. Collect the entire amount of juice that can be expressed and mix it well. Keep the grinding machine, press, and cloths clean, and use them only for pulp. ANALYSIS (a) Sugar: Measure out 100 ml of the expressed juice in a 100-110 ml flask, add 2-4 ml of basic lead acetate solution, fill to the 110 ml mark with water, shake, filter, and polarize in a 200 mm tube. Obtain the percentage of sugar from Table 6. Analyze the pulp water in the same way, using 1-2 ml of lead acetate. 4. FLUME PULP AND PULP WATER Determine every 2 hours: (a) Sugar. SAMPLING The sample should be taken by a laboratory employe and should be as nearly representative as possible of the pulp leaving the battery at the time. Obtain the sample from the discharge of the pit, from the flume leading to the pump, or from the return line of the pump, using a long handled dipper. Take the sample while a good sized stream of pulp is flowing in order to avoid excessive admixture of washout water, transferring it to the same kind of container which is used for the regular pulp samples. PREPARATION OF SAMPLE Grind and prepare the sample in the same manner as the regular pulp sample. ANALYSIS (a) Sugar: Determine the sugar in the pulp and the water in the same manner as in the regular pulp and pulp water samples. 5. FIRST SATURATION JUICE Determine every hour on a catch sample : (a) Alkalinity. II. REGULAR FACTORY CONTROL 21 Determine every 4 hours on a composite sample : (b) Brix. (c) Apparent Purity. SAMPLING Take a catch sample every hour from the cocks or troughs of the first presses, avoiding any admixture of wash water. Make up the composite sample by mixing equal portions of the four hourly samples. Keep the container for the composite sample clean, and add a few drops of formaldehyde to prevent decom- position. ANALYSIS (a) Alkalinity: Follow the "General Methods," 10 (a). (b) Brix: Follow the "General Methods," 1 (a), using the original juice, and not the carbonated sample described in (c) below. (c) Apparent Purity: Heat to 80 in a water bath and car- bonate at this temperature to faint alkalinity with phenolphthalein. Then heat to at least 85, filter, cool, redetermine the Brix, and determine the apparent purity according to the "General Meth- ods," 4 (b). NOTE: When the melted sugar is added at the blow-ups or at a point beyond the second saturation, a composite sample of Second Saturation Juice may be used for the apparent purity determination without laboratory carbonation 6. SECOND AND THIRD SATURATION JUICE Determine every hour on a catch sample : (a) Alkalinity. Determine every 4 hours on a composite sample : (b) Brix. SAMPLING Take a catch sample every hour from the cocks or troughs of the respective filters, avoiding any admixture of wash water. Make up the composite sample by mixing equal portions of the four hourly samples. Keep the containers for the composite samples 22 METHODS OF ANALYSIS clean, and add a few drops of formaldehyde to prevent decom- position. ANALYSIS Follow the "General Methods," 10 (a) and 1 (a). 7. EVAPORATOR THIN JUICE Determine every 4 hours on a composite sample : (a) Brix. (b) Apparent Purity. (c) Lime Salts (CaO to 100 Brix). SAMPLING Take a catch sample every hour from the pump, or at a suit- able point in the pipe line between the thin juice filters and the first body of the evaporators. Make up the composite sample by mixing equal portions of the four hourly samples. Keep the con- tainer for the composite sample clean, and add a few drops of formaldehyde to prevent decomposition. ANALYSIS Follow the "General Methods," 1 (a), 4 (b), and 12 (b). Add 1-2 ml of alumina cream before making up to the mark, if trouble is encountered in obtaining a clear filtrate. 8. EVAPORATOR THICK JUICE. Determine every hour on a catch sample : (a) Alkalinity. Determine every 4 hours on a composite sample : (b) Brix. (c) Apparent Purity. (d) Lime Salts (CaO to 100 Brix). SAMPLING Take a sample every hour from the pump, or from the line between the evaporator outlet and the blow-up inlet. Do not take II. REGULAR FACTORY CONTROL 23 the sample from the last body of the evaporators, because the sample so drawn is not always representative of the juice leaving the evaporators. Make up the composite sample by mixing equal portions of the four hourly samples. ANALYSIS (a) AIM h) if it and (b) Brix: Follow the " General Meth- ods," 10 (a) and 1 (a). (c) Apparent Purity: Dilute to the approximate density of the evaporator thin juice and determine according to "General Methods," 4 (b). The dilution is prescribed in this case in order to eliminate the small variation in the purity test which would be caused if the thin and thick juice were analyzed at different densities. (d) Lime Salts (CaO to 100 Brix): Use 20 ml of the solu- tion diluted to thin juice density as in (c), and follow the "Gen- eral Methods" for the determination of CaO by Soap Solution in linn juices, 12 (b). 9. BLOW-UP THICK JUICE Determine every hour on a catch sample: (a) Alkalinity. Determine every 4 hours on a composite sample : (b) Lime Salts (CaO to 100 Brix). SAMPLING Take a catch sample every hour from the cocks or troughs of the thick juice filters. Make up the composite sample by mixing equal portions of the four hourly samples. ANALYSIS (a) All-nlnnfj,; Follow the "General Methods," 10 (a). (b) Lime Salts (CaO to 100 Brix) : Dilute to approximately 23 Brix, determine the Brix, and use 10 ml, following the "Gen- eral Methods," 12 (a). Or dilute to thin juice density, determine the Brix, and use 20 ml, following the "General Methods," 12 (b). 10. LIME KILN GAS Determine every 4 hours : (a) Carbon dioxide (C0 2 ). 24 METHODS OF ANALYSIS (b) Oxygen (0). (c) Carbon monoxide (CO). SAMPLING Obtain the gas by means of a pipe leading to the laboratory from a point in the main gas line between the gas washer and the carbonators. Provide the laboratory line with a vent leading out- side the building by means of which the line may be exhausted and kept filled with fresh gas. ANALYSIS Use an Orsat apparatus provided with three pipettes and a water jacketed burette. First make sure that the vent line has been open for several minutes, to insure a supply of fresh gas. Fill the Orsat burette with water by raising the leveling bottle, then put it into communication with the gas supply, lower the level- ing bottle below the zero point of the burette, and allow the gas to fill the burette. Then expel the gas sample and draw in another in the same manner, to rinse out connections, etc., or allow the gas to bubble for a few moments through the water in the leveling bottle; in the latter case be sure that no gas is left trapped in the rubber tube between the burette and the leveling bottle. Put the three-way cock into communication with the atmosphere, at the same time raising the leveling bottle until the level of the water in it is at the level of the zero point on the burette. When equilibrium has been reached, i. e., when the water in the burette has reached the zero mark while the water in the bottle is at the same level, the apparatus contains 100 ml of gas measured at atmospheric pressure; turn the three-way cock so that no gas can enter or leave the apparatus. Be careful never to allow the level of the water in the burette to fall while the three-way cock is open to the atmosphere, otherwise air will be drawn into the apparatus which will dilute the gas and render the analysis inac- curate. Raise the leveling bottle, open the stopcock of the first absorption pipette, and force the greater part of the gas into it, then lower the bottle and draw most of the gas back into the burette. Repeat this twice, the last time bringing the absorption liquid to the mark on the absorption pipette, then close the stop- cock. Bring the leveling bottle to the point where its water level corresponds to that of the burette, then read off the percentage of carbon dioxide. Repeat the absorption process until the vari- ation is not over 0.2%. II. REGULAR FACTORY CONTROL 25 Absorb the oxygen and carbon monoxide in a similar manner in the other two pipettes, obtaining the percentages by difference. Renew the solutions in the absorption pipettes every two weeks, or as often as is found to be necessary. See Chap. XXV, 14, regarding the preparation of the absorption solutions. 11. DIME TO SLACKER Determine every 24 hours: (a) CaO by Titration. SAMPLING Obtain a one-pint sample every 2 hours, from the pile of lime from which the slacker is being fed, by breaking off small pieces, approximately one inch cubes. In taking the sample reject such material as sand, coke, unburned limestone, etc., which will be eliminated in the form of discard from the slacker. Keep the samples sealed and in a dry place. PREPARATION OP SAMPLE Crush the twelve pints representing the average sample for the 24 hours to one-quarter inch size in a jaw crusher, mix and quarter, repeating the mixing and quartering until the sample is reduced to about one pint. Grind this sample to 60 mesh on a bucking board or in a disc pulverizer. Mix the 60 mesh material and fill a four ounce bottle by taking small portions from various parts of the sample. Seal this sample and take it to the laboratory. Handle the lime as rapidly as possible during the preparation of the sample to avoid absorption of moisture. ANALYSIS Determine the CaO by Titration, according to the "General Methods," Chap. I, 11. 12. MILK OF LIME Determine every hour : (a) Brix. (b) CaO (grams in 100 ml). 26 METHODS OP ANALYSIS SAMPLING Take a catch sample from the discharge line of the pump. ANALYSIS (a) Brix: Cool under vacuum, mix by inverting the cylin- der gently a few times, and determine the Brix in the regular manner, obtaining the reading immediately after mixing before the insoluble material has had time to settle. (b) CaO: Measure out 10 ml of the cooled liquid with a pipette into a porcelain casserole. Add 50-100 ml of water and proceed as in the "General Methods," 11. Subtract the number of ml of alkali from the number of ml of acid used, and divide by 2. 13. LIME CAKE, FIRST PRESSES Determine every 3 hours : (a) Total Sugar. (b) Free Sugar. (c) CaO. (d) Sugar to 100 CaO. SAMPLING (PLATE AND FRAME PRESSES) All samples are to be taken by a laboratory employe, who should receive the following instructions: (1) Visit the press floor at irregular intervals. (2) Sample any press or presses which are being dumped. (3) As a rule, do not sample a press the washing of which is finished while the employe is on the press floor. (4) Use a special closed can provided with a tube which cuts a plug one inch in diameter from the cake. (5) Sample several frames selected at random in each press. (6) Distribute the points in each frame where samples are taken equally over the face of the cake, taking one plug from each corner and one from the middle of the frame. (7) At least five presses shall enter into each sample taken to the laboratory for analysis. NOTE: If conditions warrant it, a man under laboratory supervision should be stationed permanently on the press floor so that all presses dumped may be sampled. II. REGULAR FACTORY CONTROL 27 SAMPLING (KELLY PRESSES) Where the manner of installation permits, catch a portion of the cake discharged from each frame by laying a board diagonally across the hopper before the press is opened, placing one end of the board flush against a corner of the hopper near the press in order that a small portion of any cake which may have fallen off into the drum and may not have been properly washed may be included in the sample. When the press has been emptied, obtain an average sample of the material on the board by means of a sampling device of the kind used for sampling plate and frame presses, or by means of a piece of tubing about l 1 ^ inches in diameter. Where the presses are set too low to admit of the board being used, employ a rectangular metal box attached to a long curved handle, the whole of rigid construction, by means of which sam- ples may be caught underneath the several frames as the cake drops off; preserve the various samples taken in a covered con- tainer. In catching the samples be careful to avoid any water from the hose used for washing the cake off the frames. If an appreciable amount of cake falls off into the drum, en- deavor to include a proportionate amount of this in the sample. Follow also the general instructions under " Sampling (Plate and Frame Presses) " as far as they can be made to apply to Kelly presses, but do not under any circumstances obtain the sample by scraping the cake from the sides of the outer frames or from the top of the several frames. PREPARATION OF SAMPLE Transfer the entire sample to a large iron mortar and mix thoroughly with an iron pestle. ANALYSIS (a) Total Sugar Method I: Weigh out 53 grams in a counterpoised Monel metal cup, or " capsule," of about 350 ml capacity. Add from an automatic pipette 177 ml of a 10% solu- tion of commercial zinc nitrate. Put in a piece of metal chain, cover with an aluminum disc enclosed in a rubber envelope, and shake vigorously until the cake has been completely disintegrated. Filter and polarize in a 200 mm tube. The reading gives directly the percentage of total sugar. Total Sugar Method II: Weigh out 54 grams in a counter- poised metal cup and add slowly 177 ml of dilute acetic acid (see 28 METHODS OF ANALYSIS Chap. XXV, 1), stirring with a glass rod until most of the foam- ing has ceased. Put in a piece of metal chain, cover, and shake as in the previous method. Then add 3 ml of basic lead acetate solution, shake again, filter, and polarize in a 200 mm tube. The reading gives directly the percentage of total sugar. (b) Free Sugar Method I: Weigh out 53 grams and de- termine as in "Total Sugar Method I," adding, in place of the zinc nitrate solution, 177 ml of water containing 3 ml of lead acetate in each 177 ml. Free Sugar Method II: Weigh out 54 grams, and determine as in "Total Sugar Method II," adding 177 ml of water without any acetic acid, followed by 3 ml of lead acetate. (c) CaO: Weigh out 5 grams and proceed as in the "Gen- eral Methods," 11. (d) Sugar to 100 CaO: Multiply the percentage of total sugar by 100 and divide by the percentage of CaO. 14. LIME CAKE, SECOND PRESSES Determine every 8 hours: (a) Total Sugar. (b) CaO. SAMPLING AND PREPARATION OF SAMPLE Take and prepare the sample in the same manner as the first lime cake. ANALYSIS Determine total sugar and CaO in the same manner as in the first lime cake. 15. LIME SEWER Determine every 2 hours : (a) Total Sugar. (b) CaO. (c) Sugar to 100 CaO. SAMPLING Obtain a continuous sample if a suitable device is available. In the absence of this take a catch sample at least every hour from II. REGULAR FACTORY CONTROL 29 the mud mixer, or, in the absence of a mud mixer, at some point in the line leading to the sewer, or if possible at the point of dis- charge into the sewer. Mix the sample thoroughly until any lumps are broken up, and take a portion to the laboratory. Make up a composite sample every 2 hours. ANALYSIS If the material is thin enough to measure readily, use Method II for total sugar. If the material is thick, use Method I. (a) Total Sugar Method I: Mix the sample well, and de- termine as in the case of "Lime Cake, First Presses," Method I or Method II. Total Sugar Method II: Mix the sample well, measure out 100 ml in a 100-110 ml flask, add a few drops of phenolphthalein and neutralize with acetic acid. Add 3 ml of lead acetate, make up to the 110 ml mark with water, shake, filter, and polarize in a 200 mm tube. Obtain the "grams of sugar in 100 ml" from Table 6. (b) CaO: If the total sugar has been determined by taking a definite weight of the material, mix the sample well, weigh out 10 grams, and determine as in the case of "Lime Cake, First Presses. ' ' Subtract the number of ml of alkali from the number of ml of acid used, and divide by 2. If the total sugar has been determined by measuring out a definite volume, use 10 ml, or a multiple thereof, and determine as in the case of "Lime Cake, First Presses." If 10 ml is used, subtract the number of ml of alkali from the number of ml of acid used, and divide by 2. (c) Sugar to 100 CaO: Multiply the percentage of total sugar by 100 and divide by the percentage of CaO. 16. EXCESS WATER Determine every 4 hours: (a) Brix. (b) Total Sugar. SAMPLING Obtain the sample from the excess water tank or pump. 30 METHODS OF ANALYSIS ANALYSIS (a) Brix: Follow the " General Methods," 1 (a). (b) Total Sugar: Determine as in the case of "Lime Sewer, Total Sugar Method II." 17. SWEET WATER. Determine every 4 hours on a catch sample : (a) Brix. Determine every 8 hours on a catch sample : (b) Apparent Purity. (c) Lime Salts (CaO to 100 Brix). SAMPLING Take a catch sample from the sweet water tank every 4 hours. ANALYSIS (a) Brix: Follow the "General Methods," 1 (a). (b) Apparent Purity: Evaporate to approximately thin juice density, and carbonate and proceed as in the case of "5. First Saturation Juice." (c) Lime Salts (CaO to 100 Brix) : Use the carbonated solu- tion prepared for the apparent purity determination, and follow the "General Methods," 12 (b). 18. FILTER CLOTH WASH WATER Determine every 8 hours: (a) Sugar. SAMPLING Take a small sample from each tank or washing machine emptied to the sewer, and keep in a covered container. Do not include in the sample any water returned to the process. ANALYSIS Mix well and determine as in the case of "Lime Sewer, Total Sugar Method II." n. REGULAR FACTORY CONTROL 31 19. MAIN SEWER Determine every 2 hours: (a) Sugar. SAMPLING Take a catch sample every 2 hours at a point where it will represent all sewer water leaving the main factory, but avoiding the pulp silo drainage if possible. Or take more frequent samples and composite every 2 hours. ANALYSIS Mix well and determine as in the case of "Lime Sewer, Total Sugar Method II." Polarize in a 400 mm tube and obtain the percentage of sugar from Table 7. 20. WHITE PAN STORAGE TANKS Determine at least every 8 hours : (a) Brix. (b) Alkalinity. (c) Apparent Purity. SAMPLING Take samples from each tank on the pan floor at the beginning of every shift. Special samples sent to the laboratory at any time during the shift may be used in lieu of these samples. ANALYSIS Follow the "General Methods." 21. WHITE MASSECUITE Determine on every pan dropped : (a) Brix. (b) Alkalinity. (c) Apparent Purity. (d) Lime Salts (CaO to 100 Brix). 32 METHODS OF ANALYSIS SAMPLING Take the sample from the pan or from the spout leading to the mixer before the pan is steamed out. ANALYSIS Follow the "General Methods." 22. HIGH GREEN AND WASH SYRUPS Determine either once or twice during the spinning of every pan, or at regular intervals of every 2 hours : (a) Apparent Purity. SAMPLING Take the samples from the machine receiving tanks where such tanks are in use, otherwise from the troughs leading from the machine spouts to the pumps, or from the pumps. Whenever possible obtain samples that have been mixed by steam. Do not take the samples from the machine spouts. ANALYSIS Follow the "General Methods." 23. MOISTURE IN WHITE SUGAR Determine moisture every 8 hours in the following samples: (1) Wet Sugar. (2) Sugar leaving upper granulator. (3) Standard granulated. (4) Table granulated. SAMPLING Provide a sufficient number of 1 x 3 inch test tubes and rubber stoppers; it is advisable to heat both the test tubes and stoppers in a drying oven to make sure that they are perfectly dry. Sample each kind of sugar every 2 hours by filling a test tube, and stopper immediately. Make up a composite sample every 8 hours for each kind of sugar sampled by emptying the four individual samples into a wide mouth, glass stoppered bottle and mixing thoroughly. II. REGULAR FACTORY CONTROL 33 Obtain the wet sugar from the discharge into the wet box or from the feed of the wet box to the upper granulator. Sample the "sugar leaving upper granulator" at the discharge from the upper to the lower granulator. Obtain the Standard and Table granulated at the discharge from the dry boxes into the bag. If the factory has only a single granulator system, omit sample (2). ANALYSIS . Place approximately fj grains in the case of wet sugar, and 10 grams in the case of granulated, in a 2 x 1% inch aluminum dish provided with a cover, which has been previously dried at 100-105. Cover the dish, and weigh accurately, but as rapidly as possible, on an analytical balance. Remove the cover and dry at 100-105 in a glycerin oven for 5 hours. Replace the cover, cool in a desiccator over sulphuric acid, and weigh. Keep thermometers in the desiccator and balance case, and do not make the weighings until the difference in temperature is 2 or less. The loss in weight after 5 hours heating is considered to represent the amount of moisture. NOTE: The concentrated sulphuric acid in the desiccator must be renewed once every week, experience having shown that sugar, after drying for 5 hours or more, is capable of absorbing n-tih , from strong acid after it has become diluted with small amounts of moisture. The acid should be renewed also at any time u'Jii'n it becomes discolored from contamination with organic mat- The cover of the desiccator should be frequently cleaned and coated with fresh vaseline. 24. PERCOLATION TESTS OF WHITE SUGAR If the white sugar is not up to standard, make percolation tests occasionally to obtain an approximate idea of how much of the color is due to adhering syrup which should have been washed out in the centrifugal machines. Close the bottom of a one-pint Oldberg percolator with a loosely fitting cotton plug, put in 250 grams of sugar and add 250 ml of distilled water. Catch the percolate in 1 x 6 inch text tubes in four or five successive portions, and compare the color of the solutions. 25. DUST BOX Determine every 8 hours: (a) Brix. 34 METHODS OF ANALYSIS (b) Alkalinity. (c) Apparent Purity. SAMPLING Take a catch sample of the liquid in the dust box. ANALYSIS Follow the "General Methods." 26. REMELT PAN STORAGE TANKS Determine at least every 8 hours: (a) Brix. (b) Apparent Purity. SAMPLING See "White Pan Storage Tanks." ANALYSIS Follow the "General Methods." 27. REMELT MASSE CUITE FROM PAN Determine on every pan dropped: (a) Brix. (b) Alkalinity. (c) Apparent Purity. (d) Lime Salts (CaO to 100 Brix). Determine every 24 hours : (e) True Purity. (f) Raffinose (% on dry substance). SAMPLING Take the sample from the pan or from the trough leading to the crystallizers before the pan is steamed out. ANALYSIS Follow the "General Methods." Obtain the dry substance for the true purity determination either by the refractometer or by oven drying. II. REGULAU FACTORY CONTROL 35 28. EEMELT MASSECUITE FROM CRYSTALLIZEB. Determine on every crystallizer dropped: (a) Brix. (b) Alkalinity. (c) Apparent Purity. SAMPLING Take a sample from the discharge of the crystallizer a few minutes after the gate has been opened. ANALYSIS Follow the " General Methods." 29. LOW GREEN AND WASH SYRUPS. Determine either once or twice during the spinning of every crystallizer, or at regular intervals of every 2 hours: (a) Apparent Purity. SAMPLING Sample in the same manner as "High Green and Wash Syrup." ANALYSIS Follow the "General Methods." 30. REMELT SUGAR Determine every 4 hours: (a) Apparent Purity. (b) Polarization. Determine every 24 hours: (c) Sulphuric Acid (SO,). SAMPLING A laboratory employe should take samples at irregular inter- vals, preferably from the discharge of the scroll into the melter, or at some other suitable place if this is not possible. Keep in. 36 METHODS OF ANALYSIS a covered can, and mix thoroughly before analysis, taking care to break up any lumps. For the sulphuric acid determination make up a 24 hour composite sample by mixing* equal portions of the samples prepared every 4 hours for the regular laboratory analysis. ANALYSIS (a) Apparent Purity: Weigh out 130 grams in a counter- poised copper beaker, dissolve in hot water, pour into a 500 ml Kohlrausch flask, rinsing the beaker with water, cool to approxi- mately 20, make up to the mark with water, shake well, and deter- mine the apparent purity as in the "General Methods." (b) Polarization: Increase the polariscope reading obtained in the apparent purity determination by one-tenth of its value. (c) Sulphuric Acid (SOJ: Follow the "General Methods," using 20 grams of material. 31. SUGAR MELTER Determine every 8 hours: (a) Brix. (b) Apparent Purity. Determine every 2 hours, when lime is added to the melter : (c) Alkalinity. SAMPLING Take a catch sample from the melter or melter pump. ANALYSIS (a) Brix and (b) Apparent Purity: Follow the "General Methods." In case lime is added to the melter, the sample should be carbonated and filtered before the purity is determined, as in the case of "First Saturation Juice.' 1 (c) Alkalinity: Measure out 10" ml and titrate in the cold with N/28 sulphuric acid according to the "General Methods." 32. MOLASSES PRODUCED Determine every 8 hours : (a) Brix. II. REGULAR FACTORY CONTROL 37 (b) Sugar. (c) Apparent Purity. Determine at least every 24 hours: (d) True Purity. (e) Raffinose (% on dry substance). SAMPLING Draw at least one sample from every scale tank weighed, and if possible take several samples at intervals during the period when the tank is being filled or emptied. Composite the individual samples in a large bucket and mix well before analysis. ANALYSIS Follow the * ' General Methods. ' ' Obtain the dry substance for the true purity determination either by the refractometer or by oven drying. 33. CONDENSED WATERS Examine every hour : (a) Boiler feed water (both the "tank" and "returned direct"), press wash water, pure and impure battery supply water. Examine every 2 hours: (b) All individual pan and evaporator tail pipes. SAMPLING Collect continuous samples with an automatic sampling device. Protect the samples from contamination both during the time when they are being drawn and when they are being brought to the laboratory. See Chap. XVII, 2, regarding the collection of campaign sam- ples for analysis, and of weekly samples of battery supply water. EXAMINATION Test with alpha-naphthol as described in the "General Meth- ords," I, 13. As the reagents employed frequently become con- taminated, check them up every day with water of negative reaction. 38 METHODS OF ANALYSIS NOTE: If sugar is found, determine the source at once and report it to the operating department. It is desirable to have in use a "board" or some system representing a flow chart of the condensed waters, in order that the source of sugar may be readily and quickly located. 34. BOILER WATER. Determine every 8 hours on each boiler in service : (a) Alkalinity. SAMPLING Draw from the sampling line, first allowing the water to run a few moments to rinse out the pipe. ANALYSIS Measure out 10 ml with a pipette into a porcelain dish and follow the "General Methods," 10 (a), using phenolphthalein as indicator. Dilute with sufficient neutral water to make the color reaction distinct. 35. WEEKLY COMPOSITE SAMPLES Determine : (a) Brix. (b) Apparent Purity. (c) Dry Substance (by oven drying). (d) Sugar (direct polarization). (e) Sugar by Inversion. (f) Raffinose. (g) Invert Sugar, (h) Ash (Sulphated). (i) Undetermined. (j) Lime Salts (CaO to 100 Brix). (k) Sulphuric Acid (S0 3 ). (1) Organic Coefficient. (m) Dry Substance (by refractometer, if available). SAMPLING Make up an average sample of each of the following products by taking equal portions of each sample brought to the laboratory II. REGULAR FACTORY CONTROL 39 during the week and preserving in a sealed jar or stoppered bottle. (1) Evaporator Thick Juice. (2) White Massecuite. (3) Remelt Massecuite (from pan). (4) Remelt Sugar. (5) Molasses Produced. (6) Molasses Worked. (7) Cold Saccharate Cake. (8) Cold Perfectly Washed Saccharate Cake. (9) Hot Saccharate Cake. (10) Hot Perfectly Washed Saccharate Cake. (11) Saccharate Milk. In the case of the saccharate cakes and milk, use the thick syrup obtained by evaporating the thin juice from the apparent purity determination to 60-70 Brix on a water bath. Concentrate this juice as soon as it is available, not allowing it to stand in a thin condition. When the massecuite samples are desired for analysis, heat the containers by immersion in hot water, remove the contents, and mix thoroughly in order to obtain a uniform mixture of sugar crystals and mother syrup. ANALYSIS Follow the "General Methods." Analyses may be made, if desired, on "double diluted" solutions in the case of massecuites, raw sugar, and molasses, using twice the amount of material as when analyzing original material direct. Preserve the double diluted solutions from decomposition with 3 to 4 drops of a 40% formaldehyde solution, but do not use any double diluted material which has stood for more than eight hours. Determine the dry substance in Remelt Sugar by heating approximately 5 grams without dissolving in water and without the use of sand. Make all the prescribed determinations except as follows : (1) Omit the Brix determination in the case of Remelt Sugar. (2) In the case of the Cold and Hot Perfectly Washed Cakes determine only the Brix, dry substance, sugar, sugar by inversion, raffinose, ash, and apparent purity. To obtain the "percentage on dry substance" in any case, multiply the "percentage on original" by 100 and divide by the percentage of dry substance. Use the dry substance found by oven drying in calculating percentages on dry substance. 40 METHODS OP ANALYSIS To obtain (i) Undetermined, subtract from 100 the sum of the percentages of (e) Sugar by Inversion, (f) Eaffinose, (g) Invert Sugar, and (h) Ash (all percentages on dry substance). Calculate (1) Organic Coefficient as described in the "General Methods," I, 8. NOTE: See Chap. XVII, 2 (b) regarding the collection of weekly average samples of pure and impure battery supply water for the determination of total solids. 36. TEMPERATURE DATA. GENERAL Obtain the necessary temperature data either from the charts of recording thermometers or by averaging readings taken every 2 hours by a laboratory employe. Check recording thermometers previous to every campaign, and if possible at occasional intervals during the campaign. It is advisable to have provision for a well near each recording thermometer, by means of which the latter may be checked in situ with an accurate indicating thermometer. The following directions apply to particular cases. DIFFUSION BATTERY TEMPERATURE READINGS A laboratory employe should take a series of readings of the thermometers on each battery, starting in every case at the "cos- sette cell ' ' and continuing successively along the other cells in cir- culation. Do not record readings of any cells not in circulation at the time. Take the readings at least every 2 hours. In order that the figures obtained may be comparable at all factories, observe also the following precautions : (1) Commence the readings immediately after the period of "sending over" begins and not during the period of diffusing a fresh cell. (2) The figure reported for the temperature of cell No. 1 should represent the temperature of the juice entering the cossette cell and not the temperature of the juice from the cossette cell which goes to the measuring tank. (3) The last temperature reading should represent the tem- perature of the battery supply water entering the "pulp" or "water" cell. The arrangement of thermometers on the batteries II. REGULAR FACTORY CONTROL 41 is such that in most cases this reading can be obtained from a battery thermometer. (4) As the position of the thermometers on different bat- teries varies, the matter should be gone over individually at each factory and arrangements should be made to have the readings properly taken. Obtain the "average maximum temperature of the battery" by averaging the temperature readings of those cells carried at the maximum temperature. JUICE LEAVING FIRST PRESSES Obtain every 2 hours by filling a sample bucket from the press cocks and taking a reading immediately with a mercury ther- mometer. SUGAR LEAVING UPPER GRANULATORS Fill a sample bucket every 2 hours from the discharge from the upper to the lower granulator arid insert the bulb of a mercury thermometer into the middle of the mass of sugar. SUGAR AS SACKED Take readings every 2 hours by inserting a mercury ther- mometer deeply into a bag of sugar just filled at the sacking station. REMELT MASSECUITE AS DROPPED Insert a mercury thermometer in the sample taken for the laboratory analysis; obtain the reading immediately after the sample is taken. Or obtain the information from the pan recording thermometer or the sugar boiler's record. KKMKLT M.\ SMECTITE AS SPUN Take a sample every 2 hours from the goosenecks of the mixer and insert a mercury thermometer. HI. SULPHATE CONTROL 1. INTRODUCTION Whenever the concentration of sulphuric acid in the remelt massecuite exceeds the amount which can be held in solution and eliminated in the molasses (usually 1.0 1.5 per cent S0 3 on mo- lasses dry substance), the excess crystallizes out, mostly as potas- sium sulphate, in the remelt sugar. This not only impairs the quality of the remelt sugar, but may even in extreme cases lead to the presence of small amounts of S0 3 in the white sugar. The usual practice to control this is the treatment of the melted sugar, when necessary, with barium oxide, calcium chloride, or lime. The special sulphate control described in this chapter is designed to throw light on the amount of sulphuric acid in the various products, including the amount formed in sulphuring the juice, and on the efficacy of the melted sugar treatment when used. The determination of sulphuric acid (S0 3 ) in the remelt sugar (see section 7) is prescribed as a regular daily test, The deter- mination should be made also in the white sugar (section 6) whenever the S0 3 in the remelt sugar exceeds 1.00 per cent. The determinations described in sections 7 10 should be made when- ever treatment for the removal of sulphates is being employed. The determinations described in sections 2 6 are for use on special occasions when it is desired to investigate the amount of sulphuric acid formed at the sulphur stations. 2. SECOND SATURATION JUICE Determine : (a) Sulphuric Acid (S0 3 to 100 Brix). III. SULPHATE CONTROL 43 SAMPLING Make up a composite sample by mixing equal amounts of the composite samples prepared every 4 hours for the regular labora- tory analysis. (See Chap. II, 6.) Use a few drops of formalde- hyde to preserve the samples. ANALYSIS (a) Sulphuric Acid (S0 3 to 100 Brix): Follow the "General Methods," Chap. I, 9. Either determine the Brix or use the average of the regular Brix determinations. 3. THIRD SATURATION JUICE Determine : (a) Sulphuric Acid (S0 3 to 100 Brix). SAMPLING AND ANALYSIS Make up a composite sample and analyze in a similar manner to "2. Second Saturation Juice." 4. BLOW-UP THICK JUICE BEFORE SULPHUR Determine : (a) Sulphuric Acid (S0 3 to 100 Brix). SAMPLING AND ANALYSIS Make up a composite sample from the samples of evaporator thick juice prepared every 4 hours for the regular laboratory analysis, and analyze in a similar manner to "2. Second Satura- tion Juice." Note: If melted sugar is added to the blow-ups, this deter- mination is of no value. 5. BLOW-UP THICK JUICE AFTER SULPHUR Determine : (a) Brix. (b) Sulphuric Acid (S0 3 to 100 Brix). 44 METHODS OF ANALYSIS SAMPLING AND ANALYSIS . Make up a composite sample from the samples prepared every 4 hours for the regular laboratory analysis, and analyze in a simi- lar manner to "2. Second Saturation Juice." Determine the Brix in the regular manner. 6. WHITE SUGAR Determine every 24 hours : (a) Sulphuric Acid (S0 3 011 original). SAMPLING Make up a composite sample by mixing equal amounts of the samples of Standard granulated sugar prepared every 8 hours for the moisture determination. ANALYSIS Follow the "General Methods/' I, 9. Make a blank S0 3 test on the distilled water and reagents, and deduct the correction found from the amount found in the analysis of the sugar. 7. REMELT SUGAR Determine every 24 hours : (a) Sulphuric Acid (S0 3 on original). SAMPLING Make up a composite sample by mixing equal portions of the samples prepared every 4 hours for the regular laboratory analysis. ANALYSIS Follow the "General Methods," making sure that an excess of barium chloride solution is added. NOTE: This is a test required in the "Regular Factory Con- trol." See Chap. II, 30, (c). 8. MELTED SUGAR BEFORE TREATMENT Determine every hour: (a) Alkalinity. (Determine only when lime or barium oxide is used for treatment.) HI. SULPHATE CONTROL 45 Determine every 24 hours : (b) Brix. (c) Sulphuric Acid (S0 3 to 100 Brix). SAMPLING If lime or barium oxide is being used for treatment, which is usually continuous, take a catch sample from the'melter every hour. If calcium chloride is used for treatment, which is usually inter- mittent, take a catch sample of each lot treated previous to the addi- tion of the calcium chloride. Make up a composite sample by mix- ing equal portions of the individual samples. ANALYSIS (a) Alkalinity: If the alkalinity is 0.2 or less, titrate 10 ml with N/28 acid according to the general method for alkalinity. If the alkalinity is higher, titrate 50 ml with Steffen acid; in this case divide the number of ml of acid used by 10 to obtain the al- kalinity in terms of * ' grams of CaO per 100 ml. ' ' (b) Brix and (c) Sulphuric Acid (S0 3 to 100 Brix): Fol- low the ' ' General Methods. ' ' 9. MELTED SUGAR AFTER TREATMENT Determine every 8 hours, as in regular factory control : (a) Brix. (b) Apparent Purity. Determine every 24 hours : (c) Sulphuric Acid (S0 3 to 100 Brix). SAMPLING Take a catch sample every 2 hours, if possible, from the cocks or trough of the filter press. Mix equal amounts of these samples to obtain the composite samples when needed. ANALYSIS (a) Brix and (b) Apparent Purity: Follow the ''General Methods." In case lime or barium oxide is added to the melter, the sample should be carbonated and filtered before the purity is determined, as in the case of "First Saturation Juice." (See Chap. II, 5.) 46 METHODS OF ANALYSIS (c) Sulphuric Acid (S0 3 to 100 Brix) : Follow the ' ' General Methods." 10. SULPHATE CAKE Determine every 24 hours : (a) Sugar. (b) Sulphuric Acid (S0 3 ). SAMPLING Follow in general the method of sampling outlined under "Lime Cake., First Presses," Chap II, 13. ANALYSIS (a) Sugar: Use either of the methods for "total sugar" described under "Lime Cake, First Presses," Chap. II, 13 (a). (b) Sulphuric Acid (SOJ: Weigh out 2 5 grams of cake, add 100 ml of water, neutralize with hydrochloric acid, and add 3 ml in excess. Boil for a few minutes, filter, and proceed as in the "General Methods," Chap. I, 9, making sure that an excess of barium chloride solution is added. IV. STEFFEN PROCESS CONTROL 1. GENERAL All samples in connection with the Steffen Process control must be taken by a laboratory employe. 2. MOLASSES WORKED Determine every 8 hours : (a) Brix. (b) Sugar. (c) Apparent Purity. Determine every 24 hours: (d) Sugar by Inversion (Per cent on original). SAMPLING Take a catch sample at least every 2 hours, and preferably every hour, at the molasses scale tank. Keep the individual samples in a covered container, and mix thoroughly previous to analysis. ANALYSIS Follow the " General Methods." Determine the direct polar- ization and the polarization after inversion on a composite sample representing the molasses worked during the entire 24 hours, and calculate the percentage of "sugar by inversion" in the molasses. 3. SOLUTION FOR COOLER Determine every 3 hours : (a) Brix. 48 METHODS OF ANALYSIS (b) Alkalinity. (c) Sugar (grams in 100 ml). SAMPLING Take a catch sample of the solution iri the cooler after the pro- peller has been started and immediately preceding the beginning of the lime addition. ANALYSIS ( a ) Brix : Follow the " General Methods. ' ' (b) Alkalinity: Mix the sample well and transfer 50 ml with a pipette to a 100 ml flask. Add a few drops of phenolphthalein and titrate to neutrality with Steffen standard acid (1 ml = .05 g CaO). Divide by 10 the number of ml of acid required. See 1 ' General Methods, "1,10 ( c ) . (c) Sugar: Add 3 6 ml of basic lead acetate to the neutral- ized solution obtained in (b), fill to the 100 ml mark with water, shake, filter, and polarize in a 200 mm tube. Multiply the reading by .52 or use Table 9, to obtain the grams of sugar in 100 ml. 4. LIME POWDER Determine every 8 hours : (a) Loss on Ignition. (b) CaO by Titration. (c) Percentage Coarser than 200 mesh. SAMPLING Take a catch sample every hour from the discharge of each mill in operation, taking an equal amount of material from each mill. Composite the hourly samples by transferring to glass bottles pro- vided with tightly fitting rubber or ground stoppers, keeping sepa- rate samples for each mill. For (a) Loss on Ignition and (b) CaO ~by Titration, make up a composite sample by taking equal portions from each mill composite and mixing thoroughly. ANALYSIS (a) Loss on Ignition: Weigh out approximately 1 gram on an analytical balance, in a covered platinum crucible. Ignite to constant weight in an electric furnace or over a good blast lamp, IV. STEFFEN PROCESS CONTROL 49 cool in a desiccator, and weigh. Multiply the loss in weight by 100 and divide by the weight of the sample. (b) CaO by Tit rat ion: Weigh out 5 grams, transfer to a porcelain casserole, and follow the " General Methods," I, 11. (c) Percentage Coarser than 200 mesh: Determine for each mill separately. Weigh out 20 grams on a pulp balance, and trans- fer to a 200 mesh, brass wire sieve (width of opening = .0029 inch) . Brush the material carefully with a two-inch flat camel hair brush until practically no more fine powder passes through. Weigh the coarse residue on a pulp balance. Multiply the weight of the residue by 5 to obtain the percentage. When the sieve becomes clogged, clean it with hydrochloric acid, rinse it well with water, and dry it in a warm place. SPECIAL DETERMINATIONS (d) Sugar-soluble CaO: Rinse 5 grams of lime powder into a 200 ml flask, and add 150 ml of a freshly prepared, 25 Brix sugar solution. (Or add approximately 40 grams of sugar and dissolve by the addition of water.) Fill to the mark with water, stopper the flask and shake vigorously, repeating the shaking at short intervals as the lime settles to the bottom. Filter at the end of thirty minutes, and titrate 100 ml with the standard nitric acid (1 ml = .05 g CaO), using phenolphthalein as indicator. Multiply by 2 the number of ml of acid required, to obtain the percentage of CaO. (e) Slacking Test:.. Into a beaker of 250 ml capacity measure out 100 ml of water at exactly 20. Add 25 grams of the lime powder, using a thermometer as a stirring rod, and continue to stir until there is no further rise in temperature. Record the num- ber of degrees increase in temperature over the original 20, and the number of minutes required to attain the maximum tempera- ture. 5. COOLER WASTE WATER Determine every hour: (a) Sugar (grams in 100 ml). SAMPLING Take a catch sample, just previous to the time it is required for analysis, from a finished cooler, after all the lime has been added, and just before the finished cooler is dropped. 50 METHODS OP ANALYSIS ANALYSIS Filter a portion immediately through filter paper. Transfer 50 ml of the filtrate with a pipette to a 100 ml flask, add a few drops of phenolphthalein, neutralize with Steffen standard acid, and pro- ceed as in the determination of sugar in "Cold Press Waste Water," 6 (c). 6. COLD PRESS WASTE WATER Determine every 2 hours: (a) Brix. (b) Alkalinity. Determine every hour : (c) Sugar (grams in 100 ml). SAMPLING Collect a continuous sample from the cold waste water line in the manner described below under "7. Total Waste Water,'"' or take a catch sample every hour from the discharge of the cold presses. Mix the sample well before analysis. ANALYSIS (a) Brix: Follow the "General Methods." (b) Alkalinity: Transfer 50 ml with a pipette to a 100 ml flask. Add a few drops of phenolphthalein and titrate to neutrality with Steffen standard acid (1 ml = .05 g CaO). Divide the num- ber of ml of acid required by 10. See "General Methods," I, 10 (c). (c) Sugar: Add 2 4 ml of basic lead acetate to the neutral- ized solution obtained in (b), fill to the 100 ml mark with water, shake, filter, and polarize in a 200 mm tube. Multiply the reading by .52, or use Table 9, to obtain the grams of sugar in 100 ml. 7. TOTAL WASTE WATER Determine every 2 hours: (a) Brix. (b) Alkalinity. Determine every hour: (c) Sugar (grams in 100 ml). IV. STEPFEN PROCESS CONTROL 51 SAMPLING Collect an average sample from the pipe line which conducts the final waste water outside the factory, by means of a continuous, automatic sampling device which delivers into a large vessel pro- vided with an overflow at the top and a drain at the bottom. Mix the entire sample, take a small portion for analysis, and empty cut the remainder by opening the drain valve. If for any reason it is impossible to secure a continuous sample, take a catch sample every hour. Mix the sample well before analysis. ANALYSIS Analyze as in the case of "Cold Press Waste Water," cooling first if necessary. 8. COLD WASH WATER (FINAL) Determine every 4 hours : (a) Brix. SAMPLING Sample the wash water coming from the presses at the time when the washing is finished. The sample used for analysis should preferably represent a composite of samples obtained from at least three presses. This sample cannot be obtained at factories equipped with vacuum filters. ANALYSIS Determine the Brix in the regular manner. 9. COLD WASH WATER (AVERAGE) Determine every 4 hours : (a) Brix. (b) Alkalinity. (c) Sugar (grams in 100 ml). SAMPLING Take a sample from the wash water tank. ANALYSIS Analyze as in the case of ' ' Cold Press Waste Water. ' ' 52 METHODS OF ANALYSIS 10. HOT WASH WATER (FINAL) Determine every 4 hours : (a) Brix. (b) Alkalinity. (c) Sugar (grams in 100 ml). SAMPLING Sample in the same manner as the final cold wash water. The sample must represent the wash water coming from the hot presses at the time when the washing is finished. At factories equipped with vacuum filters, where this sample cannot be obtained, substi- tute the "average" hot wash water. ANALYSIS Analyze as in the case of "Cold Press Waste Water." 11. COLD SACCHARATE CAKE Determine every 3 hours : (a) Apparent Purity. (b) Lime Salts (CaO to 100 Brix). Determine every 8 hours : (c) Apparent Purity (Perfectly Washed). (d) Sugar. (e) CaO. (f) CaO to 100 Sugar. Determine every 24 hours : (g) Moisture. (h) True Purity. (i) Raffinose (Per cent on dry substance), (j) True Purity (Perfectly Washed). SAMPLING Take a sample once an hour from various parts of the cake in several frames, using a spoon and bucket. In the case of vacuum filters take small portions of the material dropping from the drums of all the units in operation. Sample Kelly Presses in the manner described under II, 13, "Lime Cake Sampling (Kelly Presses)." IV. STEFFEN PROCESS CONTROL 53 Preserve the samples in a covered container and make up com posite samples at the times when the various determinations are due, except as otherwise noted. Mix all composite samples well. ANALYSIS (a) Apparent Purity: The following special apparatus is needed: A carbonator with steam and carbon dioxide gas connec- tions, and an evaporator heated by steam, both so constructed as to obviate any possibility of burning the juice. Mix a suitable amount of the cake with 4 5 parts of water un- til a homogeneous mixture is obtained. Transfer to the laboratory carbonator, heat to 80 85, and carbonate at this temperature to faint alkalinity with phenolphthalein. Do not carbonate to neu- trality or acidity. When the carbonation is finished, heat to boiling, and filter. Concentrate sufficient of the filtrate to about 23 Brix in the laboratory evaporator, being careful not to carry the evap- oration much beyond this point on account of the danger of burning the juice. Draw off the liquid into a copper can or suitable ves- sel, and carbonate again to faint alkalinity. Filter, preferably under vacuum through a Buechner funnel. Cool the filtrate in a cylinder and determine the apparent purity as described in the ''General Methods." (b) Lime Salts (CaO to 100 Brix): Use 10 ml of the solu- tion prepared for the apparent purity determination, and follow the "General Methods," 12 (a). (c) Apparent Purity (Perfectly Washed) Apparatus: Use the regular equipment which consists of a closed cylindrical reser- voir, a small filter press, a vacuum leaf filter, and a rectangular tank divided into two sections, each of which is subdivided into two compartments by partitions extending nearly to the bottom. The reservoir has the necessary fittings at the bottom for connect- ing it to the small press or the vacuum leaf. Vacuum, air pres- sure, charging lines, and a relief valve are provided at the top of the tank. Clean the filter cloths frequently with hydrochloric acid and water. Use whichever of the following methods is found to give the most consistent results: Method I (Elutriation): Add 3 parts of the coldest water ob- tainable to 1 part of the sample, and stir until all lumps are broken up and a perfectly homogeneous mixture is obtained. Filter im- mediately through the laboratory press, allowing the pressure to 54 METHODS OP ANALYSIS rise gradually to 40 pounds per square inch and maintaining this pressure until the nitrate ceases to flow or comes in slow drops. Mix the cake thus obtained with 4 5 parts of water; and proceed exactly as under (a) "Apparent Purity." Method 11 (Vacuum Filtration): Fill one section of the rec- tangular tank of the equipment described above with finished cooler solution and submerge the leaf in one of the compartments. Open the valves in the vacuum line at the top of the reservoir and in the line connecting the leaf to the bottom of the reservoir, keep- ing all other valves closed. Maintain a vacuum of at least 15 inches on the gage and allow the cake to form until it is flush with the guide, stirring the solution continually during filtration in order to insure the formation of an even cake. When cake of the re- quired thickness has formed, transfer the leaf to the other section of the tank which has been filled with cold water, and allow 8 liters of wash water to pass through the cake ; this is most easily meas- ured by observing the level of the water at the time when washing is commenced and gradually adding 8 liters of cold water. When the same level is reached after the addition of the 8 liters, remove the leaf from the tank and allow the cake to dry for 5 minutes with the vacuum on. Shut off the vacuum, remove the cake, mix it with 4 5 parts of water, and proceed exactly as under (a) "Apparent Purity." If the cake cracks before the washing is completed, dis- card it and repeat the test. Clean the leaf frequently by washing it first with hydrochloric acid and then with water. Method 111 (Combined Elutriation and Washing) : Take a catch sample of finished cooler solution (about 10 liters is required) , and filter it immediately through the 3% inch frame of the labora- tory filter press under 30 pounds air pressure; do not allow air to go through the cake by permitting the reservoir to run empty. This will produce a cake weighing 5% pounds. Mix this cake thor- oughly and quickly with 100% of cold water, 5% pounds or 2600 ml, and filter through the 2%-inch frame of the small press at 30 pounds pressure ; again, do not allow air to pass through the cake. This will produce a cake weighing 4% pounds. Drain and wash out the reservoir, then introduce 100% of cold water, 4% pounds or 2150 ml, and force it through the cake at 15 pounds pressure, al- lowing air to pass through the cake for one-half minute after the water has all gone through. This yields a final eake of uniform weight and moisture content. Mix this cake with 4 5 parts of *It will facilitate the washing if the plug at the top of the 2V 2 inch frame is removed and a small rod is forced through the cake to the port. IV. STEFFEN PROCESS CONTROL 55 water, and proceed exactly as under (a) "Apparent Purity." If the two frames used are not of exactly the dimensions given, obtain a sufficient number of weights of cake to establish the amount of water required for elutriation and washing, which should be 100% on the weight of the cake in each case. (d) Sugar: Weigh oat 13 grams of the cake in a counter- poised nickel dish, reduce to a thin cream with water, and rinse into a 100 ml flask. Add a few drops of phenolphthalein and neu- tralize with dilute acetic acid, avoiding any great excess. Cool, add 3 5 ml of lead acetate, fill to the mark with water, shake, filter and polarize in a 200 mm tube. Multiply the polariscope reading by 2 to obtain the percentage of sugar. (e) CaO: Weigh out 10 grams of the cake, transfer to a porcelain casserole, and follow the "General Methods," I, 11. Subtract the number of ml of alkali from the number of ml of acid used, and divide by 2 to obtain the percentage of CaO. (f) CaO to 100 Sugar: Multiply the percentage of CaO by 100 and divide by the percentage of sugar. (g) Moisture: Weigh out approximately 10 grams of the composite cake sample in a covered aluminum dish, and dry for 5 6 hours at 100 105 as under the determination of dry sub- stance in the "General Methods," repeating the drying for one hour periods until the loss in any period is not over 0.2%. (h) True Purity: Evaporate on a water bath to approxi- mately 50 Brix a sample composed of equal portions of the 23 Brix juice used for the apparent purity determinations. Deter- mine the true purity as in the "General Methods." Obtain the dry substance either by the refractometer or by oven drying. (i) Raffinose (Per cent on dry substance): This is obtained in connection with the true purity determination. (j) True Purity (Perfectly Washed): Make up a composite sample and determine as under (h), using equal portions of the 23 Brix juice prepared for the determination of the apparent purity of the perfectly washed cakes. 12. HOT SACCHARATE CAKE Determine every 8 hours: (a) Apparent Purity. (b) Lime Salts (CaO to 100 Brix). (c) Apparent Purity (Perfectly Washed). 56 METHODS OF ANALYSIS (d) Sugar. (e) CaO. (f) CaO to 100 Sugar. Determine every 24 hours : (g) Moisture (h) True Purity. (i) Baffin ose (% on dry substance), (j) True Purity (Perfectly Washed). SAMPLING Follow the methods described under "11. Cold Saccharate Cake." In the case of Vallez presses, obtain the sample from the discharge of the press scroll before the water is turned on. If two different kinds of filters are in use, adjust the system of sampling so as to show the relative efficiency of the two types. ANALYSIS Follow the methods under "11. Cold Saccharate Cake." In making the perfectly washed cake, use Method I with the follow- ing modifications and precautions: (1) Use a catch sample of the hot saccharate cake, not allowing it to cool any more than can be avoided; (2) Elutriate with hot water (nearly boil'ing) ; (3) Heat up the apparatus with hot water before starting the filtration, 13". S AC CH ABATE MILK Determine every hour: (a) Brix. (b) CaO (grams in 100 ml). Determine every 4 hours: (c) Apparent Purity. SAMPLING Take a catch sample from the discharge line of the pump. For the purity determination make up a composite sample from equal amounts of the four previous hourly samples. ANALYSIS (a) Brix and (b) CaO: Determine as in the case of "Milk of Lime," Chap. II, 12. IV. STEFFEN PROCESS CONTROL 57 (c) Apparent rurity: To a composite of the previous hourly samples add 3 4 parts of water, mix well, and proceed with the carbonation, etc., as under 11 (a), "Cold Saccharate Cake- Apparent Purity." 14. SMALL COOLER TESTS Make occasional tests with the laboratory cooler to check up the efficiency of the factory coolers. See Chap. XXIII, 5 and 17, for directions regarding the speed and operation of the cooler. Determine : (a) Sugar in "Solution for Cooler." (b) Lime Added to 100 Sugar. (c) Sugar in Waste Water. (d) Percentage of Sugar Precipitated. Record also the temperature at start and finish, and the time required to add the lime. SAMPLING Use a sample of molasses and dilute with water to the required density or take a sample of the "Solution for Cooler" from the factory coolers. Take also a sample of the lime powder being used in the Steffen House at the time. OPERATION OF COOLER TEST See that the cooler is clean and well drained, and pour in 14,050 ml of the molasses solution. Commence the circulation of the cooling water. Allow the solution in the cooler to come to per- fect rest, in order to prevent the formation of foam when the propeller is started, then start the propeller, and, when the solu- tion has become well mixed, remove 50 ml for the determination of the sugar content, leaving a volume of 14,000 ml of solution in the cooler. When the solution is sufficiently cold, place in the hopper the weighed amount of lime which is estimated to be sufficient, or a little less than this amount, and introduce it into the solution through the bolter. When the lime has all been added, remove a small amount of the finished cooler solution without stopping the propeller, filter it immediately, and determine the sugar in the regular mamn'r. using 50 ml of the filtrate. If the result shows 58 METHODS OF ANALYSIS the lime addition to be insufficient, estimate the additional amount required, add this, test the finished cooler solution again as before, and repeat this procedure until the sugar 4 in the waste water is reduced to the desired percentage. Wash out the cooler thoroughly immediately after each test to prevent the tubes from becoming stopped up, being careful to avoid wetting the bolter. In general follow the current factory practice with regard to such conditions as the temperature of precipitation, the concen- tration of the cooler solution, and the sugar content of the waste water. It may often be desirable, however, to vary some of these conditions to obtain special information. The time of adding the lime may also be varied by changing the speed of the conveyor, or by feeding the lime to the conveyor by hand, and it will often be found that the rate of adding the lime has a great influence on the efficiency of the precipitation. ANALYSIS Use the regular methods given elsewhere in this chapter. Cal- culate the percentage of sugar precipitated as follows : Let a = sugar (grams in 100 ml) in Solution for Cooler b = sugar (grams in 100 ml) in Waste Water x = percentage of sugar precipitated 100 (a b) Then x= - - a Calculate the lime addition as follows: Let c = grams of lime powder used d = volume of cooler solution in milliliters (14000) y = lime to 100 sugar Then y== .0001ad If, however, the sample of " solution for cooler" has been obtained from the factory coolers and therefore contains lime from the previous cooler, determine the alkalinity and correct the lime addi- tion as indicated in the following formula : Let e = alkalinity (grams of CaO in 100 ml) of Solution for Cooler f = % CaO in lime powder de c + Then y = .0001 ad IV. STEFFEN PROCESS CONTROL 59 EXAMPLE Leta= 5.41 b = .52 c= 765 d = 14000 e= .70 f = 94.5 100 (5.41 .52) Then x = _ - : = 90.4 765 + 5.41 .70 X 14000 94.5 = = .0001 X 5.41 X 14000 15. TEMPERATURE DATA GENERAL Refer to the general instructions in the section of the same title in Chapter II, 36. The following directions apply to particular a in the Steffen Process Control. COOLER SOLUTION, AVERAGE MAXIMUM TEMPERATURE Record the maximum temperature reached in each case during the cycle of a sufficient number of coolers to give a fair average, and derive the average of these figures. Obtain the data from a recording thermometer or from the cooler man's record. ( 'OLD WASTE WATER, AVERAGE TEMPERATURE Obtain every 2 hours by filling a sample bucket from the dis- charge of the cold presses and taking a reading immediately with a mercury thermometer. Or obtain from a thermometer installed in the line leading from the cold presses to the heating system. HOT SOLUTION This should represent the temperature at which the heated waste water leaves the heating system and should be obtained from a thermometer suitably installed to indicate this. HOT WASTE WATER Obtain every 2 hours by filling a sample bucket from the dis- charge of the hot presses and taking a reading immediately with a. mercury thermometer. 60 METHODS OF ANALYSIS ADDITIONAL TESTS REQUIRED IN CONNECTION WITH DORR THICKENER VACUUM FILTER INSTALLATIONS 16. FEED TO THICKENER Determine eveiy 2 hours: (a) Brix. (b) Alkalinity. (c) Sugar (grams in 100 ml). SAMPLING Take a catch sample every 2 hours from the hot solution feed line to the Dorr Thickener, and filter immediately through paper. ANALYSIS Cool and analyze the filtrate as in the case of "6. Cold Press Waste Water." 17. OVERFLOW FROM THICKENER Determine every 2 hours : (a) Brix. (b) Alkalinity. (c) Sugar (grams in 100 ml). SAMPLING Take a catch sample every 2 hours, consisting of an equal amount from each of the pipe lines leading from the overflow boxes to the heat exchanger. ANALYSIS Mix the sample, cool ? and analyze as in the case of "Cold Press Waste Water." 18. DISCHARGE FROM THICKENER. Determine every 4 hours : (a) Brix. IV. STEFFEN PROCESS CONTROL 61 SAMPLING Take a catch sample of the thickened discharge every 4 hours, < insisting of an equal amount from each of the discharges into the hot filter tanks. ANALYSIS Mix the sample well, and transfer to a hydrometer jar. After cooling to approximately 20, mix again and determine the Brix in the regular manner, taking the reading as quickly as possible before the suspended matter has time to settle. 19. HOT FILTER WASTE WATER Determine every 2 hours : (a) Brix. (b) Alkalinity. (c) Sugar (grains in 100 ml). SAMPLING Take a catch sample every 2 hours from the discharge into the heat exchanger. ANALYSIS Cool and analyze as in the case of "Cold Press Waste Water." V, PULP DRYER CONTROL 1. GENERAL. All samples in connection with the Pulp Dryer Control must be taken by a laboratory employe. On account of the large number of moisture determinations it is advisable to have two drying ovens. A vacuum oven is recom- mended for the determination of moisture in "Pulp Leaving Dryer" and "Pulp as Sacked," and a double walled glycerin drying oven for the other moisture and dry substance determina- tions; the temperature should be carried at 100 105 C. in both kinds of ovens. Aluminum dishes, 3 inches in diameter x % inch high, provided with covers of the same material, should be used. As the determination of moisture in dried pulp requires sev- eral hours, a rapid' method is employed to give the operating men better control. This method is to heat for 1 hour in the oven and multiply the loss found by a factor, which is calculated from de- terminations made in the regular manner by heating for 5 6 hours and then for successive periods of one hour until the loss of weight in one hour is not over 0.1%. This factor varies from 1.05 to 1.15, and it is recommended that a factor of 1.10 be used until a more accurate factor is found for each laboratory. 2. MOLASSES TO PULP DRYER Determine every 8 hours : (a) Brix. SAMPLING Take a sample every 2 hours from the molasses scale tank in the Dryer House. Transfer the individual samples to a covered V. PULP DRYER CONTROL 63 container and mix thoroughly previous to analysis. Do not take any samples if molasses is not being- used. ANALYSIS Follow the "General Methods," I, 1 (b). 3. WATER FROM PRESSES Determine every 4 hours : (a) Sugar. Determine every 8 hours : (b) Dry Substance (grams in 100 ml). SAMPLING Take a catch sample of the water leaving the presses, being careful not to include water from any other source in the sample, and analyze immediately. ANALYSIS (a) Sugar: Determine as under "Pulp and Pulp "Water," Chapter II, 3. (b) Dry Substance: Mix the sample well and transfer 50 ml to a weighed porcelain evaporating dish, being careful to include a proper proportion of the suspended matter. Evaporate to dry- ness on a water bath and complete the drying in an oven at 100 105 ; about 11/2 hours in the oven is required. Multiply the weight of dry substance by 2 to obtain the percentage. 4. WATER FROM PULPEFANGER Determine every 8 hours: (a) Dry Substance (grams in 100 ml). SAMPLING Take a catch sample of the water leaving the pulpef anger, and analyze immediately. ANALYSIS (a) Dry Substance: Mix the sample and determine as under 'Water from Presses." Note: Special tests on this and other waters, to determine the amount of fine particles of pulp in suspension, may be made as follows: 64 METHODS OF ANALYSIS Determine the dry substance after nitration through paper; the difference between this and the total amount of dry substance will show the maxi- mum amount that can be removed. Determine the dry substance also after pouring the water through a sieve having the same width of open- ing as the pulpef anger screen; this will give an approximate idea of the amount that it is possible to recover under working conditions. 5. PULP ENTERING PRESSES Determine every 8 hours : (a) Moisture. SAMPLING Take a good-sized sample (several quarts) from the discharge of the separator, in such a manner as to secure as representative a sample as possible of the material discharged, using a dipper which will catch all of the accompanying water as well as the actual pulp. If it is impossible to obtain the sample at this place,, take the sample from the slide to the presses, sampling from at least two presses which are running and using care to get an average sample. Put the entire sample in a "pulp can" of the same type used for the samples of pulp from the diffusion battery, and after al- lowing it to drain for 15 minutes, or longer, weigh separately the drained pulp and water thus obtained. (The water may be meas- ured instead of weighed, if desired. ) Grind the drained pulp in an Enterprise Meat Chopper and mix it well. Save portions of the pulp and the water for analysis. ANALYSIS Weigh out 10 grams of the ground pulp in a 3x%-inch alumi- num dish, and dry at 100 105 in a glycerin oven for 6 8 hours, or for a period which has been found to be long enough to give con- stant weight. In establishing this period consider the weight con- stant when the loss after an additional heating for one hour is not over 0.1%. Check the accuracy of this period at least once a week. Evaporate 50 ml of the drained water and determine the dry substance as under " Water from Presses." Calculate the percentage of moisture in the "pulp entering presses " as a weighted average from the weights and moisture con- tent of the drained pulp and water. E. g., if 4,000 grams of drained pulp and 1,000 grams of drained water are obtained containing respectively 94.80 and 99.70% moisture, the result is (4000 X 94.80) + (1000 X 99.70) 4000 + 1000 95.8% V. PULP DRYER CONTROL 65 6. PULP LEAVING PRESSES Determine every 4 hours: (a) Moisture. SAMPLING Take a sample every hour from the discharge of the pulp con- veyor, if it is possible to secure the sample at this point without danger. Otherwise take the sample from the discharge spouts of the presses, but distribute the sampling well among all the presses in operation. Make up a composite sample every 4 hours and mix it well. ANALYSIS (a) Moisture: Weigh out 10 grams in a 3x%-inch aluminum dish, and dry at 100 105 in a glycerin oven for 6 8 hours, or for a period which has been found to be long enough to give constant weight. In establishing this period consider the weight constant when the loss after an additional heating for one hour is not over 0.1%. Check the accuracy of this period at least once a week. 7. DRIED PULP LEAVING DRYERS Determine every 3 hours for each drum separately : (a) Moisture. SAMPLING Take representative catch samples from the discharge of each drum and analyze immediately. ANALYSIS (a) Moisture: "Weigh out 10 grams in a 3x%-inch aluminum dish and dry in a vacuum oven at 100 105 for exactly 1 hour. Cool in a desiccator and weigh. Multiply the percentage loss by the factor which has been established, and report as the percentage of moisture. To control the factor make frequent tests by heating samples for 2 or 3 hours longer, and then for successive periods of one hour until the loss of weight in one hour is not over 0.1%. At the beginning of the campaign use a factor of 1.10 until a more ac- curate figure is established. 66 METHODS OF ANALYSIS 8. DRIED PULP AS SACKED Determine every 3 hours: (a) Moisture. (b) Polarization. SAMPLING Take a sample every hour from at least three bags as they are filled at the sacking station, and keep in a tight container. Mix the hourly samples to make composite samples when needed. If plain and molasses pulp are produced on the same day, save samples of each and analyze separately. Save portions of each composite sample for a weekly composite sample. ( See ' ' Weekly Analysis of Dried Pulp, "below.) ANALYSIS (a) Moisture: Weigh out 10 grams of the mixed composite sample and dry for 3 4 hours in a vacuum oven at 100 105. Cool in a desiccator and weigh. Report the percentage loss at the percentage of moisture. As the time of drying necessary to elim- inate all the moisture varies considerably, the length of the drying period should be frequently checked and regulated accordingly. (b) Polarization: Weigh out *12.6 grams, transfer to a 200.6 ml flask, add 1215 ml of basic lead acetate, and fill about three-fourths full with water. Digest exactly as in the determina- tion of sugar in cossettes, Chapter II, 1 (a). Polarize in a 400 mm tube and multiply the reading by two to obtain the percentage of sugar. 9. WEEKLY ANALYSIS OF DRIED PULP Make a weekly analysis of plain and molasses pulp separately, comprising the following determinations : (a) Moisture. (b) Crude Protein. (c) Crude Fat. (d) Crude Fiber. *This weight is figured as the equivalent of the half-normal weight after allowing 7 ml as the volume of the marc in 13 grams of Molasses Pulp containing 15 per cent sugar. Plain Pulp is so low in polarization that the same weight may be used without appreciable error. V. PULP DRYER CONTROL 67 (e) Ash. (f) Nitrogen-free Extract. SAMPLING Save 15 grams of each sample used for the analysis of " Dried Pulp as Sacked," and keep in a tight container. Save separate samples of plain and molasses pulp if both are produced during the same week. PRKI-ARATION OP SAMPLE Mix the sample well with the hands and save a portion for the determination of moisture. Crush at least 50 grams of the re- mainder in an iron *mortar, crusher, or disc pulverizer, to pass a sieve having circular openings 1 mm in diameter. (Or use a regular 20-mesh sieve.) Preserve both samples in tight containers. ANALYSIS Follow the methods in Chap. XX, ''Foods and Feeding Stuffs." Determine the moisture in duplicate in both the original and the ground material. Make all other determinations on the ground material, and correct the results for the loss of moisture during grinding. For example : Let a = percentage of moisture in original material b = percentage of moisture in ground material c = percentage of crude protein in ground material x = percentage of crude protein in original material c (100 a) Then x = . L. 100 b NOTE As the amount of crude fat in dried pulp is small and very constant, this determination may be omitted on the weekly samples, but should be made on a campaign average sample. When the crude fat is not determined, allow 0.2 for the percentage of crude fat in calculating the nitrogen-free extract. 10. TEMPERATURE DATA GENERAL Refer to the general instructions in the section of the same title in Chapter II, 36. *Flain pulp of normal moisture content can be easily ground in a disc pulverizer. Molasses pulp is best crushed in an iron mortar. 68 METHODS OF ANALYSIS MOLASSES TO PULP DRYER Obtain every 2 hours from the line leading to the drying drum. PULP ENTERING PRESSES Obtain every 2 hours the temperature of the pulp just previous to entering a press which is in operation. GAS LEAVING FURNACE Obtain from the recording pyrometer at the furnace. GAS LEAVING DRYER Obtain from the recording thermometer at the exit of the dryer. VI. PULP SILO CONTROL 1. GENERAL Sample and analyze "pulp entering silo" once a day during campaign. Sample and analyze "pulp sold" once a day (except on Sundays and holidays during intercampaign) as long as any unsold pulp is on hand, but only on days when wagons are being loaded at the silo. 2. PULP ENTERING SILO Determine : (a) Dry Substance. SAMPLING Take a good-sized sample from the discharge of the pulpe- fanger, enough to fill a ten-quart bucket three-fourths full, in such a manner as to obtain as nearly as representative a sample as pos- sible of the mixture of pulp and water discharged into the silo. Drain in a "pulp can" as in the case of "Pulp Entering Presses," Chapter V, 5, "Pulp Dryer Control." ANALYSIS Analyze as under "Pulp Entering Presses," Chapter V, 5, "Pulp Dryer Control." 3. PULP SOLD Determine : (a) Acidity. (b) Dry Substance. S \MI-IJNG Take three samples from the top of the wall of pulp where the wagons are being loaded ; take another set of three samples from 70 METHODS OF ANALYSIS the middle; and take a third set of three samples from the bottom. Mix the nine samples to form a composite sample for analysis. ANALYSIS (a) Acidity: Weigh out 10 grams of the well mixed sample, and rinse into a beaker or casserole with a little neutral, distilled water. Add a few drops of phenolphthalein and then N/28 alkali in excess, and dilute to a total volume of about 200 ml. Cover with a watch glass and boil gently for 15 minutes. Cool and titrate with N/28 acid, continuing the addition of the acid until the solu- tion remains colorless for 15 minutes. The amount of standard alkali originally added should be such that not less than 5 ml nor more than 10 ml of the standard acid is subsequently required for neutralization. Subtract the number of ml of acid from the num- ber of ml of alkali used, and divide by 100 to obtain the acidity (in terms of per cent CaO by weight). (b) Dry Substance: Weigh out 10 grams of the sample, the acidity of which has been previously determined as in (a), using a tared aluminum moisture dish provided with a cover and a small glass rod. Add 8 10 ml of water and the exact weight of freshly ignited C. P. calcium oxide indicated by the acidity test to be re- quired for neutralization. Stir with heating until a uniform mix- ture is obtained. (Add a drop of phenolphthalein to show when all the particles of pulp have come in contact with the calcium oxide ; the phenolphthalein will retain its pink color, which will be uniformly distributed when the mixing is perfect). Dry in a glycerin oven at 100 105 for 5 6 hours, and then for successive periods of one hour until the loss in weight in any period is less than 0.1%. Obtain the percentage of dry substance by the following formula : Let a = weight of pulp used b = acidity of pulp (grams of CaO in 100 ml) c = weight of dried material x == weight of CaO required y = percentage of dry substance Then x = ^- 100 (e .68 x) Andy=- Or, as a = 10, y = 10 (c .68 x) tt A cl I HI the use of Table 16. VI. PULP SILO CONTROL 71 y" can be conveniently obtained by The factor .68 in the above formulas is derived as follows: Assuming acetic acid to be the principal acid present, the acetic acid of the original material is converted to calcium acetate in the dried sample in the ratio of the molecular equivalents, i. e. of 120 to 158. Then, since the molecular equivalent of calcium oxide is 56, (158 120) -=- 56 = .68, which repre- sents the factor by which the amount of calcium oxide used must be multi- plied to obtain the deduction necessary to convert the calcium acetate back to free acetic acid. VII. BOILER HOUSE CONTROL 1. GENERAL No definite routine should be followed in the boiler house con- trol work; irregularity in the time of sampling and testing the in- dividual boilers will tend to give more nearly average results. The boiler house control man should take and prepare all the necessary coal and ash samples, make the flue gas analysis, and obtain the draft and temperature readings and any other necessary data. If a boiler house control man is not employed, the man in charge of unloading the coal should take the coal samples, and the Assistant Chemist should obtain the ash samples; the other data on flue gas analysis and temperature, draft, etc., will not be obtained except for what average figures are available from the recording instru- ments. 2. SAMPLING OF COAL Use a sampler consisting of a piece of 2-inch pipe about 4 feet long, provided with a spring valve at one end to retain the coal in the sampler. Sample all cars unloaded, just previous to un- loading, by driving the sampler through the coal in the car and collecting the coal retained in the pipe. Take 3 samples from each car, one in a corner about two feet equally distant from the sides of the car, one in the center of the car, and one in the corner diagonally opposite the position of the first sample. Preserve all the samples in a can provided with a tightly fitting cover, such as a milk can, or in a number of such containers, and keep in a cool place. Sample cars loaded from the storage pit in the same manner as cars received from the mine; if coal is hauled from the storage piles, take one sample from every fifth wagonload. Take no samples from cars loaded from the drippage pit, or from cars into which any drippage has been loaded; pay special attention to this point VII. BOILER HOUSE CONTROL 73 to avoid contaminating the regular sample with drippage. It' coal Irom different sources (mine, storage pit, etc.) is being used, in- clude in the gross sample amounts from each source in approximate proportion to the amounts from each source used. Sample the coal used in the Pulp Dryer in exactly the same manner. The sampling should be done in this case by the man who unloads the coal for the dryer but should be under the super- vision of the boiler house control man. 3. PREPARATION OF COAL SAMPLES When all the coal for a day's use has been sampled, crush the entire gross sample to Vi-inch size and reduce to 1 to 2 quarts by mixing and quartering on a large piece of canvas; do this as rap- idly as possible to avoid loss of moisture. Keep the sample in a fruit jar closed with a tightly fitting cover provided with a rubber gasket. At the end of the week grind the entire seven samples repre- senting the week's run of coal to 60-mesh size in the pebble mill described in Chap. XXIII, 9. Put up and seal a 4-oz. sample of the ground material, and forward it without delay to the central laboratory for analysis. Be careful to clean the mill thoroughly after each week's sample is prepared, and employ it exclusively for grinding coal. 4. SAMPLING OF ASHES (a) IN BOILER HOUSES EQUIPPED WITH CHAIN GRATE STOKKUS Obtain samples of grate 1 and flume ashes as follows : (1) Grate (Stoker) Ash : I'M- a sampler consisting of a rec- tangular box with hinged cover fastened to a long handle. Obtain 3 samples per shift, if possible, from the discharge of each stoker in operation, taking a sufficient quantity so that the total sample for the 8 hours will amount to about one gallon. Save separate samples for each shift for the set of boilers in charge of each fire- man. This will make 6 samples per 24 hours at the large factories and 3 at the small factories. (2) Flume Ash: Obtain the sample by holding a closely woven sack over the discharge of the flume ash line, or over the special sampler provided for this purpose, in such a manner as to obtain an average of all solid material delivered through the line. Take a sample at least twice a shift and make up a composite 74 METHODS OF ANALYSIS sample for each shift by mixing at least 1 quart of each of the in- dividual samples. (b) IN BOILER HOUSES EQUIPPED WITH HAND FIRED FURNACES Obtain samples of pan, grate, and flume ashes as follows : (1) Pan Ash: Take a small sample of the ash in the pan of each boiler in operation at least 3 times per shift ; the total sample for the shift should be about one gallon. Save separate samples for each shift. If a boiler house control man is not employed, ob- tain a 1-quart sample once a shift representing an average of the ash in the pans at the time of sampling. (2) Grate Ash: Take samples only when the fires are being pulled and before the ash is wet down. Obtain an average sample of at least 1 gallon once a shift, or oftener if a boiler house control man is employed. Crush the gross sample to break up large lumps, mix, and save a 1-quart sample representing the work of each shift. (3) Flume Ash: Obtain at least twice a shift as described in 11 (a), (2)," above. If a boiler house control man is not employed, obtain at least once a shift. (c) IN PULP DRYERS The boiler house control man or the Assistant Chemist should obtain an average sample of the grate ash at least once per shift, as described in (a) (1). 5. PREPARATION OF ASH SAMPLES Break up any large lumps by crushing, mix well, take out 1 quart and crush to 10 mesh size in a jaw crusher. Mix the crushed sample and grind at least one-fourth of it to 60 mesh size in a disc pulverizer. Mix well and save 4 ounces for analysis. As the samples of ash are analyzed on a dry basis, no care need be taken to avoid loss or gain of moisture during the prepara- tion of the sample. Any samples which are very wet, however, such as the flume ashes, should first be dried in a shallow tray in a warm place before being prepared for analysis. If the special boiler house control is carried on, the samples of ashes collected to represent the work of each shift should be analyzed separately. Otherwise a composite sample of each kind of ashes should be prepared at the end of every week and sent to the central laboratory, together with the coal sample, for analysis. See Chapter XV, 10, regarding the analysis of ash samples. VII. BOILER HOUSE CONTROL 75 6. DRAFT Take draft readings, both "furnace" and "differential," on the individual boilers at the time when samples of the grate ash are collected. Check all the draft gages at the zero point at least once a shift, and test all connections for air leaks frequently. The liquid used in Ellison and in Blouck differential draft gages is, unless otherwise specified, mineral oil of .834 specific .irravity at 60 F., colored red or blue. The best temporary substi- tute is kerosene, having nearly the same specific gravity. Water must not be used. In the absence of a boiler house control man or the necessary differential gages, no readings will be recorded. 7. FLUE GAS ANALYSIS. Immediately after the ash sample is taken and the draft read- ings are made, determine the percentage of carbon dioxide in the flue gas, using an Orsat apparatus or one of the modified forms of the same, and following the method prescribed for the analysis of lime kiln gas, Chap. II, 10. Change the caustic alkali solution every 2 days. The addition of a few drops of phenolphthalein to the water in the measuring burette will be of value to indicate contamination from the alkali solution. Rinse out the sampling pipe thoroughly before drawing gas into the apparatus. Do not make any flue gas analyses on banked boilers. The gas sampling pipe should pass through a hole drilled in the brickwork, and the open end through which the gas enters should be close to the point where the gases leave the boiler and where the velocity of the gas stream is a maximum. Leakage around the sampler should be stopped with asbestos packing. The proper position of the sampler is of great importance. It is also advisable, especially when the C0 2 is high, to make some complete analyses in which oxygen and carbon monoxide (CO) are determined. In the absence of the special boiler house control, no indi- vidual flue gas analyses will ordinarily be made. 8. TEMPERATURE OF AIR AND FLUE GAS (a) AIR ENTERING FURNACES Take readings at the time when the flue gas is analyzed, of thermometers in different parts of the boiler room hung near the 76 METHODS OF ANALYSIS point where the air enters below the stokers but not so close that they will be heated by radiation from the fire. (b) FLUE GAS If the boilers are equipped with individual thermometers 01? if a suitable pyrometer is available, determine the temperature of the flue gas at the point where it leaves the boiler at the time when the gas is analyzed. If only a general recording instrument is available, take several readings during the period of ash sampling and gas analysis, and use the average of these readings as a basis for figuring the heat loss. 9.' CALCULATION OF HEAT LOSSES (a) DATA REQUIRED (1) Moisture, Ash, and Calorific Value of Coal. On account of the fact that the results of the coal analysis are not available until several days after the samples are taken and then only for weekly samples, use the average analysis to date of the coal burned during the campaign, recalculating these averages when each new set of figures is received from the central laboratory. During the first few days of the campaign, or until figures have been received from the central laboratory, use the average coal analysis of the preceding campaign. (2) Carbon and Hydrogen in Coal. Use average figures obtained from the analyses of the Bureau of Mines. (See refer- ences in Section 10.) For northern Colorado lignite (sub-bitu : minous) coal the percentage of carbon may be taken as 57 and the percentage of hydrogen as 6, if the amount of combustible is approximately 75 per cent. (3) Other data required are obtained from the daily deter- minations. (b) Loss IN DRY FLUE GAS Obtain from the chart (^drawing S-1756 or S-132-M) the "B. T. U. lost in dry flue gas per pound of carbon burned," according to the average flue gas analysis, and the average tern- perature of the air and of the flue gas. *The Lovell factory, where natural gas is used, should employ the chart in drawing S-126-M. VII. BOILER HOUSE CONTROL 77 Let T = temperature ( F) of flue gas t = temperature ( F) of air entering furnaces B = B. T. U. found from the chart A = calorific value (B. T. U.) of the coal as fired C = % carbon in coal as fired L 1 = percentage loss of heat in dry flue gas Then Ll = _B A EXAMPLE Assume 12% C0 2 in flue gas and temperature of 500 F., boiler room temperature of 80 F., and 9000 B. T. U. in coal con- taining 57% carbon. From the chart T t = 420, and B = 2120. 57 X 2120 L, = = 0.4 9000 For coal containing 57% carbon, the calculation may be short- ened by the use of Table 17. The value found in the table multi- plied by 100 and divided by the B. T. U. in the coal gives the percentage loss desired. If the percentage of carbon in the coal is not taken as 57, the table may still be used by multiplying by C 1 a factor equal to ,where C is the percentage of carbon in the 57 coal. EXAMPLE For 12% COo and T t = 420, Table 17 gives 1208 B. T. U. Then 1208 X 1Q =13.4 9000 Note that the chart gives "B. T. U. per pound of carbon burned" and the table "B. T. U. per pound of coal burned." (c) Loss DUE TO MOISTURE The loss due to moisture is composed of: (1) Loss due to moisture in the coal as fired. (2) Loss due to moisture resulting from the *burning of the hydrogen component of the fuel. In addition to the symbols previously used, Lot M = % moisture in coal as fired H = % hydrogen in coal as fired *The Lovell factory, where natural gas is used, should calculate this loss in accordance with the chart in drawing S-153-M. 78 METHODS OF ANALYSIS w = boiling point ( F.) of water (202 for 5000 feet elevation) L 2 = percentage loss of heat due to moisture Then L 2 = M + 9 H x [( w t) + 976.6 + .47 (T w)] A EXAMPLE Assume in addition to the figures in the preceding example, 16% moisture and 6% hydrogen in the coal, and boiling point of water as 202 F. (16 + 54) X [122 + 976.6 + .47 (500 202)] jj = - _____ - _ __ y^ 9000 This calculation may be shortened as follows by the use of Tables 18 and 18 A. Let F = factor as found in Table 18. F' = factor as found in Table 18 A. FF' Then L 2 = A EXAMPLE According to the data previously given, F = 70.0 and F' = 1239 Then L, = = 9.6 9000 (d) TOTAL Loss IN FLUE GAS Let L 3 = total percentage loss of heat in flue gas Then L 3 = L, + L 2 EXAMPLE L 3 = 13.4 + 9.6 = 23.0 (e) Loss DUE TO COMBUSTIBLE IN ASH This is based on the analysis of the coal and of the grate (stoker) ashes, the combustible matter in the ashes being assumed to consist of pure carbon of a calorific value of 14600 B. T. IT. Let D = % ash in coal as fired E = % ash in ashes L 4 = percentage loss of heat due to combustible in ashes 14600 D (100 E) Then L 4 = A E VII. BOILER HOUSE CONTROL 79 14600 D Or it k =F - _ - a factor which can be used for a number A of calculations E EXAMPLE Assume the coal to contain 12% ash, and the ashes 60% ash. 14600X12X40 =13Q 9000 X 60 (f) TOTAL KNOWN LOSSES If L 5 = total known heat losses, Then L 5 =L 3 + L 4 EXAMPLE L 5 = 23.0 + 13.0 = 36.0 10. BIBLIOGRAPHY 11 Sampling 1 and Analyzing Flue Gas" Bur. Mines, Bulletin 97. "Combustion and Flue Gas Analysis" Bur. Mines, Tech. Paper 219. "Apparatus for the Exact Analysis of Flue Gas" Bur. Mines, Tech. Paper 31. "Measuring the Temperature of Gases in Boiler Settings" Bur. Mines, Bulletin 145. U. S. Geological Survey Professional Paper 48, and Bur. Mines Bulletins 22, 85, and 123 Analyses of mine and car samples of coals of the United States, 1904 1916. "Steam" Babcock & Wilcox Co., New York. VIII, POTASH CONTROL (BEET CAMPAIGN) 1. GENERAL Each factory engaged in potash recovery should send to the Central Laboratory weekly average samples of Molasses Worked, Saccharate Cake, and Total Waste Water, which should represent, in each case an average of all laboratory samples taken during the week, as described in Chapter II, 35, "Weekly Composite Sam- ples. " The samples and information, as specified in detail below, should be forwarded to the Central Laboratory as soon as possible after the end of every week, at least not later than Monday noon. (a) MOLASSES WORKED Forward 100 grams of the average sample of the molasses worked during the week. (b) SACCHARATE CAKE Forward an amount equivalent to 100 grams of dry substance, of an average sample of Saccharate Cake, representing a weighted average of the cold and hot cakes made up as in the following example : Brix of Cold Saccharate Cake 62.0 Brix of Hot Saccharate Cake 55.0 Tons of Dry Sub. in Cold Saccharate cake for Week 450 Tons of Dry Sub. in Hot Saccharate Cake for Week 60 Tons of Dry Sub. in Total Saccharate Cake for Week 510 Then the number of grams of the original material of Cold Cake to be used for the sample is 450 100 _ H23 510 .620 And the number of grams of IJot Cake is 510 .550 VIII. POTASH CONTROL (BEET CAMPAIGN) 81 The material referred to above is of course the syrup obtained after the carbonation and evaporation of the cake from the saccha- rate presses. (c) TOTAL WASTE WATER Forward 100 grains of the weekly average samples. (d) DATA REQUIRED Forward also the following data, both for the week and to date: Tons of Molasses Worked. % Sugar in Molasses Worked. Sugar in Total Waste Water, per cent on Sugar in Molasses Worked. Cubic Feet of Total Waste Water Produced. Cubic Feet of Waste Water Actually in Reservoir. Total Waste Water, Brix. Total Waste Water, Alkalinity. Total Waste Water, Sugar. 2. ANALYSIS The Central Laboratory will make the necessary analyses ac- cording to the standard methods described in Chapter IX, 12, and elsewhere in the "Methods of Analysis/' IX. POTASH CONTROL (POTASH CAMPAIGN) This chapter relates to the laboratory control work which is to be carried on during- the potash campaign at every factory engaged in potash recovery. 1. LIQUOR ENTERING FACTORY Determine every 4 hours : (a) Brix. (b) Alkalinity. (c) Sugar. SAMPLING Take a catch sample every 4 hours from the line from the reservoir to the factory before the liquor has passed through any heater. ANALYSIS Determine as in the case of Steffen Waste Water, Chap. IV, 6. 2. FIRST SATURATION LIQUOR Determine every hour : (a) Alkalinity. SAMPLING Take) a cateh sample from the cocks or troughs of the first presses, avoiding any admixture of wash water. ANALYSIS Determine the alkalinity in the regular manner with N/28 acid. NOTE : If double carbonation is not employed, this determina- tion is necessarily omitted. IX. POTASH CONTROL ( POTASH CAMPAIGN) 83 3. THIN LIQUOR ENTERING EVAPORATORS Determine every 4 hours: (a) Brix. Determine every hour: (b) Alkalinity. (c) Reaction with CO 2 . SAMPLING Take a catch sample from the pump, or at a suitable point in the line between the filters and the evaporators. ANALYSIS (a) Brix: Determine in the regular manner. (b) Alkalinity: Determine as in the case of; " First Satura- tion Liquor." (c) Reaction with C0 2 : Pass carbon dioxide gas for a few minutes through a portion of the sample in a 1 x 6 inch test tube. If any cloudiness results, report as "P" indicating the formation of a precipitate, and if no cloudiness appears report as "0." 4. EVAPORATOR THICK LIQUOR PRODUCED Determine every 4 hours: (a) Brix. Determine every 24 hours : (b) Sugar. SAMPLING Take a sample from the pump, or from the line to the potash scale tank. Do not take the sample from the last body of the evaporators or from the scale tank. Take a sample each time when liquor is let out of the evaporators, and composite equal portions of the individual samples. ANALYSIS (a) Brix: Follow the "General Methods," 1 (a). (b) Sugar: Transfer 13 grams to a 100 ml flask, add a few drops of phenolphthalein, and neutralize with dilute acetic acid. 84 METHODS OF ANALYSIS Add 4 6 ml of basic lead acetate, make up to the mark, filter, and polarize in a 200 mm tube. Multiply the reading by 2. 5. FILTER PRESS CAKE Determine every 8 hours : (a) Weight per cake. SAMPLING Take a representative sample at least every 8 hours in the manner described in Chap. II, 13, "Lime Cake." Save equal por- tions for the weekly composite sample described below. DETERMINATION Determine the average weight of one cake in pounds once a shift by catching and weighing two or three cakes taken at random. In the case of Kelly presses the amount of cake is best calculated from the difference in alkalinity between the original and car- bonated liquor and the CaO content of the cake. 6. CONDENSED WATERS Examine, by the *alpha-naphthol test, the boiler feed water every hour, and the press wash and evaporator tail pipe waters every 2 hours. Test also the drips from each evaporator body as frequently as practicable. See Chap. XVII, 2 (c) regarding the collection of campaign samples for analysis. 7. BOILER WATER Determine every 8 hours on each boiler in service : (a) Alkalinity. SAMPLING Draw from the sampling line, first allowing the water to run a few moments to rinse out the pipe. ANALYSIS Measure out 10 ml with a pipette into a porcelain dish and follow the "General Methods," I, 10 (a), using phenolphthalein 'See Chapter I, 13. IX. POTASH CONTROL ( POTASH CAMPAIGN) 85 as indicator. Dilute with sufficient neutral water to make the coloi reaction distinct. 8. CAEBONATION GAS Determine every 4 hours: (a) C0 2 . SAMPLING AND ANALYSIS Obtain the sample and determine the percentage of C0 2 as described in* Chap. II, 10, "Lime Kiln Gas. ? ? 9. EVAPORATOR THICK LIQUOR ENTERING FURNACE Determine every 2 hours: (a) Brix. I )rt ermine every 24 hour- : (b) Dry Substance. (c) Lixiviated Ash. SAMPLING Take a sample every 2 hours from the line leading from the storage tank to the furnace. Make up a composite sample for the dry substance and ash determinations. ANALYSIS Follow the "General Methods." 10. CRUDE ASH AS SACKED Determine every 24 hours: (a) Acid Insoluble. (b) Lixiviated Ash. SAM i 'LING The man at the sacking station should take a small measureful from each bag filled and transfer it to a covered container. A laboratory employe should mix the gross sample well and transfer a suitable amount to a tightly stoppered bottle. If the material is shipped as fast as it is sacked, this sampling 'an be combined with the collection of samples representing each ear-load lot described in Chapter X. 86 METHODS OF ANALYSIS ANALYSIS (a) Acid Insoluble and (b) Lixiviated Ash: Follow the methods given under "Crude Potash," Chap. X, 6 and 8. 11. TEMPERATURE DATA Take readings every 2 hours of the thermometers indicating the temperature of the liquor entering and leaving each set of heaters; record also the kind of steam or vapor used in each case. Take readings also every 2 hours of the temperature of the liquor in each body of the evaporators. 12. WEEKLY COMPOSITE SAMPLES SAMPLING Make up a composite sample of each of the products mentioned below by taking equal portions of each sample brought to the lab- oratory during the week and preserving in a sealed jar or stoppered bottle. (a) LIQUOR ENTERING FACTORY Determine dry substance (after carbonation) and K 2 0. (b) THIN LIQUOR ENTERING EVAPORATORS Determine dry substance and K 2 0. (c) FILTER PRESS CAKE Determine dry substance and K 2 0. (d) EVAPORATOR THICK LIQUOR PRODUCED Determine dry substance, lixiviated ash, K 2 0, and NH 3 . (e) CRUDE ASH AS SACKED Determine lixiviated ash, K 2 0, and NH 3 . ANALYSIS (1) Dry Substance: Determine in uncarbonated liquors (waste water entering factory) as follows: Transfer 50 ml to a 100 ml flask and carbonate at 80 to faint alkalinity with phenolph- thalein. Heat .to at least 85, cool, and make up to the 100 ml mark. Mix and filter through a dry filter. Determine the dry substance in the filtrate by drying on sand according to the ' ' Gen- eral Methods, ' ' Chap. I, 2. Double the percentage found to obtain the percentage in the original liquor. IX. POTASH CONTROL ( POTASH CAMPAIGN) 87 Determine in "thin liquor entering evaporators" and in thick liquor by drying on sand without preliminary carbonation. Determine in filter press cake by drying 10 grams directly as in the case of Saccharate Cake, Chap. IV, 11 (g). (2) Lixiviated Ash: Follow the "General Methods," I, 7 (b). (3) Potash (K 2 0): Directions for the determination in crude ash will be found in Chap. X, 9. In the case of liquors and filter press cake proceed as follows: \\Vifrh out a suitable amount (20 grams of thin liquors, 1 gram of thick liquor, and 10 grams of filter press cake) in a platinum dish, add a little water and 1 ml of sulphuric acid (1 to 1). Evapo- rate on a water bath and heat cautiously on a *Hillebrand radiator until the sulphuric acid is expelled. Then ignite at a dull red heat until the ash is white. Add a little strong hydrochloric acid, warm slightly in order to loosen the mass from the dish, and dissolve in about 25 ml of water. Add a slight excess of ammonium hydroxide, heat to boiling, and add sufficient ammonium oxalate to precipitate all the lime present. After standing for at least one-half hour, filter, and wash well with hot water. Then proceed as in the determination of potash in crude ash, Chap. X, 9. (4) Nitrogen as Ammonia (NH Z ): Determine the total nitrogen as in the analysis of crude potash, Chap. X, 10. 13. STEAM CALCULATION Calculate a heat balance every week. The manner of calcu- lating- the heat units in the steam theoretically required can best be explained by the following example, which is based on 100 kilo- grams of waste water entering the factory. The value of the latmt heat of steam is taken as 540 calories per kilogram or 971 B. T. U. per pound. Live or 1st 2nd Exhaust Vapor Vapor HKATKRS BEFORE CARBONATIOX to 100 kg of liquor heated from 10 (80-10) *See Chap. XXIII, 15. 88 METHODS OF ANALYSIS HEATERS AFTER CARBONATION OR AT CARBONATION Live or 1st 2nd Exhaust Vapor Vapor 100 kg of liquor heated from 75 to 90 10 (90 75) _ 540 HEATERS BETWEEN PRESSES AND EVAPORATORS Quantity = Weight of liquor plus weight of wash water minus (lime cake minus C0 2 ) ==103' kg. 103 kg of liquor heated from 85 to 105 103 (105 85) : _ = 3.8 kg 1st vapor. 3.8 540 HEATING IN EVAPORATORS 103 kg of liquor heated in 1st body from 105 to 110 103 (110 105) 1 L = 1.0 kg exhaust 1.0 540 Totals 1.0 6.6 13.0 EVAPORATION Assume that, according to actual scale weights, 6.0 kg of thick liquor has been produced per 100 kg of thin liquor introduced. Then kg of water evaporated = 103 6.0 = 97.0 Another method by which the amount of evaporation may be calculated is from the percentage of dry substance in the thin and thick liquors. STEAM CONSUMPTION kg of Steam 97.0 total kg of water evaporated 6.6 kg evaporated single effect 6.6 90.4 26.0 kg evaporated double effect (2 X 13.0) 13.0 64.4 kg evaporated quintuple effect 12.9 32.5 Live or exhaust steam used for heating 1.0 Total Steam Required 33.5 IX. POTASH CONTROL ( POTASH CAMPAIGN) 89 The total strain theoretically required is then 33.5 kg per 100 kg of thin liquor, or 33.5 tons per 100 tons of thin liquor intro- duced. Now let A = tons of thin liquor introduced. B = tons of steam required per 100 tons of thin liquor (33.5 in the above example). C = tons of coal burned. D = calorific value (B. T. U. per Ib.) of coal burned. X = B. T. U. theoretically required. Y = B. T. U. in coal burned. Then tons of steam required is - 100 And X = _^? . X 2000 X 971 = 19420 AB 100 where 971 is the latent heat of steam in B. T. U. per pound, Also Y = 2000 CD. The ratio of X to Y is then a measure of the combined effi- ciency of the boiler house and the heat utilization. X. CRUDE POTASH 1. SAMPLING Take a large sample representing each car of crude ash shipped. If the potash is shipped at the time when it is sacked, obtain the sample by taking a small measureful from each sack before it is sewed, until the number of sacks required to load the car has been filled. A suitable measure can be made by riveting a handle on a 20 ml sheet iron crucible, or a tin measure of similar size (38 x 32 mm) may be used. If the potash is not shipped at the time when it is sacked, obtain the sample at the time of shipment by drawing a sample from each bag by means of a suitable trier, preferably of the "In- diana type." The latter consists of two telescoping, slotted brass tubes terminating in a solid, pointed end. This enables the sampler to be inserted full length into the bag before any material can enter the sample chamber. The latter is then opened and the sample is allowed to flow in, whereupon the sampler is closed and then withdrawn, so that, a complete core of the entire bag is re- moved. The sampler should be about 18 inches long, or long enough to extend all the way through the bag. Transfer the samples, as they are taken, in every case to a covered container, and employ every possible precaution to pre- vent unnecessary exposure to the air. 2. PREPARATION OF SAMPLES (a) GENERAL METHOD Reduce the gross sample to two portions of about 2 pounds each by means of a riffle sampler. Save one of these portions for the screen test. Reduce the other portion further, and put up three 4 ounce samples and seal them immediately, as described X. CRUDE POTASH 91 below. Handle the sample as rapidly as possible throughout in order to prevent absorption of moisture. See section 3* regarding the further preparation of the sample for analysis. (b) OPTIONAL, METHOD This method may be used only for crude ash consigned within the company for refining or other purposes, and not for fertilizer material sold to other concerns. Proceed as in (a) up to the point where the sample is reduced to two portions of about 2 pounds each. Save one of these for the screen test, as before, but grind the other portion, the full 2 pounds, in a porcelain *pebble mill for two hours, or sufficiently long to reduce it to 60 mesh size. After grinding, open the mill and put up immediately the three samples described below. (c) DESCRIPTION OP SAMPLES Put up three samples for each car, labeled with the name of the factory, the name and address of the consignee, the car number, the weight of material, and the date of shipment. Designate them respectively "Seller's No. 1," "Seller's No. 2," and "Seller's No. 3." Save an additional sample of the unground material for the screen test, as previously described. Use "Seller's No. 1" sample for the local laboratory analysis, and seal and save for future reference the portion of this sample left over from the analysis. Hold the other two seller's samples subject to the receipt of instructions. Do not destroy or break the seals of any of the Seller's No. 2 or No. 3 samples without authori- zation from the General Office. As the container for Seller's No. 2 and No. 3 samples, use a seamless tin salve box of four ounces capacity, provided with a slip cover, also seamless. Immediately after filling seal with a double layer of adhesive tape, to exclude moisture, and impregnate the tape with at least two coats of paraffin by rotating the box with the edge immersed in melted paraffin; allow each coat to cool and harden before applying the next coat which is used to close the blowholes in the previous coat. Attach a wax seal also as a guarantee against tampering. The container for Seller's No. 1 sample may be: (1) A seamless tin box sealed with tape and paraffin as described above. *The mill should be of the size which has a jar 8.75 x 9.65 inches (outside) rotating at the rate of 60-75 R. P. M. 92 METHODS OF ANALYSIS (2) A glass bottle with ground glass stopper, sealed with at least two coats of paraffin. (3) A glass bottle with a flat cork stopper, inserted so that the top of the stopper is at least % inch below the top of the neck of the bottle, and covered with at least two coats of paraffin. 3. PREPARATION OF SAMPLE FOR ANALYSIS If the sample has been prepared as in 2 (b), no further prepa- ration is required before analysis. Otherwise prepare the sample for analysis by putting the entire sample through a sieve having circular openings 1 mm in diameter, grinding in a mortar the portion remaining on the sieve until all the particles pass through. Grind and sift as rapidly as possible to prevent absorption of moisture, and avoid exposing any of the material unnecessarily to the air. 4. ANALYSIS (GENERAL) Make the following determinations for each carload shipped : moisture, acid insoluble, lixiviated ash,, potash, ammonia, and screen test. Make complete analysis of a composite sample repre- senting the entire season's production. Use due care in weighing on account of the hygroscopic nature of the material. Weigh in covered dishes or watch glasses, or from a weighing bottle, and as a rule make no effort to secure an even fraction or multiple of a gram. 5. MOISTURE Weigh out approximately 2 grams in a covered aluminum " moisture dish." Heat for about 5 hours at 130 C., cool in a desiccator and weigh. Repeat the heating for one hour periods until the loss of weight is not over 0.2%. Consider the loss in weight to represent the moisture. 6. ACID INSOLUBLE. Weigh out approximately 1 gram, transfer to a 250 ml beaker, and add 150 ml of water and 15 ml of concentrated hydrochloric acid. Keep the beaker covered with a watch glass during the addition of the acid and add the acid slowly. Digest on a hot plate for 3045 minutes. Filter through a tared filter or Gooch crucible X. CRUDE POTASH 93 which has previously been washed with water and dried to constant weight. Wash with hot water, and dry to constant weight at 100105. 7. WATER INSOLUBLE Determine as in "6," adding water but no hydrochloric acid. 8. LIXIVIATED ASH Weigh out approximately 1 gram and transfer to a platinum dish. Heat to a dull redness to carbonize any organic matter present, then cool, extract with water, etc., following the procedure given in the "General Methods, " Chap. I, 7 (b), and observing all the precautions there prescribed. 9. POTASH (*Lindo-Gladding Method) REAGENTS (a) Ammonium Chloride Solution: Dissolve 100 grams of ammonium chloride in 500 ml of water, add 5 10 grams of pulver- ized potassium-platinic chloride, and shake at intervals for 6 8 hours. Allow the mixture to settle over night and filter. The residue may be used for the preparation of a fresh supply. (b) Platinum Solution: A platinic chloride solution contain- ing the equivalent of 1 gram of metallic platinum (2.65 grams of H 2 PtCl 6 .6H 2 0) in every 10 ml. (Note that the salt sold commer- cially as "platinic chloride" has the formula H 2 PtCl 6 .6H 2 0). (c) 80% Alcohol: Grain alcohol of sp. gr. 0.8645 at C. DETERMINATION Boil 5 grams of the sample with 300 ml of water for thirty minutes. Add to the hot solution a slight excess of ammonium hydroxide and then sufficient ammonium oxalate (1 or 2 ml) to precipitate all the lime present. After standing for one-half hour, cool, make up to a volume of 500 ml, mix, and pass through a dry filter. Evaporate |25 ml of the filtrate nearly to dryness, add *The method is, with a few additions and modifications, that of the Association of Official Agricultural Chemists. tThe pipette and flask used should be carefully standardized against each other. 94 METHODS OP ANALYSIS 1 ml of dilute sulphuric acid (1 to 1), and evaporate to dryness on a water bath. Finish the evaporation on a, *Hillebrand radiator and ignite until all ammonium salts are expelled. Maintain a full red heat until the residue is perfectly white. Dissolve the residue in hot water, using at least 20 ml for each decigram of potassium oxide present. Filter if there is any insoluble residue. Add a few drops of hydrochloric acid, and platinum solution in excess (5 ml). Evaporate on a water bath to a thick paste. Treat the residue with 80% alcohol, avoiding exposure to ammonia. Filter through a Gooch crucible which has been previously washed with 80% alcohol and dried to constant weight. Wash the pre- cipitate thoroughly with 80% alcohol both by decantation and on the filter, continuing the washing after the filtrate is colorless. Then wash with 10 ml of the ammonium chloride solution to remove impurities from the precipitate and repeat 5 or 6 times. Wash again thoroughly with 80% alcohol, dry the precipitate for 30 minutes at 100 C., cool in a desiccator, and weigh. Repeat the drying until constant weight is attained. The precipitate should be perfectly soluble in water. Use the factor .1938 to con- vert K 2 PtCl 6 to K 2 0. GOOCH CRUCIBLES The ignited asbestos for the felt is f prepared as follows : Cut long-fibered crysolite asbestos across the fibres into pieces 3/16 inch long, and ignite in a crucible or dish at a low red heat for at least 30 minutes. When cool, transfer to a porcelain mortar and mace- rate to a pulp with, strong hydrochloric acid. Dilute this paste with a large amount of water, pour into a tall beaker, and allow to settle until the fibrous mass collects at the bottom, leaving the fine, milky silt in suspension. Remove all of this fine, milky mate- rial by repeated washing and decantation until the wash water becomes practically clear. Asbestos prepared in this manner makes a felt that filters rapidly. Preserve in water in a stoppered bottle. Form the filter by pouring enough of the suspended asbestos into the crucible to form a layer 1/16 inch thick when drawn down by suction. Exactly the right amount must be learned by experience. A properly prepared felt will filter rapidly and yet retain the finest precipitate. Before commencing a filtration, moisten the dry filter with a little 80% alcohol. *Chap. XXIII, 15. fBureau of Mines, Technical Paper 212, p. 13. X. CRUDE POTASH 95 10. TOTAL NITROGEN AS AMMONIA Determine total nitrogen by the Kjeldahl or Gunning method, both modified to include the nitrogen of nitrates. Calculate the nitrogen as ammonia (NH 3 ). The Gunning 1 Modified Method is as follows : REAGENTS For ordinary work N/2 acid is recommended. For work in determining very small amounts of nitrogen N/10 acid is recom- mended. In titrating mineral acids against ammonium hydroxide solution use cochineal or methyl red as indicator. (a) Standard Sulphuric Acid: Determine the absolute strength of the acid by precipitation with barium chloride solution as follows: Dilute a measured quantity of the acid to be stand- ardized to approximately 100 ml, heat to boiling and add drop by drop a 10% solution of barium chloride until no further pre- cipitation occurs. Continue the boiling for about 5 minutes, allow to stand for 5 hours or longer in a warm place, pour the superna- tant liquid on a tared Gooch or on an ashless filter, treat the pre- cipitate with 25 30 ml of boiling water, transfer to the filter and wash with boiling water until the filtrate is free from chlorine. Dry, ignite over a Bunsen burner and weigh as barium sulphate. See also Chap. XXV, 21 (a) (3). A normal solution of sulphuric acid has the following equivalents : 1 ml = .04904 gram H 2 S0 4 1 ml = .01401 gram N 1 ml = .01703 gram NH 3 (b) Standard Alkali Solution: Accurately determine the strength of this solution by titration against the standard acid. N/10 solution is recommend. (c) Sulphuric Acid: Of sp. gr. 1.84 and free from nitrates and ammonium sulphate. (d) Sodium Hydroxide Solution: A saturated solution, free from nitrates. (e) Cochineal Solution: Digest, with frequent agitation, 3 grams of pulverized cochineal in a mixture of 50 ml of strong alcohol and 200 ml of water for 1 or 2 days at ordinary tempera- ture, and then filter. *Methods of Anal, of the Assoc. of Off. Agric. Chemists. 96 METHODS OF ANALYSIS (f) Methyl Red Solution: Dissolve 1 gram of methyl red (dimethyl-amino-azo-benzene-ortho-carbonic acid) in 100 ml of 95% alcohol. (g) Potassium Sulphate: Pulverized. (h) Sodium Thio sulphate. (i) Commercial Salicylic Acid. APPARATUS (a) Kjeldahl Flasks for both Digestion and Distillation: Total capacity of about 550 ml, made of hard, moderately thick, and well-annealed glass. (b) Distillation Flasks: For distillation any suitable flask of about 550 ml capacity may be used. It is fitted with a rubber stopper through which passes the lower end of a Kjeldahl con- necting bulb to prevent sodium hydroxide being carried over me- chanically during distillation. The bulb should be about 3 cm in diameter, and the tubes should be of the same diameter as the condenser tube with which the upper end of the bulb tube is con- nected by means of rubber tubing. DETERMINATION Place 0.7 3.5 grams, according to the nitrogen content, of the substance to be analyzed in a digestion flask. Add 30 35 ml of salicylic acid mixture (30 ml of sulphuric acid to 1 gram of sali- cylic acid) ; shake until thoroughly mixed, and allow to stand for at least 30 minutes with frequent shaking. Add 5 grams of sodium thiosulphatel and heat the solution for 5 minutes; cool; add 10 grams of potassium sulphate and heat very gently until foaming ceases, then strongly until nearly colorless. Do not add either potassium permanganate or potassium sulphide. After cooling dilute with about 200 ml of water. Next add sufficient sodium hydroxide solution to make the reaction strongly alkaline (50 ml is usually enough), pouring it down the side of the flask so that it does not mix at once with the acid solution. Before neutralizing it is convenient to add a few drops of phe- nolphthalein indicator or a piece of litmus paper. The pink color given by phenolphthalein indicating an alkaline reaction is, how- ever, destroyed by a considerable excess of strong fixed alkali. Connect the flask immediately with the condenser, mix the contents by shaking, distil into a measured quantity of the stand- ard acid until all ammonia has passed over, and titrate with the X. CRUDE POTASH 97 standard alkali. The first 150 ml of the distillate will generally contain all the ammonia. BLANKS Previous to use the reagents should be tested by blank experi- ments, and correction made if found necessary. 11. SCREEN TEST Weigh out 500 grams and determine the percentage retained by a 12 and 20 mesh sieve, and the percentage finer than 20 mesh. Determine the percentage of the finest fraction by subtracting from 100.0 the sum of the percentages of the other fractions. Vary this test, if necessary, to suit the specifications of each sale contract. 12. COMPLETE ANALYSIS The constituents usually reported are moisture, acid insoluble, potassium chloride, potassium sulphate, potassium sulphide, potas- sium carbonate and sodium carbonate. Directions for moisture, acid insoluble, and potash have previously been given. The fol- lowing additional determinations are required. (1) TOTAL ALKALI AS C0 2 Extract a weighed amount with hot, neutral water, filter and wash. To the filtrate add a few drops of phenolphthalein and an excess of standard sulphuric acid. Boil until all of the carbon dioxide has been expelled, then titrate back with standard sodium hydroxide. (2) CHLORINE (*Volhard Method) REAGENTS (a) N/10 or N/20 silver nitrate. (b) N/10 or N/20 ammonium or potassium sulphocyanate. (c) Ferric Indicator: A saturated solution of ferric alum (ferric ammonium sulphate). (d) Nitric Acid: Free from lower oxides of nitrogen, se- cured by diluting the usual pure acid with about % part of water, and boiling till perfectly colorless. *Methods of Anal, of the Assoc. of Off. Agric. Chemists. 98 METHODS OP ANALYSIS STANDARDIZATION Standardize the silver nitrate solution by titrating in the presence of nitric acid against weighed amounts of freshly ignited C. P. sodium chloride (finely powdered and heated for five min- utes, not quite to redness) or a standard solution of the same. Standardize the sulphocyanate solution by titrating against the silver nitrate solution. Make the titrations as described below under * ' Determination. ' ' DETERMINATION Extract a weighed amount of the sample with 50 ml of water in a 200 ml beaker. Add 5 ml of colorless nitric acid of 1.42 sp. gr., heat, filter, and wash with hot water. Add about 2 ml of the ferric indicator to 1 the filtrate. Then add a few drops of the sulpho- cyanate solution from a burette, noting the quantity. Titrate with the silver nitrate solution, adding it drop by drop and stirring constantly, to decolorization. Add about 0.5 ml more of the silver nitrate solution, filter off the silver chloride, and wash thoroughly with hot water. Titrate the combined filtrate and washings to a permanent pink color with the sulphocyanate solution. Find the amount of chlorine by difference from the total amounts of the silver nitrate and sulphocyanate solutions used. (3) SULPHURIC ACID Dissolve 1 gram of the sample in about 100 ml of water and 5 ml of concentrated hydrochloric acid, in a flask in an atmosphere of carbon dioxide. Boil the hydrochloric acid solution, main- taining the atmosphere of carbon dioxide, until any hydrogen sulphide evolved is completely expelled. Filter and wash well with hot water. Add drop by drop to the boiling solution an excess of hot 10% barium chloride solution. After standing over night, filter, wash free from chlorine with hot water, ignite, and weigh as barium sulphate (BaS0 4 ). Add a drop of sulphuric and hydrofluoric acids before finishing the ignition; this will remove any silica, if present, and convert any reduced barium sulphide back to sulphate. Multiply the weight of BaS0 4 by .7465 to con- vert to K 2 S0 4 . (4) HYDROSULPHURIC ACID Digest 1 gram of the sample with about 100 ml of water, and 20 ml of bromine water to oxidize sulphides. Acidify with hydro- X. CRUDE POTASH 99 chloric acid, and boil to complete solution and expel the excess of bromine. Filter, wash, and precipitate the sulphate sulphur in the filtrate with barium chloride as in (3). From the total sulphur thus determined, expressed as "% K 2 S0 4 ", subtract the percent- age of K,S0 4 found in (3), and multiply the difference by .6327 to obtain the percentage of potassium sulphide (K 2 S). (5) HYPOTHETICAL COMBINATIONS Calculate all of the chlorine, sulphuric acid, and hydrosul- phuric acid as potassium chloride, potassium sulphate, and potas- sium sulphide respectively. Calculate the remaining potassium as potassium carbonate. Subtract the C0 2 in the potassium carbon- ate from the " total alkali as C0 2 ", and figure the remaining C0 2 as sodium carbonate. XI. MOLASSES This chapter relates to the sampling and testing of molasses in storage and of molasses shipments. Methods relating to molasses in connection with the factory process or the Steffen process will be found in an appropriate place. 1. STEFFEN MOLASSES BOUGHT OR SOLD Determine on every car on the top sample : (a) Brix. Determine on every car on the average sample: (b) Brix. (c) Polarization. (d) Apparent Purity. SAMPLING Obtain a continuous sample through a small tap in the pipe line while each car is being loaded or unloaded. After the car is loaded, or before it is unloaded, take another sample from the top of the car. ANALYSIS (a) and (b) Brix: Determine by the double dilution method, I, 1 (b). (c) Polarization: Weigh out the half -normal weight and determine the sugar by direct polarization as in Chap. I, 3 (a). (d) Apparent Purity: Follow the "General Methods," I, 4. 2. DISCARD MOLASSES BOUGHT OR SOLD Determine on every car on the top sample : (a) Baume at 100 F. XI. MOLASSES 101 Determine on every car on the average sample : (b) Baume at 100 F. (c) Polarization. SAMPLING Sample in the same manner as Steffen molasses. ANALYSIS (a) and (b) Baume at 100 F.: Transfer approximately one quart of the molasses to a copper vessel about 6 inches in diam- eter by 8 inches high. Immerse the vessel for one hour in a * water bath to such an extent that the level of the molasses in the vessel is below that of the water in the bath, and keep the water at a gentle boil, or within a few degrees of the boiling point, for one hour. Remove any foam, fill a glass cylinder carefully with the molasses, and insert a thermometer. Allow the molasses to cool, with occasional stirring. When the temperature has fallen to almost 100 F. (38 C.), insert a Baume hydrometer standardized as described in Chap. XXIV, 3 (d), and take the reading at exactly 100 F. Be sure that the hydrometer has come to rest before the reading is made. (c) Polarization: Determine as in the case of Steffen molasses. 3. MOLASSES IN STORAGE SAMPLING Sample each molasses storage tank once a week, securing one sample from the top and, if possible, another from the bottom. If the top layer contains little or no foam, secure the sample by dipping three inches beneath the surface with an ordinary sample bucket. If foam is present, use a suitable sampling device by means of which a sample of the molasses immediately beneath the foam may be obtained. If the top sample shows a density of less than 42 Baume, take additional samples at gradually increas- ing depths to determine the extent of this condition. Secure the bottom sample from the pump or pipe line, or from a cock located near the bottom of the tank. ANALYSIS Determine the "Baume at 100 F." on each sample according to the method described under "2. Discard Molasses Bought or Sold." *This is for the purpose of removing air bubbles, and under the con* ditions and time of heating specified the amount of evaporation has been found to be unimportant. XII. BEET LABORATORY TESTS 1. GENERAL The purpose of the beet laboratory tests is to determine the quality of the beets during the latter part of the growing season and at the time of delivery during the harvest season. Determine on each sample: (a) Sugar by Cold Water Digestion. Determine as often as required: (b) Sugar by Hot Water Digestion. (c) Apparent Purity. As beets are subject to both evaporation and deterioration on standing, the samples should be worked up as soon after receipt as possible and should not be allowed to accumulate. 2. PREPARATION OF SAMPLE As each sample of beets is brought to the beet laboratory in a sack composed of such material as will best prevent evaporation, the sample should not be removed from the sack until shortly before it is to be analyzed. The samples should be cleaned, if necessary, and freed from dirt with a wire brush or other suitable apparatus, avoiding as much as possible injury to the outside sur- face. Delivery samples will have been previously tared and will require no cleaning at the beet laboratory. Field samples, and sometimes " piled" samples, will require cleaning. If a record of the average weight is desired, count and weigh the beets constituting the sample, and enter the data on the en- velope or ticket accompanying the sample. Reduce a segment of each beet of the sample to a fine pulp by passing the beet through the Keil-Dolle rasp. A conical rasp, such as the Keil disc, has been found by us by careful tests to XH. BEET LABORATORY TESTS 103 take, in the long run, an average sample of the entire beet, but the accuracy of the sample obtained is dependent on the observa- tion of the following points. (a) Place the beet in position firmly, and so that the edge of the wedge shaped segment removed coincides with the axis of the beet. (b) Take the segment from the first beet at the smaller diameter, that from the second beet at the larger diam- eter, or vice versa, and so on alternately with the re- maining beets of the sample. (c) See that all the beets in each sample are rasped and that the disc and pan are properly cleaned between samples. The reliability of the cold water digestion method in giving the correct percentage of sugar depends on the fineness of the pulp, as too coarse pulp will give low results because of incomplete extraction of the sugar. The production of sufficiently fine pulp is dependent on the observation of the following points. (d) Push each beet through the rasp at a slow, uniform rate of speed which has been found by experience to give pulp of the proper fineness. The operator should never be allowed to force the beet so violently against the disc as to retard its rotation momentarily. (e) See that the rasp is always up to the required speed of 600 revolutions per minute. (f) Keep the rasp in proper mechanical condition, as de- scribed under section 3, "Care of the Rasp." When all of the beets of the sample have been rasped, clean the disc by the momentary application of a fiber brush to each side. Transfer the pulp to a 10 inch, round bottomed, enameled mixing bowl by means of a metal or rubber spatula which fits the rasp pan closely. Cover the bowl if the balance man is not ready to handle the sample immediately. 3. CARE OF THE RASP The disc must be mounted on the shaft so that the edge will run true without oscillation. New discs should be tested to see that they are true, as otherwise it will be impossible to mount them properly. The disc should rotate at the rate of 600 700 revolutions per minute. 104 METHODS OF ANALYSIS The ease of rasping is dependent on the sharpness of the teeth, but the fineness of the pulp is dependent on an even contour of the edges of the teeth. If a rasp is found to give too coarse pulp, the disc should be faced by holding a file or carborundum stone against both the sides and the edge of the rotating disc. Very often this procedure can be improved upon by first going over the disc and filing down all teeth which project perceptibly above the general contour; large side teeth close to the edge of the rasp are particu- larly objectionable and should be reduced by filing. After this treatment very little facing will usually be necessary to put the rasp into such condition that it will produce pulp of the proper fineness. The facing should be done gradually and the character of the pulp tested by comparative cold and hot water digestion, until a point is reached where the rasp yields fine pulp, but is still sufficiently sharp so that the beets may be ground without undue effort. New discs will commonly require facing before the pulp is satisfactory. The quality of the pulp can be judged only ap- proximately, by observation and must be determined by the average difference between series of comparative hot and cold water diges- tion tests. This difference should be less than 0.1 per cent on the weight of the beets, and, if it exceeds this figure, the rasp should be given attention. When the disc becomes dull, the edge teeth should be shar- pened with a cant file, care being taken to keep the teeth of as uniform size and even contour as possible. The edge should then be faced lightly, if necessary, as previously described. As the edge becomes wider from wearing down, it will be found increasingly difficult to obtain fine pulp, until a point is eventually reached where the disc will have to be discarded. A scale of calcium oxalate frequently deposits on the disc, especially when immature beets are being rasped. As this forms a polished surface, its presence is easily overlooked. It has the effect of filling up the interstices between the teeth and thereby making the rasp dull. This scale can be removed mechanically, or very readily by immersing the disc in strong nitric acid diluted with an equal volume of water. The scale formation will be lessened if the disc is washed with hot water whenever the rasp is shut down for any length of time. The rasp pan should not be allowed to come into contact with the rotating disc when it is removed after the grinding of each sample. For the same reason fiber brushes are preferable to wire brushes for cleaning the discs between samples. XII. BEET LABORATORY TESTS 105 At the end of every day the rasp should be thoroughly washed and scrubbed, and then dried well. 4. DETERMINATION OF SUGAR BY COLD WATER DIGESTION SPECIAL APPARATUS (a) A pulp balance of suitable capacity and sensibility. (b) A sufficient number of Monel metal capsules about 3 inches high by 3 inches in diameter, all adjusted to the same tare. (c) Automatic pipettes which have been carefully standard- ized to deliver 177 ml, as described in Chap. XXIV, 2 (d). (d) Aluminum discs with a round hole in the middle, pro- vided with rubber envelopes, to serve as capsule covers. SPECIAL REAGENT (a) Dilute lead acetate: Mix one part of basic lead acetate solution of standard strength (55 Brix) with 30 parts of water. The milky solution may be used without being allowed to settle. DETERMINATION Mix the sample of fine pulp thoroughly with a spoon or spatula, or by other suitable means. Weigh out 26 grams in a clean, dry capsule, discarding any fragments of skin, rootlets, etc., which may be occasionally discovered. Weigh the pulp within an accuracy of 20 milligrams, and do not waste time in attempting to weigh any more closely. Add 177 ml of the dilute lead acetate solution from the automatic pipette, cover, and shake vigorously for a few seconds. Let the covered capsule stand for at least 20 minutos, again shake vigorously, remove the cover, filter, and polarize in a 400 mm continuous tube. The reading gives directly the percentage of sugar. Check the zero point of the polariscope at least four times a day, check the tare of the capsules once a day, and check the normal weight frequently. Check the thoroughness of the mixing occasionally by making sugar determinations on several samples taken at random from different parts of the same bowl of pulp. 106 METHODS OF ANALYSIS 5. DETERMINATION OF SUGAR BY HOT WATER DIGESTION Check the accuracy of the cold water digestion tests by making hot water digestions on some of the regular samples of pulp. In general aim to check about 5% of the total samples in this way, and in particular use these tests to keep track of the performance of each rasp in service. The average difference between the hot and cold water tests should not exceed 0.1%. Carry out the hot water digestion exactly as in the case of cassettes, as described in Chap. II, 1 (a), with the following modi- fication occasioned by the fact that pulp from the Keil-Dolle rasp is apt to contain occluded air which is not removed by ether or by prolonged heating during digestion. After transferring the pulp to the 200.6 ml flask and adding the strong lead acetate, fill the flask about half full with water and place under vacuum for 3 or 4 minutes, carefully at first until frothing has ceased. Then disengage the flask, add more water, and proceed with the digestion in the prescribed manner. 6. APPARENT PURITY. Make up a composite sample by taking equal portions of pulp from a. number of the regular samples after rasping and mixing. Test at least 6 composite samples a day, and make it a rule that each composite sample shall represent the same number of indi- vidual samples, in order that a correct average of the daily work may be readily obtained. Do not hold any pulp for more than 2 3 hours, however, on account of the danger of deterioration. Obtain the pressed juice and determine the apparent purity exactly as described in Chap. II, 1, "Cassettes," under "Prepara- tion of Sample" and under "Analysis, (b) Apparent Purity," paying due regard to the standard pressure specified. XIII. ASH ANALYSIS OF SUGAR FACTORY PRODUCTS 1. PREPARATION AND DETERMINATION OF LIXIVIATED ASH Weigh out approximately 3 grams of molasses (in the case of other products an amount equivalent to about 0.5 gram of ash) in a platinum dish, and char at a low temperature, never employing a full red heat because of the danger of volatilizing alkali chlorides and of fusing the ash. Follow exactly the procedure for the determination of lixiviated ash as described in Chap. I, 7 (b). It will probably be most convenient to prepare at one time sufficient ash for all the determinations, and then, after grinding and mixing, preserve it in a tightly stoppered bottle. Avoid un- necessary exposure to the air in preparing the sample, so that it will not absorb moisture. As the anhydrous ash is very hygro- scopic, no attempt should be made to weigh out even multiples or fractions of a gram; weighing by difference, from a weighing bottle, is recommended. To save time, the ash used for the determination of silica, iron and aluminum, calcium, and magnesium ; of potassium and sodium ; and of phosphoric acid may be prepared by adding sulphuric acid to a weighed amount of the original molasses or juice in each case, and igniting as in the determination of sulphated ash, I, 7 (a). In this case the percentages of the various constituents must be figured on the percentage of lixiviated ash in the molasses or juice as determined. It will probably be preferable, however, to use a prepared sample of lixiviated ash for all the determinations, as described above. 2. SILICA AND INSOLUBLE Dissolve approximately 0.5 gram of the ash, prepared as in "1," with water, cover with a watch glass, and add cautiously 108 METHODS OF ANALYSIS a slight excess of hydrochloric acid. Heat till effervescence has ceased, then remove and wash the watch glass, and evaporate to dry ness on the water bath. Moisten the residue with 5 10 ml of concentrated hydrochloric acid, cover the dish, and digest for 5 10 minutes on the bath. Add sufficient water to dissolve the salts, and heat again on the bath until solution is complete. Filter, wash first with cold water or with hot dilute hydrochloric acid, and then with hot water. Evaporate the filtrate to dryness, digest the residue with acid as before, but in smaller amount, and repeat the previous procedure. The second evaporation will usually com- plete the removal of all the silica. Ignite the two filters over a good burner, followed by a blast if necessary, and weigh as Si(X. 3. IRON AND ALUMINUM (a) In the absence of phosphoric acid: Oxidize any ferrous iron in the filtrate from "2" by adding several milliliters of bro- mine water, and boil off the bromine. Then cool somewhat, add enough hydrochloric acid to insure a total of 10 15 ml of strong acid, make *slightly alkaline with ammonium hydroxide, and boil for a few moments. The ammonia should not be in such excess as to require long boiling to expel the most of it, nor is the expulsion of the whole of it necessary or desirable. Filter as soon as the precipitate settles, wash with hot water, ignite, and weigh as Fe 2 3 + A1 2 3 . Multiply by .6994 to obtain the iron (Fe) equiva- lent. (b) In the presence of phosphoric acid: After oxidizing the iron with bromine water and boiling as in (a), nearly neutralize with a sodium carbonate solution, adding it drop by drop until a slight permanent precipitate is produced, which is then redis- solved by the addition of a few drops of hydrochloric acid. Add 2 3 grams of sodium acetate (or 5 10 ml of a 30% solution), then add a ferric chloride solution of known iron content drop by drop from a burette as long as any precipitate is formed, avoiding any excess. As soon as the phosphoric acid is all precipitated, the blood- red ferric acetate is formed. If the solution turns red without the addition of any ferric chloride, none should be added, for in that case the iron is in excess of the phosphoric acid. Up to this point the volume should be kept as small as possible. Now dilute to a volume of at least 150 ml with boiling water, and boil for *See Hillebrand, U. S. Geol. Surv. Bull. 700, p. 107. XIII. ASH ANALYSIS OF SUGAR FACTORY PRODUCTS 109 not more than two or three minutes. Filter while hot, and wash with hot water containing a little sodium acetate. Redissolve the precipitate in hydrochloric acid, using enough to insure a total of 10 15 ml of strong acid, and reprecipitate with ammonium hydroxide as in (a), combining the filtrate with the filtrate from the basic acetate precipitation. Ignite and weigh as Fe 2 3 + A1 2 3 -f- PgOs- From the weight of the precipitate deduct the Fe 2 3 equivalent of the ferric chloride added, deduct also the amount of P 2 O 5 present as determined in "9," then multiply by .6994 to obtain the iron equivalent of the iron and aluminum present. (c) Determination of iron and aluminum separately: Fuse, in a platinum crucible, the ignited precipitate obtained as in (a) or (b) with about 4 grams of fused potassium hydrogen sulphate. This fusion takes but a few minutes and must not be continued unnecessarily. After cooling, add 5 ml of concentrated sulphuric acid and heat until copious fumes of sulphuric acid are given off. Cool, transfer to a flask, add water, and digest till the solution is clear. Reduce with zinc, cool, titrate with N/50 potassium per- manganate (standardized against sodium oxalate), and calculate to iron (Fe). Obtain the aluminum by difference. 4. CALCIUM Use the filtrate from 3 (a), or the two combined filtrates from 3 (b), which should be slightly alkaline with ammonia. To the boiling solution add drop by drop, from a pipette, burette, or capillary tube, 10 ml of hot ammonium oxalate solution, or suf- ficient to precipitate all the calcium present. Filter after standing for at least one hour, wash with hot water, and determine as oxide or sulphate as described under ''Limestone," Chap. XVI, 5. Mul- tiply the weight of CaO by .7146, or of CaS0 4 by .2944, to convert to calcium (Ca). For very accurate work, the ignited calcium oxide is dissolved in hydrochloric acid and reprecipitated with ammonia and ammo- nium oxalate. 5. MAGNESIUM To the filtrate from l< 4" add 10 ml of sodium ammonium phos- phate or disodium hydrogen phosphate solution. After vigorous stirring add ammonium hydroxide in considerable excess. After 110 METHODS OF ANALYSIS standing over night, filter, and wash with dilute ammonium hydroxide (ammonium hydroxide of 0.90 sp. gr. diluted to ten times its volume). Char the paper slowly without allowing it to ignite, burn off the carbon over a gradually increasing flame, then apply a weak blast for a long time and repeat to constant weight to insure volatilization of any excess of P 2 5 over and above that required for the pyrophosphate formula. Weigh as Mg 2 P 2 7 and multiply by .2184 to convert to magnesium (Mg). For very accurate work, the precipitate on the filter is dis- solved in dilute hydrochloric acid, and the magnesium is reprecipi- tated by adding a few drops of sodium or sodium ammonium phos- phate and ammonia, which is added gradually with stirring and finally in slight excess. 6. POTASSIUM AND SODIUM Extract approximately 0.2 gram of ash, prepared as in "1," with water and hydrochloric acid as in "2." Remove the soluble silica as described in " 2, " evaporate the filtrate and washings to dryness, dissolve in hot water, add 5 ml of barium hydroxide solution, and heat to boiling; let settle for a few minutes, and de- termine if the precipitation is complete by the addition of barium hydroxide solution to a little of the clear liquid. When no fur- ther precipitate is produced, filter and wash thoroughly with hot water. Heat the filtrate to boiling, add ammonium hydroxide and ammonium carbonate to complete the precipitation of the barium, calcium, etc., let stand a short time on the water bath, filter, and wash the precipitate throughly with hot water; evaporate the filtrate and washings to dryness, expel ammonium salts by heating below redness, treat with a little hot water, add a few drops of ammonium hydroxide, 1 or 2 drops of ammonium carbonate, and a few drops of ammonium oxalate ; let stand a few minutes on the water bath, set aside for a few hours, filter, evaporate to complete dryness on the water bath, and heat to dull redness until all ammonium salts are expelled and the residue is nearly or quite white. Dissolve in a minimum amount of water, filter into a tared platinum dish, add a few drops of hydrochloric acid, evaporate to dryness on the water bath, heat to dull redness, cool in a desiccator, and weigh as potassium and sodium chlorides. Repeat the heating until con- stant weight is obtained. Dissolve in a small amount of water; if any residue remains, the separation must be repeated until the residue of potassium and sodium chlorides is entirely soluble. Xni. ASH ANALYSIS OP SUGAR FACTORY PRODUCTS 111 Dissolve the residue with water, using at least 20 ml for each deci- gram of potassium oxide present, add 5 ml of platinic chloride solution, and proceed as in the determination of potash by the Lindo-Gladding method, Chap. X, 9. Calculate the sodium by difference from the weight of the combined potassium and sodium chlorides. If the determination of potassium alone, and not sodium, is required, this may be made by saturating the original juice or molasses with sulphuric acid, and proceeding as in the determina- tion of potash in liquors as described in Chap. IX, 12 (3). 7. CHLORINE (*Volhard Method) REAGENTS (a) N/10 or N/20 silver nitrate. (b) N/10 or N/20 ammonium or potassium sulphocyanate. (c) Ferric indicator: A saturated solution of ferric alum (ferric ammonium sulphate). (d) Nitric Acid: Free from lower oxides of nitrogen, se- cured by diluting the usual pure acid with about !/4 part of water, and boiling till perfectly colorless. STANDARDIZATION Standardize the silver nitrate solution by titrating in the pres- ence of nitric acid against weighed amounts of freshly ignited C. P. sodium chloride (finely powdered and heated for five minutes, not quite to redness) or a standard solution of the same. Stand- ardize the sulphocyanate solution by titrating against the silver nitrate solution. Make the titrations as described below under ' ' Determination. ' ' DETERMINATION Dissolve a weighed amount of ash, prepared as in "1," in 50 ml of water in a 200 ml beaker. Add 5 ml of colorless nitric acid of 1.42 sp. gr., heat, filter if there is any important amount of insoluble matter, and wash with hot water. Add about 2 ml of the ferric indicator to the filtrate. Then add a few drops of the sulphocyanate solution from a burette, noting the quantity. Titrate with the silver nitrate solution, adding it drop by drop and stirring constantly to decolorization. Add about 0.5 ml more *Methods of Anal, of the Assoc. of Off. Agric. Chemists. 112 METHODS OF ANALYSIS of the silver nitrate solution, filter off the silver chloride, and wash thoroughly with hot water. Titrate the combined filtrate and washings to a permanent pink color with the sulphocyanate solu- tion. Find the amount of chlorine by difference from the total amounts of the silver nitrate and sulphocyanate solutions used. 8. SULPHURIC ACID Extract approximately 1 gram of ash, prepared as in "1," with water and hydrochloric acid as in "2." Filter, wash with hot water, heat the filtrate to boiling and add drop by drop 5 10 ml of a hot, 10% barium chloride solution, or sufficient to precipi- tate all the sulphuric acid. After standing over night, filter, wash free from chlorine with hot water, ignite, and weigh as barium sulphate (BaS0 4 ). Add a drop of sulphuric and hydrofluoric acids before finishing the ignition; this will remove any silica, if present, and convert any reduced barium sulphide back to sul- phate. Multiply by .4115 to convert to S0 4 . 9. ^PHOSPHORIC ACID REAGENTS (a) Moly~bdate solution: Dissolve 100 grams of molybdic acid in dilute ammonium hydroxide (144 ml of ammonium hydroxide of 0.90 sp. gr. and 271 ml of water) ; pour this solu- tion slowly and with constant stirring into dilute nitric acid (489 ml of nitric acid of 1.42 sp. gr. and 1148 ml of water. Keep the mixture in a warm place for several days or until a portion heated to 40 deposits no yellow precipitate of ammonium phos- phomolybdate. Decant the solution from any sediment and preserve in glass-stoppered vessels. (b) Ammonium nitrate solution: Dissolve 200 grams of commercial ammonium nitrate, phosphate free, in water and dilute to 2 liters. (c) Magnesia mixture: Dissolve 22 grams of recently ig- nited calcined magnesia in dilute hydrochloric acid, avoiding an excess of the latter. Add a little calcined magnesia in excess, and boil a few minutes to precipitate iron, aluminum, and phosphoric acid; filter; add 280 grams of ammonium chloride, 261 ml of ammonium hydroxide (sp. gr. 0.90) and dilute to 2 liters. Instead of the solution of 22 grams of calcined magnesia, 110 grams of crystallized magnesium chloride (MgCl 2 .6H 2 0) dissolved in water *Methods of Anal, of the Assoc. of Off. Agric. Chemists. ASH ANALYSIS OF SUGAR FACTORY PRODUCTS 113 may be used, then add 280 grams of ammonium chloride and proceed as above. (d) Dilute ammonium hydroxide for washing: Dilute 100 ml of ammonium hydroxide (sp. gr. 0.90) to 1 liter. DETERMINATION Extract a weighed amount of ash, prepared as in "1," with water and hydrochloric acid as in "2." Remove the soluble silica as described in "2," neutralize the filtrate and washings with ammonium hydroxide, clear with a few drops of nitric acid, and add about 15 grams of dry ammonium nitrate or a solution contain- ing that amount. To the hot solution add 60 80 ml of the molyb- date solution for every decigram of phosphoric acid (P 2 5 ) that is present. Digest at about 65 C. for an hour, and determine if the phosphoric acid has been completely precipitated by the addi- tion of more molybdate solution to the clear supernatant liquid. Filter and wash with cold water or, preferably, ammonium nitrate solution. Dissolve the precipitate on the filter with ammonium hydroxide and hot water, and wash into a beaker to a bulk of not more than 100 ml. Nearly neutralize with hydrochloric acid, cool, and add magnesia mixture from a burette; add slowly (about 1 drop per second) stirring vigorously. After 15 minutes add 12 ml of ammonium hydroxide of 0.90 sp. gr. Let stand till the supernatant liquid is clear (2 hours is usually enough), filter, and wash with the dilute ammonium hydroxide until the washings are practically free from chlorine. Ignite the precipitate as de- scribed under the determination of magnesium, and weigh as magnesium pyrophosphate, Mg 2 P 2 7 . Multiply by .6379 to con- vert to P 2 5 and by .8534 to convert to P0 4 . 10. CARBONIC ACID Carbonic acid (CO 3 ) is usually calculated by difference, as the amount necessary to saturate the excess of basic over acid ions. It may be accurately determined by the method described in Chap. XIV, 16. 11. HYPOTHETICAL COMBINATIONS Join phosphoric acid to calcium; if there is any uncombined phosphoric acid remaining, join it to magnesium and sodium re- spectively. Then assign the residual basic ions in the following order: potassium, sodium, magnesium, calcium, and iron, to the residual acid ions in the following order : chlorine, sulphuric acid, and carbonic acid. 114 METHODS OP ANALYSIS Sometimes the total of all the constituents or the direct deter- mination of carbon dioxide will indicate that the silica should be calculated to the silicic acid ion (Si0 3 ) and combined with calcium. 12. STATEMENT OF ANALYSIS Report the analysis in the following form: MOLASSES ASH Factory. (Date) Description of Sample: MOLASSES ANALYSIS % on % on % on Original Dry Sub. Lix'd. Ash Dry Substance 80.12 Lixiviated Ash 11.46 14.30 Sulphated Ash 12.02 15.00 Factor, Sulph'd to Lix'd Ash 953 Potassium Oxide, K 2 5.83 7.28 50.87 Sodium Oxide, Na 2 1.00 1.25 8.73 % on Lix'd Ash ASH ANALYSIS Silica and Insoluble Iron and Aluminum, as Iron Fe Calcium . Ca Magnesium Mg Potassium K Sodium Na Chlorine Cl Sulphuric Acid S0 4 Phosphoric Acid P0 4 Carbonic Acid C0 3 Total COMBINATIONS Silica and Insoluble Potassium Chloride KC1 Potassium Sulphate K 2 S0 4 Potassium Carbonate K 2 C0 3 Sodium Carbonate Na 2 C0 3 Magnesium Carbonate MgC0 3 Calcium Carbonate CaC0 3 Ferrous Carbonate FeCO 3 Sodium Phosphate Na 3 P0 4 Magnesium Phosphate .. . .Mg 3 (P0 4 ) 2 Calcium Phosphate Ca 3 (P0 4 ) Total , (NOTE: Omit combinations not required.) XIV. SCALES AND DEPOSITS The composition, of scales varies so widely that it is difficult to prescribe methods for everything which may be encountered. The following methods will, however, generally cover the impor- tant constituents of scales deposited from water or juice in a beet sugar factory. 1. SAMPLING Obtain samples before the apparatus is boiled out, or, if this is not possible, take samples after boiling out and include a nota- tion to this effect in the record. In obtaining the sample observe caution to avoid contamination with the underlying metal. To this end chipping will be found more reliable than scraping. Take sam- ples from several parts of the apparatus in which the scale is found, and endeavor in every case to get portions which accurately rep- resent the entire thickness of the incrustation. Note the average thickness of the scale (in decimal inches) using calipers where practicable. Note also the hardness and other physical characteristics of the scale. 2. PREPARATION OF SAMPLE If the sample is moist, dry it before grinding. Reduce the entire sample to 60 mesh, mix thoroughly, dry 20 50 grams to. constant weight in an oven at 100 105, cool in a desiccator, and preserve in a stoppered bottle. From this one general sample take all weighed portions for analysis. 3. QUALITATIVE EXAMINATION Previous to any quantitative determinations, examine portions of the sample for the' following : insoluble, soluble silica, copper, iron and aluminum, manganese, zinc, calcium, magnesium, potas- sium, and sodium; and for the following acids: hydrochloric, hydrosulphuric, sulphurous, sulphuric, phosphoric, carbonic, oxalic. 116 METHODS OF ANALYSIS acetic, tartaric, and citric. The methods for the qualitative exam- ination are so well known that they need not be repeated here. Since the presence of manganese, or of the other metals not mentioned, will be quite unusual, as also acetic, tartaric, and citric acids, the quantitative methods for them will not be given. QUANTITATIVE EXAMINATION 4. INSOLUBLE Ignite 1 gram of the thoroughly dried sample in a platinum crucible at a moderate heat to decompose organic acids, never heating above a dull redness, on account of the danger of volatiliz- ing alkalies. Transfer to a beaker, add 20 ml of 1 :1 hydrochloric acid, 5 10 ml of concentrated nitric acid, and water to a volume of about 150 ml. Digest on a hot plate for one hour, replacing the water lost by evaporation. Filter, wash with hot water, ignite and weigh the residue. 5. SOLUBLE SILICA Evaporate the filtrate from "4" to dryness on a water bath in a platinum or porcelain dish. Add 5 10 ml of concentrated hydrochloric acid, cover the dish, and digest for 5 10 minutes on the bath. Add sufficient water to dissolve the salts, and heat again on the bath until solution is complete. Filter, wash first with cold water or with hot dilute hydrochloric acid until the absence of any yellow color in the precipitate or paper indicates the re- moval of the iron, then finish the washing with hot water. Evapo- rate the filtrate to dryness, digest the residue with acid as before, but in smaller amount, and repeat the previous procedure. The second evaporation will usually complete the removal of all the silica. Ignite the two filters over a good burner, followed by a blast if necessary, and weigh as Si0 2 . 6. COPPER If more than a trace of copper is present, remove it from the filtrate from "5" by the following procedure. Heat the solution, which is already acid with hydrochloric acid, to boiling, and satu- rate with washed hydrogen sulphide gas, continuing the saturation until the solution has cooled to room temperature. Filter off the copper sulphide, washing well with hydrogen sulphide water. Do XIV. SCALES AND DEPOSITS 117 not allow the filter to run - dry, as traces of the sulphide will be oxidized to sulphate on exposure to the air and will pass into the filtrate. If the amount of copper is very small, it may be estimated with sufficient accuracy by igniting and weighing as cupric oxide (CuO). Otherwise use the following volumetric method. *Low VOLUMETRIC METHOD REAGENTS (a) Standard Sodium Thiosulphate Solution: A solution containing 19 grams of the pure crystals in 1 liter. (b) Starch Indicator: Mix about 0.5 gram of finely pow- dered potato starch with cold water to a thin paste; pour into about 100 ml of boiling water. STANDARDIZATION Weigh accurately about 0.2 gram of pure copper foil and transfer to a 250 ml flask. Dissolve by warming with 5 ml of a mixture of equal volumes of strong nitric acid and water. Dilute to 50 ml, boil till all brown oxides of nitrogen have been expelled, add 5 ml of strong bromine water, and boil until the bromine is completely driven off. Cool somewhat and add a slight excess of strong ammonium hydroxide (about 7 ml). Again boil until the excess of ammonia is expelled, as shown by a change of color of the liquid and a partial precipitation. Then add a slight excess of strong acetic acid (3 or 4 ml of 80% acid) and boil for a minute. Cool to room temperature and add 10 ml of 30% potassium iodide solution. Titrate at once with the thiosulphate solution until the brown tinge has become weak, then add sufficient starch indicator to produce a marked blue coloration. Continue the titration cautiously until the color due to free iodine has entirely vanished. The blue color changes toward the end to a faint lilac. If at this point the thiosulphate be added drop by drop and a little time allowed for complete reaction after each addition, there is no difficulty in determining the end point within a single drop. One ml of the thiosulphate will be found to correspond to about 0.005 gram of copper. DETERMINATION Place the filter containing the copper sulphide precipitate in a small flask, add 4 5 ml of concentrated sulphuric acid and the *Methods of Anal, of the Assoc. of Off. Agric. Chemists. 118 METHODS OF ANALYSIS same amount of nitric acid and heat until white fumes appear. Continue the oxidization, adding a little nitric acid from time to time, until the liquid remains colorless upon heating to the appear- ance of white fumes. Cool, dilute with about 30 ml of water, add an excess of bromine water, boil until all bromine is expelled, and proceed exactly as above under ' ' Standardization. " 7. IRON AND ALUMINUM Boil the filtrate from "6" to expel hydrogen sulphide, then add bromine water (use the filtrate from "5" if copper has not been determined) and proceed as in Chap. XIII, 3 (a) or (b), according to whether phosphoric acid is present or not. Employ the latter method (basic acetate separation) in any case, if zinc is to be subsequently determined. 8. ZINC Having precipitated the iron, aluminum, and phosphoric acid by the basic acetate method as in Chap. XIII, 3" (b), pass hydrogen sulphide into the filtrate until all the zinc sulphide, which should be pure white, is precipitated. Filter, and wash with hydrogen sulphide water containing a little ammonium nitrate. Char the paper at a low temperature, heat to 800 900 in a muffle for one hour, and weigh as ZnO. Multiply by .8034 to convert to zinc (Zn.) 9. CALCIUM AND MAGNESIUM Boil the filtrate from "8" to expel hydrogen sulphide (use the filtrate from "7" if zinc has not been determined), make alkaline with ammonia, and determine as in Chap. XIII, 4 and 5. 10. POTASSIUM AND SODIUM Determine as in Chap. XIII, 6, or as follows: Weigh out, from the dried sample, enough material to give approximately 0.2 gram of the combined sulphates of magnesium, potassium, and sodium. Dissolve in hydrochloric acid and remove silica as in "4" and "5." Concentrate the filtrate and add a few milliliters of dilute sulphuric acid. Continue the evaporation over a Hillebrand radiator until fumes of S0 3 come off copiously, repeating the addition of sulphuric acid, if necessary, to decom- pose organic matter. Drive off the excess of sulphuric acid, take up with hot water and a few drops of hydrochloric acid, then remove iron, aluminum, and calcium as in "7" and "9." (This XIV. SCALES AND DEPOSITS 119 can be done in one operation.) Evaporate the filtrate in a plati- num dish, adding toward the last a drop or two of sulphuric acid, and drive off the ammonium salts and the last traces of sulphuric acid by gentle ignition. Finally heat to dull redness, preferably in a muffle, to decompose bisulphates. Cool and weigh as MgS0 4 + K 2 S0 4 + Na,S0 4 . Repeat the ignition to constant weight. From this point on avoid exposure to ammonia fumes. Dissolve the residue in water, acidify with a few drops of hydrochloric acid, add chloroplatinic acid solution in excess and proceed as in the determination of potassium, Chap. X, 8. Mul- tiply the weight of potassium platinic chloride, converted to per- centage, by .3854 to convert to potassium sulphate, and multiply the percentage of magnesium, determined as in "8," by 4.9498 to convert to magnesium sulphate. Subtract the sum of these two from the percentage of combined sulphates to obtain the sodium sulphate, which multiplied by .3238 gives the percentage of sodium (Na) v . Multiply potassium platinic chloride by .1609 to obtain potassium (K). 11. CHLORINE. Determine as in Chap. XIII, 7. It sometimes happens that the solution is too dark to permit the chlorine to be determined volumetrically. In this event proceed as follows: Prepare a nitric acid solution of a weighed portion of the material, as for the volumetric method, and filter. Add a sufficient amount of silver nitrate solution to precipitate all the chlorine, avoiding any great excess. Heat to 50 and allow to stand for about one hour in a dark place. Filter through a Gooch crucible, and wash the precipitate several times by decantation with cold water slightly acidified with nitric acid. Transfer the precipitate to the Gooch and wash free from silver nitrate. Dry for half an hour at 100, and finally at 130 to constant weight. Multiply silver chloride by .2474 to convert to chlorine (Cl). 12. SULPHURIC ACID (SULPHATE SULPHUR) (a) Method I: Digest 1 gram of the sample with about 100 ml of water, and an excess of bromine water or sodium peroxide to oxidize sulphides and sulphites. Acidify with hydrochloric acid, and boil to complete solution and expel the excess of bromine. Filter and wash well with hot water. Add drop by drop to the boiling solution an excess of hot, 10% barium chloride solution. After standing over night, filter, wash free from chlorine with 120 METHODS OF ANALYSIS hot water, ignite, and weigh as barium sulphate. Add a drop of sulphuric and hydrofluoric acids before finishing the ignition ; this will remove any silica, if present, and convert any reduced barium sulphide back to sulphate. From the total sulphur thus determined subtract the sulphite and sulphide sulphur determined as in ' ' 13 " and "14" to obtain the sulphate sulphur. (b) Method II: Dissolve 1 gram of the sample in about 100 ml of water and 5 ml- of concentrated hydrochloric acid, in a flask in an atmosphere of carbon dioxide. Boil the hydrochloric acid solution, maintaining the atmosphere of carbon dioxide, until the hydrosulphuric and sulphurous acids have been completely ex- pelled. Filter, wash, and precipitate the sulphate sulphur in the filtrate with barium chloride as in Method I. Multiply the weight of barium sulphate by .4115 to convert to S0 4 . 13. SULPHUROUS ACID (SULPHITE SULPHUR) APPARATUS A distillation flask, set above a burner, and fitted with a 3-hole rubber stopper. Through one hole of the stopper passes a dropping funnel or thistle tube, the stem of which reaches nearly to the bottom of the flask. Through another hole a glass tube extends nearly to the surface of the liquid in the flask and connects at the upper end to a carbon dioxide generator through a washing bottle. Through the third hole a short tube leads through a safety bulb to a short Liebig condenser which is so inclined that the lower end reaches well into the receiving vessel. The details of the generator are not important as long as the rate of flow of the gas can be regulated and the gas passes through a washing bottle. DETERMINATION Transfer 10 grams of the material to the distillation flask, fit in the stopper, and connect to the condenser and the gas gen- erator; then introduce through the funnel or thistle tube 250 ml of recently boiled, distilled water.. Start a current of gas through the apparatus, and place a receiving flask or beaker containing 100 ml of nearly saturated bromine water under the end of the condenser with the tip of the condenser extending below the surface of the bromine water. When all the air has been displaced by carbon dioxide gas, introduce a sufficient amount of copper sul- phate solution to prevent the distillation of sulphide sulphur, and add 10 20 ml of a 20%, glacial phosphoric acid solution, intro- XIV. SCALES AND DEPOSITS 121 ducing it through the dropping funnel slowly until frothing has ceased. Start the distillation and continue until 150 ml of dis- tillate has passed over, watching that the bromine does not become too weak in the receiving solution. More bromine water may be added from time to time if necessary. When the distillation is completed, disconnect the condenser from the flask and rinse with water into the distillate. Transfer the distillate to a beaker, boil off the excess of bromine, add 5 ml of dilute hydrochloric acid (1 to 3), and precipitate with barium chloride, etc., as in "12." Multiply the weight of barium sulphate by .3430 to convert to S0 3 . 14. HYDROSULPHURIC ACID (SULPHIDE SULPHUR) % Determine the sulphide sulphur by repeating the determina- tion for sulphurous acid on a fresh 10 gram sample, following exactly the method outlined in "12" with the exception that no copper sulphate is added. By this procedure the hydrosulphuric acid will be distilled over with the sulphurous acid and be weighed as barium sulphate. Multiply the weight of barium sulphate thus found by .3430 to convert to S0 3 , and subtract the S0 3 determined as in "13" to obtain the S0 3 equivalent of the sulphide sulphur. Multiply this by .4004 to convert to sulphur (S). 15. PHOSPHORIC ACID Ignite 1 to 5 grams of the sample to destroy organic matter, dissolve in dilute hydrochloric acid, add a few ml of nitric acid, and boil. Then remove the silica and proceed as in Chap. XIII, 9. 16. CARBONIC ACID The carbon dioxide in the carbonates is liberated by the action of dilute sulphuric acid, purified by bubbling through a mixture of concentrated sulphuric and chromic acids, and caught in a weighed potash bulb. *APPARATUS A wide mouth extractor (C0 2 ) flask of 60 ml capacity, fitted with a 3-hole rubber stopper through which pass: (1) a glass tube leading to an acid reservoir; (2) a connection with an absorption tower filled with soda-lime to remove carbon dioxide from the air drawn through the apparatus; (3) the end of a short Liebig reflux *An illustration of a suitable arrangement of apparatus is given on Page 104 of W. W. Scott's "Standard Methods of Chemical Analysis." 122 METHODS OP ANALYSIS condenser clamped in a vertical or inclined position. The second tube should extend well down into the flask so that the incoming air will pass directly over the surface of the liquid in the flask. The upper end of the condenser is connected by a bent tube to a bottle of sulphuric-chromic acid mixture, through which the gas bubbles on its way to the potash bulb ; this serves to oxidize S0 2 and H 2 S, and to remove the moisture in the gas from the con- denser. A calcium chloride tube is attached to the potash bulb to catch any moisture carried over from the potash solution. The exit from the calcium chloride tube is connected, through a guard tube of soda-lime and calcium chloride and a catchall bottle, to a water pump which serves as a source of suction. The Vanier potash bulb is preferable to the older Liebig and Geissler forms. In place of the potash bulb may be used a pair of soda-lime U-tubes, the first of which is filled with soda-lime, while the second is filled one-third with soda-lime, followed by calcium chloride; in this case the sulphuric acid bulb serves to indicate the rate of gas flow. DETERMINATION Weigh into the extractor flask a portion of sufficient size to give 0.1 .2 gram of C0 2 , fit in the stopper, connect all the appa- ratus except the potash bulb, and test for air leaks. Start a slow cur- rent of air through the apparatus by means of the suction pump, and, when all the air in the system has been displaced by C0 2 free air, connect the potash bulb, which has been previously weighed. Thirty minutes should be ample time to displace the air. Then introduce, very slowly at first, about 30 ml of 10 per cent sulphuric acid from the acid reservoir. Be sure that the acid is not allowed to liberate so much carbon dioxide at first that there will be a backward current through the soda-lime tower, thereby resulting in the loss of some carbon dioxide. The current of air through the apparatus should not be faster than a safe working velocity for the type of potash bulb used. When all the acid has been introduced boil the contents of the flask for about 15 minutes to expel the last traces of carbon dioxide, remove the source of heat, and let the air current continue a few minutes more, then discon- nect the potash bulb and weigh it, together with its calcium chloride tube. The increase in weight gives C0 2 directly, and, multiplied by 1.363'6, the equivalent C0 3 . XIV. SCALES AND DEPOSITS 123 Alternative Method: Employ the same apparatus and man- ipulation as just described, "but in place of the potash bulb use three small bottles filled with a measured amount of standard barium hydroxide solution. See W. W. Scott, ''Standard Methods of Chemical Analysis," page 107, for details. 17. OXALIC ACID REAGENTS (a) Calcium inch. While these requirements are not usually complied with, it should be remembered that consid- erable variations may occur in the analysis to the extent to which the size of the gross sample is below the figures above given. The gross sample should be quickly crushed and reduced in acordance with the ^methods of the Bureau of Mines. When the sample has been reduced to 25 pounds, or if the gross sample does not exceed this amount, it may conveniently be ground to 60 mesh *Bureau of Mines, Technical Papers 8 and 76. tBureau of Mines, Bulletin 116, pp. 13-15. {Bureau of Mines, Bulletin 116, p. 25, and Technical Paper 133, p. 9. XV. COAL AND COKE 127 si/.e in tin- pebble mill described in Chap. XXIII, 9. About 6 hours is required for grinding _!"> pounds. Smaller samples, which have to be ground in a mortar or other apparatus exposed to the air, should first be air dried in the fol- lowing manner: After breaking up any large lumps, place the unground sample in a shallow pan, which has been previously iied and is a.irain weighed after being filled with the coal. Kxpos- the sample to the atmosphere of the room, or to a current of air raised somewhat above the ordinary temperature (30 35 C.), until two successive weighings, made 6 to 12 hours apart, show a loss in weight of not over 0.2%. (The purpose of the drying is to reduce the moisture in the sample to such an extent that rapid change in weight will not take place while the sample is being handled in the course of analysis.) Then crush the sample, reduce if necessary, and grind to 60 mesh. Calculate the results of the analysis to coal of the original moisture content. Any samples which are excessively wet should be air dried, as just described, before being ground. 3. SAMPLING OF COKE AND PREPARATION OF SAMPLE Approximately 75 small pieces, equivalent to a total weight of 1,000 to 1,500 grams, obtained by being broken oft 3 from larger pieces with a hammer, should be taken to represent as nearly as possible an average of the car. There is room for a certain amount of personal equation, but the effort should be made to obtain as representative a sample as possible, neither intentionally selecting nor rejecting any coke which differs in appearance from the remainder. Reduce the 75 pieces constituting the original sample to 10 12 mesh si/e with a jaw cnisher. If a crusher is not available use a hammer, but crush by impact with the avoidance of any grinding. Mix thoroughly, being careful to avoid uneven distribution of the fine material which is lower in ash than the coarser part, and grind 15 grams in an agate mortar to pass a 60 mesh sieve; to avoid contamination, reserve a 60 mesh sieve for this purpose. Mix the ground sample well and transfer it to a stoppered bottle. Do not use bucking boards, disc pulverizers, or any kind of mortar except an agate mortar for grinding the crushed sample, on account of the danger of contamination. 128 METHODS OF ANALYSIS 4. MOISTURE Weigh out 1 gram of the 60 mesh sample in a covered por- celain or silica *capsule % inch deep and 1% inches in diameter, and heat for exactly one hour at 105 in a constant temperature oven. The Bureau of Mines uses an oven of a special design through which a current of dry, preheated air is passed. It will be admissible to employ a glycerin oven of the regular type as described in Chap. XXIII, 7, without the use of an air current. Cool the covered capsule in a desiccator over sulphuric acid and weigh. Call the loss in weight "moisture at 105." Moisture in coke can also be determined quickly and with adequate accuracy by simply heating to constant weight a large sample of lump coke, in any convenient oven, or on a stove, hot plate, or steam coil at a temperature of 100 200 C. 5. ASH Determine ash in the same sample on which moisture has pre- viously been determined. Place the porcelain capsule containing the sample in a cool muffle and raise the temperature gradually to about 750 ; the object of this slow heating is to avoid mechan- ical loss from the rapid escape of volatile matter, and to avoid coking the sample and thus make its burning difficult. Continue the ignition in the muffle, with occasional stirring of the ash, until all particles of carbon have disappeared. Cool in a desiccator, weigh, and repeat the ignition for periods of half an hour until the difference in weight between two successive ignitions is less than 0.0005 gram. In the absence of a muffle, ignite over a flame, but be careful first to drive off the volatile matter slowly at a low temperature. 6. VOLATILE MATTER Employ a bright, well burnished, 10 ml platinum t crucible with a closely fitting capsule cover; the crucible should be 1 inch in diameter at the top and 1 3/16 inches high, and the crucible and cover together should weigh about 15 grams. Weigh out 1 gram of the 60 mesh sample, and heat for 4 6 minutes over a low flame in order to avoid mechanical loss from the rapid escape of steam and volatile matter. (This preliminary heating is neces- sary for all kinds of coal analyzed by The Great Western Sugar *Bureau of Mines, Technical Paper 76, p. 16, fig. 1, a. fBureau of Mines, Technical Paper 76, p. 18, fig. 3, a and b. XV. COAL AND COKE 129 Company, and for petroleum coke, but may perhaps be dispensed with in the case of coke which is low in volatile matter.) Follow the preliminary heating by heating for exactly 7 min- utes in an electric muffle furnace at *850. Control the tempera- ture preferably with a pyrometer. Where pyrometers are not available, the Central Laboratory will furnish standard samples of coal and coke on which the volatile matter has been determined at 850 in a pyrometer-controlled furnace. The temperature of the furnace may be regulated by making determinations on the standard samples. Seger pyrometer cones may also be found useful. If an electric furnace is not available, follow the preliminary heating by heating for exactly 7 minutes on a platinum or nichrome triangle in the full flame of a No. 3 Meker or Scimatco burner. The bottom of the crucible should be 2 cm above the top of the burner, and, to protect it from drafts, it should be enclosed in a sheet-iron t chimney of special design. Adjust the height of the flame so that the temperature in the interior of the crucible will be 850 ; this is done by making determinations with varying lengths of flame on the standard samples furnished by the Central Laboratory. After heating for 7 minutes at 850, cool in a desiccator and weigh. The loss in weight minus the weight of moisture represents the amount of "volatile matter" (at 850). 7. FIXED CARBON Subtract from 100 the sum of the percentages of moisture, ash and volatile matter. 8. SULPHUR REAGENT Eschka Mixture is composed of two parts of light calcined magnesium oxide and one part of anhydrous sodium carbonate. It may be purchased in the form of an analyzed chemical. DETERMINATION Mix 1 gram (or for convenience of calculation 1.373 grams) of the 60 mesh coal with 6 grams of Eschka Mixture in a No. 1 *The Bureau of Mines uses a temperature of 950. This temperature is sometimes difficult to reach in an ordinary electric furnace and is hard on the life of it. The temperature adopted in any case is a matter of arbitrary selection. tBureau of Mines, Technical Paper 76, p. 18, fig. 3. 130 METHODS OF ANALYSIS porcelain crucible and heat gradually in an electric muffle, with free access of air, until all the carbon has been consumed. If an electric muffle is not available, place on a triangle in a slanting position and burn out the mixture over an alcohol, gasoline, or natural gas flame ; artificial gas as a rule contains so much sulphur that its use may introduce an error in the determination. Start tke ignition in any case at a very low heat to avoid driving off volatile matter so fast that unburned sulphur escapes ; even a small loss of sulphur dioxide may be detected by its pungent odor. The temperature should never be high enough to cause blackening of the top of the Eschka Mixture in the crucible. After the crucible has been heated very slowly and cautiously for about 30 minutes, increase the heat, and after the crucible becomes red hot stir the contents occasionally until all black par- ticles are burned out, a condition which indicates that the reaction is finished. Cool, transfer the crucible with its contents to a 200 ml beaker, and digest with 75 ml of hot water for at least 30 minutes. Filter into a300 ml beaker, wash the insoluble residue twice with hot water by decantation and then on the filter 'until the volume of solution in the 300 ml beaker is about 200 ml. Add about 4 ml of saturated bromine water, or a slight excess, and enough concentrated hydrochloric acid to make the solution slightly acid. Boil off the bromine and add slowly to the boiling solution from a pipette 10 ml of a hot 10% barium chloride solution. After standing for at least 3 hours, filter, dry, ignite, and weigh as BaS0 4 , as described in Chapter I, 9. To obtain the percentage of sulphur multiply the weight of barium sulphate by 13.73 if 1 gram of material was used, or by 10 if 1.373 grams was used. 9. CALORIFIC VALUE Determine the heat of combustion with a bomb calorimeter, by burning one gram of the 60 mesh sample in compressed oxygen gas and absorbing the total heat evolved in a weighed quantity of water in which the bomb is immersed. Measure the rise in temperature of the water with a thermometer that is graduated in hundredths of 1 C. and can be read by a telescope to .002 C. Make corrections for radiation, combustion of the iron wire, oxida- tion of nitrogen to aqueous nitric acid, and oxidation of sulphur dioxide to aqueous sulphuric acid. The calorific value obtained in this manner is the total heat of combustion with water vapor XV. COAL AND COKE 131 condensed to liquid water at the temperature of the calorimeter, i. e., 2025 C. For detailed directions consult Technical Paper 8 of the Bureau of Mines and Circular 11 of the Bureau of Standards, also the pamphlet of directions furnished with the calorimeter. On page 13 of the Bureau of Mines Paper is given an explanation and example of the customary method of calculating the radiation correction ; a shorter method is described on page 15 of the Bureau of Standards circular. The correction for iron wire is 1.7 calories (3.1 B. T. U.) per milligram. The correction for sulphur burned to sulphuric acid is 13 calories (23 B. T. U.) per 0.01 gram of sulphur. The cor- rection for nitrogen to aqueous nitric acid is made by titrating the acidity of the bomb liquor with standard ammonia solution (0.00574 gram NH 3 per ml), using methyl orange as indicator, and is equivalent to 5 calories (9 B. T. U.) per milliliter. These corrections need be determined only occasionally for each different type of coal. Use only thermometers which have been tested by the Bureau of Standards and make the necessary corrections according to the certificate. The thermometers may be either of the regular kind with a scale range of about 20 30 C., or of the Beckmann or ''differential' 7 type. Use only oxygen which is made by a liquid air process; do not use electrolytic oxygen, which contains small amounts of hydrogen. Check the water equivalent of the calori- meter by burning weighed amounts of the standard "combustion samples" (benzole acid, napthalene. and sucrose) of the Bureau of Standards of known calorific value. 10. ANALYSIS OF BOILER HOUSE ASHES See Chap. VII. 4 and 5, regarding the sampling of boiler house a-lies and the preparation of the samples. Dry a sufficient amount of the sample to approximately con- stant weight at 105. Determine the percentage of actual ash by igniting 1 gram, or approximately this amount, of the dried sample, as described in the determination of ash, section 5 of this chapter. Figure tlx- percentage of ash on the weight of the dried sample. 132 METHODS OF ANALYSIS 11. BIBLIOGRAPHY "Methods of Sampling Delivered Coal" Bur. Mines, Bulletin 116. "Directions for Sampling Coal for Shipment or Delivery" Bur. Mines, Tech. Paper 133. "Methods of Analyzing Coal and Coke" Bur. Mines, Tech. Paper 8. "Notes on the Sampling and Analysis of Coal" Bur. Mines, Tech. Paper 76. "A Convenient Multiple-unit Calorimeter Installation" Bur. Mines, Tech. Paper 91. "The Determination of Moisture in Coke" Bur. Mines, Tech. Paper 148. "The Standardization of Bomb Calorimeters" Bur. Standards, Circ. 11. "Standard Samples General Information" Bur. Standards, Circ. 25. "Coal," by E. E. Somermeier. XVI. LIMESTONE 1. GENERAL Sample every car of limestone and determine by the "rapid method :" (a) Insoluble, and iron and aluminum oxides (together). (b) Calcium carbonate. At the end of every week make up a composite sample repre- senting the week's deliveries by mixing equal portions of the sam- ples of the individual cars. If more than one kind of limestone has been received, make up and analyze separate composite samples for each kind. On the weekly average samples make the complete analysis by the gravimetric method, determining : (a) Insoluble. (b) Iron and aluminum oxides. (c) Calcium carbonate. (d) Magnesium carbonate. (e) Calcium sulphate, if present. Keep the individual car samples for at least two weeks before discarding, for possible reference. 2. SAMPLING AND PREPARATION OF SAMPLE Approximately 75 small pieces, obtained by being broken off from larger pieces with a hammer, should be taken as uniformly as possible over the top of the car before it is unloaded, or during the unloading. There is room for a certain amount of personal equation, but the effort should be made to obtain as representative a sample as possible, neither intentionally selecting nor rejecting any stone which differs in appearance from the remainder. If a piece which is sampled contains a coating of surface material, the small sample taken should be broken off in a direction which will include an approximately proportional amount of this surface material. 134 METHODS OF ANALYSIS It is quite essential to take the number of pieces specified. Even under these conditions two samples from the same car taken by different operators will occasionally differ as much as one per cent in calcium carbonate, though they will generally be much closer. Reduce the 75 pieces constituting the original sample to ^4 inch size with a jaw crusher. Mix the crushed sample well and quarter it. Reduce one of the quarters to 60 mesh size with a disc pulverizer. Mix the finely ground sample well, and preserve a suitable amount in a stoppered bottle. GRAVIMETRIC METHOD 3. INSOLUBLE Dissolve 0.4 .5 gram in 50 ml of water and 20 ml of concen- trated hydrochloric acid, in a beaker covered with a watch glass. When effervescence has ceased, heat to boiling and digest on a hot plate for 10 15 minutes. Filter, wash thoroughly with hot water, ignite and weigh the "insoluble." 4. IRON AND ALUMINUM To the filtrate from "3" add several milliliters of bromine water, or a few drops of concentrated nitric acid, and boil. Then cool somewhat, make slightly alkaline with ammonium hydroxide, and boil for a few moments. The ammonia should not be in such excess as to require long boiling to expel the most of it, nor is the expulsion of the whole of it necessary or desirable. Filter as soon as the precipitate settles, wash with hot water, ignite, and weigh as Fe 2 3 + Al,0 3 . 5. CALCIUM Dilute the filtrate from "4" to a volume of at least 150 ml, heat to boiling, and to the boiling solution add drop by drop, from a pipette, burette, or capillary tube, 20 ml of hot ammonium oxalate solution. By adding the reagent in this manner the calcium oxalate will be precipitated in a granular form which will permit of rapid filtration and it will not pass through the filter paper. Filter after standing for at least one hour, wash two or three times with hot water, and convert to oxide or sulphate, as described below. XVI. LIMESTONE 135 (a) Determination qs Oxide: Ignite over a burner of the Meker type for one-half hour or longer, in a platinum crucible which has been weighed together with its cover. After the carbon is all burnt off, put on the cover, and keep the crucible covered during the balance of the ignition, and during cooling, weighing, and subsequent ignitions. Blast for successive periods of 5 minutes until the weight is constant, or heat in an electric furnace. Cool in a desiccator over concentrated sulphuric acid, which should be renewed frequently, especially when it begins to show any sign of discoloration, and do not let the crucible stand in the desiccator for more than half an hour before weighing. Weigh as calcium oxide, and multiply by 1.7848 to convert to calcium carbonate (CaC0 3 ). (b) Determination as Sulphate: Ignite in a platinum cru- cible until all carbon is burnt off, but not necessarily until all carbonate is decomposed. After cooling, slack cautiously with a little water and add a slight excess of sulphuric acid. Evaporate on a *Hillebrand radiator until all the free acid is expelled, heat to dull redness over a flame, and weigh as calcium sulphate. Mul- tiply by .7351 to convert to calcium carbonate. Sulphuric acid may be added before the filter paper is burnt, but in this case a second addition of sulphuric acid must be made after tin- carbon is all burnt off, in order to reconvert any sulphate reduced to sulphide by the carbon of the paper. When calcium is weighed as the sulphate, certain precautions are necessary as calcium sulphate is partially converted to oxide at a red heat. After the final addition of sulphuric acid the cru- cible must not be heated above a dull redness, i. e., a redness which is barely visible in daylight. When sulphuric acid is added before the filter paper is burnt off, this degree of heat must not be 'X'-eeded at any time during the ignition. After weighing, a drop of phenolphthalein should be added; if the precipitate has been properly handled it should not give a pink color with the indicator. If a pink color is produced, add a little sulphuric acid and repeat the previous procedure until the precipitate fails to give a pink color with phenolphthalein. In th<- ignition of precipitates in general, the paper is most easily burnt if high temperatures are avoided, especially at first. The best results are probably obtained by charring the paper without allowing it to break into flame, and then raising the tem- *See Chap. XXIII, 15. 136 METHODS OP ANALYSIS perature to the point where the charred residue just begins to glow nicely. After the carbon is all burnt off, the crucible may be raised to whatever temperature the conditions of the particular deter- mination require. 6. MAGNESIUM To the filtrate from "5" add 10 ml of sodium ammonium phosphate or disodium hydrogen phosphate solution. After vig- orous stirring add ammonium hydroxide in considerable excess. After standing over night, filter, and wash with dilute ammonium hydroxide (ammonium hydroxide of 0.90 sp. gr. diluted to ten times its volume). Char the paper slowly without allowing it to ignite, burn off the carbon over a gradually increasing flame, then apply a weak blast for a long time and repeat to constant weight to insure volatilization of any excess of P 2 5 over and above that required for the pyrophosphate formula. Weigh as Mg 2 P 2 7 and multiply by .7572 to convert to magnesium carbonate (MgC0 3 ). 7. SULPHURIC ACID Sulphur seldom occurs in important amount in limestone used by beet sugar factories. If this determination is necessary, it may be made as follows : Dissolve 1 2 grams in water and hydrochloric acid, filter, and wash with hot water. Determine the sulphuric acid in the filtrate as in Chap. XIII, 8. If sulphuric acid is found present, calculate it as calcium sulphate, and subtract its calcium carbonate equivalent from the calcium carbonate equivalent of the total calcium determined as in "5-." Limestone from new or unfamiliar quarries should always be examined for sulphuric acid. RAPID METHOD 8. INSOLUBLE, AND IRON AND ALUMINUM OXIDES Dissolve 0.4 .5 gram in 50 ml of water and 20 ml of concen- trated hydrochloric acid, in a beaker covered with a watch glass. When effervescence has ceased, heat to boiling and digest on a hot plate for 10 15 minutes. Add several milliliters of bromine water, or a few drops of concentrated nitric acid, and boil. Then cool somewhat, make slightly alkaline with ammonium hydroxide, and boil for a few moments. Filter, wash well with hot water, ignite, and weigh as ''insoluble" + Fe 2 3 + A1 2 3 . XVI. LIMESTONE 1 37 9. CALCIUM RHAGBNT N/5 or N/10 Potassium rrrnunnfintate: For a N/5 solution, dissolve 6.32 gnmis of the pure crystals in water, filter through asbestos, and make up to 1 liter. One ml of this solution will be found to be equivalent to about .01 gram of calcium carbonate. K.M p in a dark bottle well protected from the light. The solution should be allowed to stand several days, if possible, before it is Mandardized, and its value will vary but little after this time. As a matter of precaution, however, it is well to restandardize it once a month. STANDARDIZATION Weigh out 1.34 grams of sodium oxalate of the *highest purity obtainable, dissolve in water, add 50 ml of dilute sulphuric acid (1 to 10), dilute to a volume of about 150 ml, heat to 70, and titrate to a permanent pink with the permanganate solution. From several such titrations determine the calcium carbonate equivalent of one ml of the permanganate. Sodium oxalate of the Bureau of Standards may be used for a primary standard. Traces of moisture can be removed from sodium oxalate by heating at 120 for two hours. DETERMINATION Dilute the filtrate from "8" to" a volume of at 'least 150 ml, heat to boiling, and to the boiling solution add drop by drop from a pipette, burette, or capillary tube, 20 ml of hot ammonium oxalate (4% solution). By adding the reagent in this manner the calcium oxalate will be precipitated in a granular form which will permit of rapid filtration and it will not pass through the filter paper. Filter after standing for at least one-half hour, and wash thoroughly, but not excessively, with hot water. Wash the precipitate into a beaker with a jet of hot water, allowing the open paper to cling to the side of the beaker above tin- liquid. Add 50 ml of dilute sulphuric acid (1 to 10), pouring it over the surface of the paper. Dilute to a volume of about 150 ml, heat to 70, and titrate with the permanganate solution. The reaction requires a short time after the addition of the perman- ganate, but, after it once begins, the permanganate may be added quite rapidly until the end point is nearly reached. Continue the *Use the grade "C. P. Special for Standardizing" and not the ordi- nary "C. P." 138 METHODS OF ANALYSIS titration drop by drop until a faint pink color persists, then intro- duce the filter paper and add a few drops more of the perman- ganate, if necessary, until the permanent end point is reached. 10. CARBONIC ACID Ignite 0.5 gram in a platinum crucible to constant weight over a good burner, followed by a blast, or in an electric furnace. The loss on ignition is considered to represent the amount of carbon dioxide. Check the efficiency of the furnace or burner occasionally by the ignition of pure calcium carbonate. If moisture is present in the original sample, it must first be dried for one hour at 100 105 and then weighed. This precaution is, however, hardly ever necessary. 11. CALCULATION OF RESULTS Multiply the percentage of C0 2 (loss on ignition) by 2.2742 to obtain the percentage of total carbonates as calcium carbonate. Subtract the percentage of calcium carbonate, as determined in "9," and multiply the difference by .8426 to obtain the percentage of magnesium carbonate. XVII. WATER 1. SAMPLING OF WATER FOR BACTERIOLOGICAL EXAMINATION (a) APPARATUS Use sterilized bottles provided with glass stoppers and with cloth caps secured by a rubber band. The bottles are cleansed with great care, rinsed in clean water, and sterilized, together with the stoppers and caps, by heating to 180 190 C. A suitable ship- ping case, containing compartments for the bottles and for icing, is also required. (b) PROCEDURE Adhere strictly to the following procedure : (1) Allow a good stream to run from the faucet or source of supply for at least 10 minutes before the sample is taken, in order that one may be sure of obtaining fresh water and not water which has been standing in the pipe. (2) Remove the rubber band and the cloth cap from the bottle, being careful not to drop the cap or to allow anything to touch the inside of it. (3 1 ) Rinse the outside of the bottle, with the stopper in place, with water from the source of supply which is to be sampled. (4) Remove the stopper, being careful not to touch any part of it except the portion which projects outside the bottle. (5) Fill the bottle completely with the water to be tested. (6) Holding the bottle in one hand and the stopper, in an inverted position, in the other hand, invert the bottle and allow some of the water to run out over the stopper. Insert the stopper while pouring, thus leaving some air space to allow the bottle to ! shaken before plating. (7) Rinse the outside of the bottle again. 140 METHODS OF ANALYSIS (8) Put the cap on the bottle, and secure with the rubber band. (9) Label the bottle with regard to the source of sample, time when taken, etc. Observe care to omit none of the steps in the procedure above described. Number Seven, which calls for rinsing the stopper and the outside of the bottle after the stopper has been inserted, is probably the one which is most apt to be forgotten. Immediately after the samples have been taken, ship them on ice to the laboratory where they are to be tested. 2. SAMPLING OF WATER FOR CHEMICAL ANALYSIS No particular directions are needed with regard to the collec- tion of special samples. The following instructions relate to the collection of weekly and campaign average samples for analysis: (a) CAMPAIGN AVERAGE SAMPLES A composite sample of each kind of water of importance, as described below, should be made up during the campaign and analyzed after the end of the campaign. The Chief or Assistant Chemist should once a shift obtain the required samples, and, in order to avoid contamination with sulphuric acid, he should use a different set of test tubes; or receptacles from that used by the sample carrier who obtains samples for the alpha-naphthol tests. A measured volume of each kind of water should be transferred to a bottle of suitable size, 'appropriately labeled, to form the composite sample. Sufficient water should be taken so that the final volume will amount to at least 2 liters, and preferably more in the case of waters low in solids. It is advisable to make up several composite samples of each water, representing successive periods of three or four weeks each during the campaign, and to test these for contamination before ' mixing to form the general composite sample. The collection of these samples should be started as soon after the beginning of the campaign as possible, when it is certain that the waters are running in a normal manner. Samples should be taken of all "condensed water," "main supply waters," etc., and will include the following: "Water from Boiler Feed Tank Condensed Water Pumped Direct to Boilers Water in Boilers XVII. WATER 141 Water Used for Washing Hot Presses and Saccharate Presses Pure Battery Supply Water Impure Battery Supply Water All Condensed Waters (including all that are tested regularly) All Main Supply W r aters, such as Ditch, Well, River, and City Water All Cooling Waters, including Tail Pipe Waters In addition to the above, any waters that may be necessary to complete the record. Analyses of different samples representing the same water need not be unnecessarily duplicated. Thus if all or a number of the pan condensers are supplied with the same water, a single composite sample may be made up for analysis from the composites of the individual tail pipes. Separate samples should be saved, however, so that they will be available if any change is made in the water system during the campaign. (b) WEEKLY AVERAGE SAMPLES OF BATTERY SUPPLY WATER \\Vekly composite samples of the battery supply water should also be collected in the same manner as the campaign average samples, separate samples of the "pure" and "impure" water being taken if a dual system is in use. At the end of every week filter the water and determine the total solids, as described below. (c) AVERAGE SAMPLES DURING POTASH CAMPAIGN Factories engaged in potash recovery should also collect aver- age samples for the potash campaign of all waters sampled for the same purpose during the beet campaign, as described in (a) above, and in addition should obtain average samples of the condensed water from the steam chamber of each evaporator body. These samples should be analyzed in full, and, in any water which may be contaminated with potash liquors by leaks or entrainment. potassium should be determined separately as described in Chap. XIV, 10. ANALYSIS The methods are taken from various sources, following in many cases those of the Association of Official Agricultural Chemists. Make all determinations on water which has been freed from sus- pended matter by filtration. 142 METHODS OF ANALYSIS 3. TOTAL SOLIDS Allow the sample to stand until all sediment has settled, and filter if necessary to secure a perfectly clear liquid. Evaporate *500 ml (preferably more if the water is low in solids) in a weighed platinum dish on a water bath. Additional platinum and porcelain dishes may be used to hasten the evaporation, the various concen- trated portions being finally rinsed into the weighed platinum dish, with the aid of a "policeman" to remove crystallized salts. After evaporation to dryness, heat to constant weight at 105 C. in a constant temperature oven. Where the complete analysis is not required and the deter- mination of total solids alone is necessary, as in the case of the weekly samples of battery supply water, evaporate 100 ml as above, and dry at i05 C. 4. TOTAL SULPHATES Dissolve the residue from "3" in the least possible amount of distilled water, and acidify with 3-5 ml of dilute sulphuric acid (1:10). Evaporate first on the water bath, and then carefully at a ftemperature sufficiently high to expel the excess of sulphuric acid without loss. Heat finally to a redness which is barely visible in daylight until the residue is white ; cool, and weigh. This treatment is prescribed to destroy organic matter, and for the indirect determination of the sodium. Subtract from the weight of "total sulphates" the amount of calcium and magnesium (as sulphates) and of silica, and iron and aluminum oxides (as such) ; the remainder is considered to be sodium sulphate and is multiplied by .3238 to convert it to sodium (Na). 5. SILICA Moisten the residue from "4" with concentrated hydrochloric- acid and evaporate to dryness on a water bath. Moisten again with concentrated hydrochloric acid, cover the dish, and digest for 5 10 minutes on the bath. Add sufficient water to dissolve the salts and heat again on the bath until solution is complete. Filter, wash with hot water, dry, ignite, and weigh the silica (Si0 2 ). *The amount should be sufficient to give, if possible, 0.5 gram of total solids and in any case not less than 0.2 gram. A preliminary determination made by evaporating 50 ml of the water will show the amount required. fThe "radiator" recommended by Hillebrand is especially good for volatilizing sulphuric acid. See Chap. XXIII, 15. XVII. WATER 143 6. IRON To the filtrate from "5" add several milliliters of bromine water, or a few drops of concentrated nitric acid, and boil. Then cool somewhat, add enough hydrochloric acid to insure a total of 10 15 ml of strong acid, make slightly alkaline with ammonium hydroxide, and boil for a few moments. The ammonia should not lie iu such excess as to require long boiling to expel the most of it, nor is the expulsion of the whole of it necessary or desirable. Filter as soon as the precipitate settles, wash with hot water, ignite, and weigh as Fe 2 3 + A1 2 3 . Report the iron and aluminum together as iron. Multiply the weight of the precipitate by .6994 to obtain the iron (Fe) equivalent. 7. CALCIUM Heat the filtrate from " 6 " to boiling, and to the boiling solu- tion add gradually about 10 ml of ammonium oxalate solution. Filter after standing for at least one hour, wash two or three times with hot water, and determine gravimetrically as oxide or sulphate as described under "Limestone," Chap. XVI, 5. Multiply the weight of CaO by .7146, or of CaS0 4 by .2944 to convert to calcium (Ca). 8. MAGNESIUM To the filtrate from "7" add 10 ml of sodium ammonium phosphate or disodium hydrogen phosphate solution. After vig- orous stirring add ammonium hydroxide in considerable excess. After standing over night, filter, and wash with dilute ammonium hydroxide (ammonium hydroxide of 0.90 sp. gr. diluted to 10 times its volume). Char the paper slowly without allowing it to ignite, burn off the carbon over a gradually increasing flame, then apply a weak blast for a long time and repeat to constant weight. \V'i:h as Mg.,P.,0- and multiply by .2184 to convert to magne- sium (Mg). 9. CHLORINE REAGENTS (a) Sulphuric acid of about N/28 strength: This solution does not have to be standardized. (b) Sodium carbonate solution of about N/28 strength: This solution does not have to be standardized. 144 METHODS OF ANALYSIS (c) Potassium chromate indicator: Dissolve 5 grams of potassium chromate in water, add a solution of silver nitrate drop by drop until a slight permanent red precipitate is produced, filter, and dilute to 100 ml. (d) Standard sodium chloride solution: Several grams of C. P. sodium chloride are finely powdered and heated for five minutes, not quite to redness. When cold, 0.8243 gram is dissolved in water and made up to 500 ml. Each ml = 0.001 gram chlorine. (e) Standard silver nitrate solution: Dissolve about 5 grams of C. P. silver nitrate in water and dilute to 1 liter. STANDARDIZATION Transfer 25 ml of the standard sodium chloride solution to a porcelain dish, or a beaker standing on a white surface. Dilute with 75 ml of chlorine-free water. Add 1 ml of the potassium chromate, and introduce the silver nitrate from a burette until a faint red color of silver chromate remains permanent on stirring. Correct for the amount of silver nitrate necessary to give in 100 ml of chlorine-free water, with 1 ml of the chromate, the shade obtained at the end of the titration of the sodium chloride solution. From 2 or 3 of such titrations calculate the strength of the silver nitrate Solution. DETERMINATION To 100 ml of the water add a few drops of phenolphthalein. If a red color appears, titrate the carbonates thus indicated to bicarbonates with the sulphuric acid solution (a). If the water is acid to methyl orange, add the sodium carbonate solution (b), from a burette until the acidity is neutralized. Add 1 ml of the chromate and titrate with the standard silver nitrate. Correct for the amount of silver nitrate necessary to give in 100 ml of chlorine-free water, with 1 ml of the chromate, the shade obtained at the end of the titration of the sample. NOTE: Greater accuracy is secured by operating in yellow light. Gas or electric light is better than daylight. 10. SULPHURIC ACID Acidify 300 ml, or a suitable amount, of the water slightly with hydrochloric acid. Heat to boiling and add drop by drop 5 10 ml of a hot, 10 per cent barium chloride solution. After standing over night, filter, wash free from chlorine with hot water, XVII. WATER 145 ignite, and weigh as barium sulphate (BaSOJ. Add a drop of sulphuric and hydrofluoric acids before finishing the ignition; this will remove any silica, if present, and convert any reduced barium sulphide back to sulphate. Multiply by .4115 to convert to S0 4 . 11. CARBONIC ACID Carbonic acid (CO 3 ) is determined by difference, as the amount necessary to saturate the excess of basic over acid ions. 12. ORGANIC AND VOLATILE MATTER. This is taken as the difference between the "total solids" and the sum of the other constituents determined. 13. SUSPENDED MATTER This determination need not be made except in the case of raw waters for new factory sites or of other waters where the amount is visibly excessive. Determine by making a total solids determina- tion on the unfiltered water, being careful that the sample is well mixed so that the portion taken will contain its proper proportion of insoluble matter. The difference between the total solids deter- mined in this manner and determined as in "3" represents the amount of "suspended matter." Record the "suspended matter" as a separate figure and do not include in the "total solids" in the statement of the analysis. 14. HYPOTHETICAL COMBINATIONS R-eport the basic and acid ions and the hypothetical combina- tions in terms of parts per 100,000. In calculating the hypothetical combinations join the basic ions in the following order : potassium, sodium, magnesium, calcium, and iron, to the acid ions in the following order: chlorine, sulphuric acid, and carbonic acid. Report silica as free SiO 2 . 15. EXAMPLE An analysis showed the following (parts per 100,000) : Total Solids 45.22 Total Sulphates 50.26 SiO, 3.80 Fe 2 6 3 and A1 2 O 3 20 (X .6994 = .14 Fe) CaO 5.12 ( X -7146 = = 3.66 Ca) Mg 2 P 2 7 6.7T (X .2184 = 1.48 Mg) Cl 2.17 BaS0 4 29.74 ( X .4115 = 12.24 S0<) ' 146 METHODS OF ANALYSIS CALCULATION OF SODIUM 5.12 CaO X 2.4279 6.77 Mg a P 2 O 7 X 1.0810 50.26 (3.80 + .20 + 12.43 26.51 Na^SO, X .3238 7.32) 12.43 CaSO 4 = 7.32 MgS0 4 = 26.51 Na 2 SO 4 = 8.58 Na CALCULATION OF SALTS AND CARBONIC ACID 2.17 Cl X .6486 2.17 Cl + 1.41 Na 8.58 Na 1.41 Na 12.24 SO 4 X .4789 12.24 SO 4 + 5.86 Na 7.17 Na 5.86 Na 1.31 Na X 2.3045 1.48 Mg X 3.4673 3.66 Ca X 2.4975 .14 Fe X 2.0746 (3.02 + 5.13 + 9.14 -f .29) (1.31 = 1.41 Na 3.58 NaCI =r 7.17 Na (uncombined) = 5.86 Na 18.10 Na 2 SO 4 = 1.31 Na (uncombined) = 3.02 Na,CO 3 r= 5.13 MgCO 3 = 9.14 CaCO 3 = .29 FeCO, 1.48 + 3.66 + .14) 10.99 CO 3 16. STATEMENT OF ANALYSIS The above analysis will then be stated as follows: Silica SiO 2 Iron Fe Calcium Ca Magnesium Mg Sodium .Na Chlorine .Cl Sulphuric Acid SO 4 Carbonic Acid CO 3 Parts per 100,000 3.80 .14 3.66 1.48 8.58 2.17 12.24 10.99 Hypothetical Combinations 43.06 Organic and Volatile Matter (by difference) 2.16 Total Solids.. ..45.22 Parts per 100,000 Silica SKV Sodium Chloride NaCI Sodium Sulphate Na 2 SO 4 Sodium Carbonate Na 2 CO 3 Magnesium Carbonate. . .MgCO 3 Calcium Carbonate .CaCO 3 Ferrous Carbonate FeCO 3 3.80 3.58 18.101 3.02) 5.13 9.141 .29 43.06 Organic and Volatile Matter (by difference) ! 2.16 Total Solids . ..45.22- XVIII. DIATOMACEOUS EARTH (KIESELGUHR) For judging- the suitability of diatomaceous earth for filtra- tion work, no chemical analysis will probably be of as much value as an actual fitration test, but in most cases the apparent specific gravity will furnish a good index. The lower the apparent specific gravity, the better is the quality of the material. The silica deter- mination will give only a general idea of the purity. 1. SAMPLING Take an average sample of each lot received, mix well, and preserve a suitable amount in a stoppered bottle. 2. APPARENT SPECIFIC GRAVITY (POUNDS PER CUBIC FOOT) The weight per cubic foot is taken as the weight of the mate- rial which occupies one cubic foot of space under the conditions specified, without packing, and is obtained as follows : Shake the material through a 20 mesh sieve held 1 inch above the top of a 25 ml porcelain crucible of known weight and capacity, returning to the sieve the portion which falls outside the crucible, until the crucible is completely filled. Then level off with a spatula, avoiding any packing, and weigh to the nearest centigram. Make this determination in triplicate. If W = weight in grams of the material in the crucible, V == volume of the crucible in milliliters, and X == apparent spe- cific gravity of the material in "pounds per cubic foot," then _, 62.43 W ~^~ Or, if the crucible holds exactly 25 ml, tlu-n x 10 w 4 148 METHODS OF ANALYSIS 3. MOISTURE Heat 0.5 gram for 3 hours in a porcelain crucible in a drying oven at 100 105, and then for successive periods of one hour until the weight is constant. Report the loss in weight as moisture. 4. ORGANIC AND VOLATILE MATTER Heat the crucible containing the dried sample from "3" to full redness over a good burner or in, an electric furnace, and ignite to constant weight. The loss in weight of the dried sample represents the amount of "organic and volatile matter." 5. SILICA Mix 0.5 gram of the material thoroughly with 4 6 parts of sodium carbonate in a platinum crucible, and fuse. When the fusion is complete, allow to cool, and extract the melt with water and hydrochloric acid. Evaporate to dryness on the water bath, and proceed as in Chap. XIII, 2, repeating the evaporation and nitration until all the silica is removed. Ignite the residue to constant weight, using a blast lamp or electric furnace for the final ignition, and weigh as Si0 2 . XIX. SULPHUR 1. SAMPLING AND PREPARATION OF SAMPLE A laboratory employe should sample each car of sulphur re- ceived, by taking representative samples from different parts of the car. Crush the entire sample to V inch size with a jaw crusher. Mix the crushed sample, and reduce it by quartering. Grind to 60 mesh size in a mortar or on a bucking board, and preserve a suitable amount in a stoppered bottle. A disc pulver- izer is not suitable, because the friction heats the sulphur and causes it to become viscous. 2. MOISTURE Heat 1 gram for exactly one hour in a porcelain crucible in a drying oven at 100 105. Report the loss in weight as moisture. 3. ASH Heat the crucible containing the dried sample from "2" until the sulphur ignites, then remove the flame and allow the sulphur to burn. When combustion has ceased, heat to full redness to constant weight, cool, and weigh the residue. 4. SULPHUR (a) Method I: Weigh out about 0.1 gram and transfer to a flask of 250 ml capacity. Add 25 ml of a strong potassium hydroxide solution, and heat in a water bath until the sulphur is all dissolved (about one-half hour is required). Cool, add 200 ml of freshly prepared bromine water and heat until the sulphur is all oxidized, adding more bromine water if necessary. Transfer to a beaker, make slightly acid with hydrochloric acid and boil until the excess of bromine is expelled, then filter and 150 METHODS OF ANALYSIS wash with hot water. Precipitate the sulphuric acid in the filtrate with barium chloride, following the procedure in Chap. XIII, 8. (b) *Method II: Dissolve about 0.1 gram in 1 ml of dry liquid bromine and, add 10 ml of concentrated nitric acid. Re- move the excess of bromine and the nitrous fumes by heat, add 100 ml of water and several ml of hydrochloric acid, and boil to expel the rest of the nitric acid. Then precipitate the sulphuric acid with barjum chloride in the regular manner. 5. ARSENIC Test qualitatively for arsenic as follows : Shake approxi- mately 1 gram of the ground sample with 15 drops of strong ammonium hydroxide and 2 ml of water. Filter after half an hour, and to the clear filtrate in a test tube add 30 drops of con- centrated hydrochloric acid and 15 drops of a 10 per cent solution of oxalic acid. Place a strip of bright copper foil in the solution and heat to 60 100 ; in the presence of arsenic an iron-colored to black film forms immediately on the copper. If the presence of arsenic is indicated, always check the reagents by a blank test. *Bjerregaard, Jour. Ind. and Eng. Chem., 11, 1055. XX. FOODS AND FEEDING STUFFS The methods are in general those of the Association of Official Agricultural Chemists. 1. PREPARATION OP SAMPLE Grind the sample so that it will pass through a sieve having circular openings 1/25 inch (1 mm) in diameter. If the sample cannot be ground, reduce it to as fine a state as possible. Deter- mine moisture in both the original and the ground sample, and correct the results of the analysis for any change in the moisture content during grinding. 2. MOISTURE Weigh out 10 grams in a 3 x % inch aluminum dish, provided with a cover, and dry in vacuo at 100 105 for 3 4 hours, and then for successive periods of one hour until the loss of weight in one hour is not over 0.1%. 3. CRUDE PROTEIN Determine nitrogen by one of the following methods, and multiply the result by 6.25 to convert to protein. KJELDAHL METHOD REAGENTS For ordinary work N/2 acid is recommended. For work in determining very small amounts of nitrogen N/10 acid is recom- mended. In titrating mineral acids against ammonium hydroxide solution use cochineal or methyl red as indicator. (a) Standard sulphuric acid: Determine the absolute strength of the acid by precipitation with barium chloride solution as follows : Dilute a measured quantiy of the acid to be stand- ardized to approximately 100 ml, heat to boiling and add drop by 152 METHODS OF ANALYSIS drop a 10% solution of barium chloride until no further precipi- tation occurs. Continue the boiling for about 5 minutes, allow to stand for 5 hours or longer in a warm place, pour the super- natant liquid on a tared Gooch or on an ashless filter, treat the precipitate with 25 30 ml of boiling water, transfer to the filter and wash with boiling water until the filtrate is free from chlorine. Dry, ignite over a Bunsen burner and weigh as barium sulphate. See also Chap. XXV, 21 (a) (3). A normal solution of sulphuric acid has the following equivalents : 1 ml = .04904 gram H 2 S0 4 1 ml = .01401 gram N 1 ml = .01703 gram NH 3 (b) Standard alkali solution: Accurately determine the strength of this solution by titration against the standard acid. N/10 solution is recommended. (c) Sulphuric acid: Of sp. gr. 1.84 and free from nitrates and ammonium sulphate. (d) Metallic mercury, or mercuric oxide: Mercuric oxide should be prepared in the wet way, but not from mercuric nitrate. (e) Copper sulphate: Crystallized. (f) Potassium permanganate: Finely pulverized. (g) Granulated zinc or pumice stone: Added to the con- tents of the distillation flask if necessary to prevent bumping. (h) Potassium sulphide solution: Dissolve 40 grams of commercial potassium sulphide in 1 liter of water. (i) Sodium hydroxide solution: A saturated solution, free from nitrates. (j) Cochineal solution: Digest, with frequent agitation, 3 grams of pulverized cochineal in a mixture of 50 ml of strong alcohol and 200 ml of water for 1 or 2 days at ordinary tempera- ture, and then filter. (k) Methyl red solution: Dissolve 1 gram of methyl red (dimethyl-amino-azo-benzene ortho-carbonic acid) in 100 ml of 95% alcohol. APPARATUS (a) Kjeldahl flasks for both digestion and distillation: Total capacity of about 550 ml, made of hard, moderately thick, and well-annealed glass. XX. POODS AND FEEDING STUFFS 153 (b) Distillation flasks: For distillation any suitable flask of about 550 ml capacity may be used. It is fitted with a rubber stopper through which passes the lower end of a Kjeldahl con- noting bulb to prevent sodium hydroxide being carried over mechanically during distillation. The bulb should be about 3 cm in diameter, and the tubes should be of the same diameter as the condenser tube with which the upper end of the bulb tube is con- nected by means of rubber tubing. DETERMINATION Place 0.7 3.5 grams, according to the nitrogen content, of the substance to be analyzed in a digestion flask with approximately 0.7 gram of mercuric oxide, or its equivalent in metallic mercury, and add 20 30 ml of sulphuric acid 0.1 0.3 gram of crystallized copper sulphate may also be used in addition to the mercury, or in place of it). Place the flask in an inclined position and heat below the boiling point of the acid until frothing has ceased. (A small piece of paraffin may be added to prevent excessive foaming. ) Then raise the heat until the acid boils briskly and digest for a time after the mixture is colorless or nearly so, or until oxidation is complete. Remove the flask from the flame, hold it upright, and while still hot add carefully potassium permanganate in small quantities at a time until, after shaking, the liquid remains green or purple. After cooling dilute with about 200 ml of water, add a few pieces of granulated zinc or pumice stone, if necessary to prevent bumping, and 25 ml of potassium sulphide solution with shaking. Next add sufficient sodium hydroxide solution to make the reaction strongly alkaline (50 ml is usually enough) pouring it down the side of the flask so that it does not mix at once with the acid solu- tion. Connect the flask immediately with the condenser, mix the contents by shaking, distil into a measured quantity of the standard acid until all ammonia has passed over, and titrate with the stand- ard alkali. The first 150 ml of the distillate will generally contain all the ammonia. The use of mercuric oxide in this operation greatly shortens the time necessary for digestion, which is rarely over an hour and a half in case of substances most difficult to oxidize, and is more 'ommonly less than an hour. In most instances the use of potas- Hum permanganate is quite unnecessary, but it is believed that in xreptiomil cases it is required for complete oxidation, and in view of the uncertainty it is always used. The potassium sulphide 154 METHODS OF ANALYSIS removes all the mercury from the solution, and so prevents the formation of mercuro-ammoiiium compounds which are not com- pletely decomposed by the sodium hydroxide. The addition of zinc gives rise to an evolution of hydrogen and prevents violent bumping. Previous to use the reagents should be tested by a blank experiment with sugar. The sugar partially reduces any nitrates present that might otherwise escape notice. GUNNING METHOD REAGENTS Potassium sulphate: Pulverized. The other reagents and standard solutions used are described above. APPARATUS The apparatus used is described above. DETERMINATION Place 0.7 3.5 grams, according to the nitrogen content, of the substance to be analyzed in a digestion flask. Add 10 grams of powdered potassium sulphate and 15 25 ml (ordinarily about 20 ml) of sulphuric acid (0.1 0.3 gram of crystallized copper sulphate may also be added). Conduct the digestion as in the Kjeldahl process, starting with a temperature below the boiling point and increasing the heat gradually until frothing ceases. Digest for a time after the mixture is colorless or nearly so, or until oxidation is complete. Do not add either potassium per- manganate or potassium sulphide. Cool, dilute, neutralize, distil, and titrate with the standard alkali. In neutralizing before distil- ling it is convenient to add a few drops of phenolphthalein indi- cator or litmus paper. The pink color given by phenolphthalein indicating an alkaline reaction is destroyed by a considerable excess of strong fixed alkali. KjELDAHL-GuNNiNG- ARNOLD METHOD REAGENTS AND APPARATUS Described above. DETERMINATION Place 0.7 3.5 grams, according to the nitrogen content, of the substance to be analyzed in a digestion flask. Add 15 18 grams of potassium sulphate, 1 gram of copper sulphate, 1 gram of mercuric oxide, or its equivalent in metallic mercury, and 25 ml of sulphuric acid. Heat gently until frothing ceases, then boil the mixture briskly, and continue the digestion for a time after XX. FOODS AND FEEDING STUFFS 155 the mixture is colorless or nearly so or until oxidation is complete. Cool, dilute with about 200 ml of water, add 50 ml of potassium sulphide solution, make strongly alkaline with sodium hydroxide solution and complete the determination as directed in the Kjel- < la 111 method. 4. CRUDE FAT REAGENTS (a) Anhydrous Ether: Use particular care in the purifi- cation of the ether. Wash ethyl ether, containing not more than 4' , alcohol, with 4 or 5 successive portions of distilled water, add solid sodium or potassium hydroxide, and let stand until most of the water has been abstracted from the ether. Decant into a dry bottle and add small pieces of carefully cleaned metallic sodium. It will be found that a considerable quantity of sodium is needed to remove, the last traces of water although little of the sodium appears to be used up in the process ; the sodium should therefore be added on each of several different days until no more hydrogen is liberated from the fresh pieces. Keep the ether, thus dehy- drated, over metallic sodium in lightly stoppered bottles. Use glass stoppered, and not cork stoppered bottles. If a brown pre- cipitate develops, which indicates that the washing was incom- plete, repurify the ether. Test each lot of ether for insoluble resi- due by evaporating a measured volume. APPARAT Use an extraction apparatus attached to the flask by a ground id ass joint cr a mercury seal, and not by a cork or rubber stopper. Alunduni extraction shells are recommended. DETERMINATION Large quantities of soluble carbohydrates may interfere with the complete extraction of the fat. In such cases extract with \vater before proceeding with the determination. Dry about 2 grams of the material thoroughly in a drying oven at 100 105. Extract with the anhydrous ether for 16 hours. Filter the extract through filter paper to remove solid particles, usinjr ether for washing. Evaporate the extract and washings carefully to drynoss, and dry at 100 105 for 30 minutes, cool in a desiccator, a.ul weigh. Continue the drying by half-hour periods until a minimum weight is obtained. For most feeds a period of 1 to 1 1 /^ hours is required. Save the residue for the crude fiber determination. 156 METHODS OF ANALYSIS 5. CRUDE FIBER REAGENTS (a) 1.25% Sulphuric Acid Solution: Exact strength, de- termined by titration. (b) 1.25% Sodium Hydroxide Solution: Exact strength, determined by titration. DETERMINATION Extract a quantity of the substance, representing about 2 grams of the dry material, with ordinary ether, or use the residue from the determination of the ether extract. To this residue in a 500 ml flask add 200 ml of boiling 1.25% sulphuric acid; connect the flask with an inverted condenser, the tube of which passes only a short distance beyond the rubber stopper into the flask, or simply cover a tall conical flask, which is well suited for this determina- tion, with a watch glass or short stemmed funnel, boil at once and continue boiling gently for 30 minutes. A blast of air conducted into the flask will serve to reduce the frothing of the liquid. Filter through linen and wash with boiling water until the washings are no longer acid ; rinse the substance back into the flask with 200 ml of boiling, 1.25% solution of sodium hydroxide, free or nearly free from sodium carbonate, boil at once, and continue boiling gently for 30 minutes as directed above for the treatment with acid, filter at once rapidly, and wash with boiling water until the washings are neutral. The last filtration may be performed upon a Grooch crucible, a linen filter, or a tared filter paper. If a linen filter is used, rinse the crude fiber, after washing is completed, into a flat-bottom platinum dish by means of a jet of water; evapo- rate to dryness on a steam bath, dry to constant weight at 110 C., weigh, incinerate completely, and weigh again. The loss in weight is considered to be crude fiber. If a tared filter paper is used, weigh in a weighing bottle. In any case the crude fiber after drying to constant weight at 110 C. must be incinerated and the amount of the ash deducted from the original weight. 6. ASH Weigh out about 2 grams and determine ash by the lixiviation method as described in Chap. I, 7 (b). 7. NITROGEN-FREE EXTRACT Subtract from 100 the sum of the percentages of moisture, crude protein, crude fat, crude fiber, and ash. XXI. COTTON SEED CAKE Sample tach car of cotton seed cake received, and determine moisture and protein. 1. SAMPLING Take a *handful of cake from each of at least 25 bags selected promiscuously throughout the car, the total sample amounting to at least 10 pounds. If possible, sample a greater number of bags. Mix the sample, remove a quart with a scoop, and preserve in a suitable container as a reference sample for size only, and so labeled. 2. PREPARATION OF SAMPLES If the original sample exceeds 15 20 pounds, reduce to this amount, but not below, by halving or quartering; otherwise grind the entire remainder of the original sample on a bucking board, or by means of other suitable apparatus, to such an extent that the largest lumps will not exceed VL inch in size, mix thoroughly, and quarter once. Repeat the procedure of grinding and quar- tering until about 3 pints of material remain. Mix thoroughly nnd make up 3 samples of about 1 pint each, using fruit jars or other suitable, tightly sealed containers. Label each sample with the car number, date of receipt and the name of the factory where received. Retain two of the above samples as referee samples for analysis, subject to shipping instructions from the General Office. Use a third sample for the laboratory analysis, and seal and save for future reference the portion of this sample left over from the analysis. Prepare the sample for analysis by putting the entire sample through a sieve having circular openings 1 mm in diameter, grind- *The directions refer to "screened cracked cake." 158 METHODS OF ANALYSIS ing the portion retained by the sieve until all the particles pass through, then mix the sample thoroughly to destroy the segregation of the hulls, which are more difficult to reduce to the necessary degree of fineness, from the other portion of the sample. To avoid change in moisture content, grind the material as rapidly as possible and do not allow it to stand exposed to the air unneces- sarily. 3. ANALYSIS Determine moisture and protein as described below. The methods are, with some unimportant modifications in wording, those of the Interstate Cotton Seed Crushers' Association. 4. MOISTURE Heat 2 to 5 grams for 3 hours in an oven at a temperature of 100 C., using an aluminum dish 2 inches in diameter, provided with a cover. As soon as the dish is removed from the oven, cover and cool in a desiccator. Report the loss in weight as moisture. 5. PROTEIN Digest 1.7512 grams of the sample with approximately 0.5 gram of metallic mercury or 0.7 gram of mercuric oxide, 10 grams of sodium or potassium sulphate, and 25 ml of sulphuric acid (sp. gr. 1.84). Place the flask in an inclined position and heat below the boiling point of the acid from 5 to 15 minutes, or until frothing has ceased. Increase the temperature and continue digestion until the liquid becomes colorless, or until complete digestion is obtained. The process is the same from now on as in the regular Kjeldahl method, except that no potassium permanganate is added. Distillation: After cooling, add about 300 ml of distilled water, a few pieces of zinc to keep the contents of the flask from bumping, and 25 ml of a 4% solution of potassium or sodium sul- phide, or a sufficient amount to precipitate all the mercury. After mixing thoroughly, add 60 ml of a sodium hydroxide solution of 1.50 sp. gr., or sufficient to make strongly alkaline, pouring it down the side of the flask so that it does not mix at once with the acid solution. Connect the flask with a condenser of glass or block tin, mix the contents of the flask by shaking and distil into an accurately measured quantity of standard sulphuric acid solution XXI. COTTON SEED CAKE 159 (N/2 recommended) to which has been added 50 ml of distilled water, until at least 200 ml of distillate is obtained, taking care that the delivery tube reaches below the level of the standard acid. Then titrate the distillate with standard fixed alkali solution (N/4 sodium hydroxide recommended). To obtain the percentage of protein, multiply the number of milliliters of acid neutralized by the distillate by 2.5, if the acid is of exactly N/2 strength. The factor for the conversion of nitrogen to protein is 6.25. Precautions: Be sure that the sample for analysis has been ground to pass a 1 millimeter sieve, as prescribed in "2." Test the reagents by a blank experiment with sugar, and make any correction found necessary. Consult Chap. XX, 3, for fuller details regarding the protein determination. XXII, SOIL The methods are in the main those of the Association of Offi- cial Agricultural Chemists, which should be consulted for full details. Make only the determinations mentioned below. If possible there should be recorded with each analysis a history of the soil, covering crop rotation, extent of manuring, the depth of the soil if less than 12 inches, and the nature of the subsoil. 1. SAMPLING OF SOIL Sampling should be done preferably when the soil is rea- sonably dry. Remove from the surface all vegetable material not incorporated with the soil, and take out an amount about one square foot in section to the depth of the plowed soil; if virgin soil is sampled, sample to a depth of 6 inches, but not below the level of the subsoil. Mix on an oil cloth ; if too wet, let it dry but not to form clods. Do this in different parts of the field, and take equal amounts of the individual samples. Mix the composite sample thoroughly, reduce by quartering to about 2 4 pounds, and air-dry in a cool, well-ventilated place. If the soil is less than 6 inches deep, take and analyze a separate sample of the subsoil. 2. PREPARATION OF SAMPLE Follow the method of the A. 0. A. C. 3. MOISTURE, VOLATILE MATTER, AND TOTAL NITROGEN Follow the methods of the A. 0. A. C. The moisture found in the air-dry soil is reported as "hygroscopic moisture." XXII. SOIL 161 4. MISCELLANEOUS INORGANIC CONSTITUENTS .Make a stiong acid digestion of the soil and determine, accord- ing to tin- A. 0. A. C. methods: (a) Insoluble residue. (b) Iron, aluminum, and phosphoric acid (collectively). (c) Manganese. (d) Calcium. (e) Phosphoric acid. (f) Sulphuric acid. (g) Potassium, (h) Sodium. 5. CARBON DIOXIDE Liberate the carbon dioxide with acid and determine by the increase in weight of a potash bulb, as in Chap. XIV, 16. 6. HUMUS Place 10 grams of the sample in a Gooch crucible, extract with \ r /t hydrochloric acid until the filtrate gives no precipitate with ammonium hydroxide and ammonium oxalate, and remove the acid by washing with water. Wash the contents of the crucible (including the asbestos filter) into a glass stoppered cylinder, with 500 ml of 49 ammonium hydroxide, and allow to remain, with occasional shaking, for 24 hours. During this time the cylinder is inclined as much as possible without bringing the contents in contact with the stopper, thus allowing the soil to settle on the side of the cylinder and exposing a very large surface to the action of the ammonium hydroxide. Place the cylinder in a vertical position and leave for 12 hours, to allow the sediment to settle. Filter the supernatant liquid (the filtrate must be perfectly clear), evaporate an aliquot, dry at 100, and weigh. Then ignite the residue and again weigh. Calculate the humus from the difference in weights between the dried and ignited residues. 7. WATER SOLUBLE Transfer 50 grams of the air dried soil, with 500 ml of water, to a 1000 ml tiask, boil for half an hour, and let stand for 24 hours with occasional shaking. Then make up to the mark, filter, evaporate an aliquot, and dry at 100 105 to constant weight. 162 METHODS OF ANALYSIS 8. MECHANICAL ANALYSIS (*T.'B. Osborne's Method) The details of this method will be given with sufficient minute- ness to make its practice possible by all analysts. Selecting the Sample: Several pounds of air-dried, fine earth are secured by passing the soil through a sieve, the holes of which are three millimeters in diameter. Sifting: Thirty grams of the above fine earth are stirred with from 300 to 400 milliliters of water and then thrown suc- cessively; upon sieves with circular holes of 1, 0.5, and 0.25 milli- meter diameter respectively. By means of successive additions of water and the use of a camel's hair brush, all the fine material is made to pass through the sieves and these at the last are agi- tated under water in a shallow dish in such a way that the soil is immersed. The finest sieve should be well wet with water on its lower surface just before using. The finest particles which render the water turbid are easily washed through. The turbid water is kept separated from the clear water which comes off with the last portions that pass the sieves. The turbid water usually does not amount to more than one liter. Elutriation: The elutriation should be carried on so as to secure three grades of silt; the diameters of the particles ranging in the first grades from 0.25 to 0.05 millimeter, in the second grade from 0.05 to 0.01 millimeter, and in the third grade from 0.01 millimeter to the impalpable powder. The term sand is applied to the first grade, silt to the second, and dust or dust and clay to the third. After the turbid liquid from the sifting has stood a short time it is decanted from the sediment and after standing until a slight deposit is formed, is again decanted and the sedi- ment examined with a microscope. If sand is present, the sub- sidence of the turbid liquid is continued until no more sand is deposited. As the sand subsides rapidly there is no difficulty in altogether freeing the liquid first decanted from this grade of particles. The sediment thus obtained contains all the sand, a part of the dust and much silt. As only dust and the finest silt render the water turbid the sediment is stirred a few times with a fresh quantity of water and decanted after standing long *From Wiley's "Principles and Practice of Agricultural Analysis," 2d ed., Vol. 1, p. 212. xxn. SOIL 163 enough to let all the sand settle. When the water decanted is free from turbidity, the last portions of the soil passing through the sieve with clear water are added to the sediment arid the decantations continued so as to remove most of the silt. When no more silt can be easily removed from the sediment without decanting sand, the decantations are made into a different vessel and the subsidences so timed as to remove as much of the silt as possible. By using a little care, at least three-quarters of the sand are thus obtained free from silt. The rest of the sand is mixed with the greater part of the silt which has been decanted into the second vessel. The size of the smallest particle in this vessel is determined with the microscope, to make sure that its contents are free from dust as they usually will be if, after settling for a few moments, they leave the water free from turbidity. The soil is thus separated into three portions, one -containing sand, one sand and silt, and the other silt, dust, and clay. The sand and silt are separated from each other by repeating the subsidences and decantations in the manner just described. In this way there is removed from the sediment, on the one hand, a portion of silt free from sand and dust, and on the other hand a portion of sand free from silt. Thus is obtained a second intermediate portion consisting of sand and silt, but less in amount than the first and containing particles of diameters much more nearly approaching 0.05 millimeter. By repeating this process a few times, this intermediate portion will be reduced to particles whose diameters are very near 0.05 millimeter and which may be divided between sand and silt, according to judgment. The amount of this is usually very small. As soon as portions are separated, which the microscope shows to be pure sand or pure silt, they are added to tha chief portions of these grades already obtained. The same process is applied to the separation of silt from dust. When all the silt has been removed from the dust and clay, the turbid water containing the dust and clay is set aside and allowed to settle in a cylindrical vessel for twenty-four hours. The vessel is filled to a height of 200 millimeters. According to Hilgard, the separation of the dust from clay during a subsidence of twenty-four hours, will give results of sufficient accuracy, although the clay then remaining suspended will not be entirely 164 METHODS OF ANALYSIS free from measurable fine particles up to 0.001 or 0.002 millimeter diameter. Small beakers and small quantities of distilled water are used at first for the decantations, as thus the duration of subsidence is less and more decantations can be made in a given time than when larger quantities of water are employed. Beakers of about 100 milliliters capacity are convenient for the coarser grades, but it is necessary to use larger vessels for the fine sediments from which turbid water accumulates that cannot be thrown away, as may be done with the clear water, from which the coarse sediments settle out completely in a short time. It is best to keep the amount of water as small as possible in working out the dust since loss is incurred in using too large quantities. It is also necessary in most cases to subject the various frac- tions obtained during elutriation, to careful kneading with a soft rubber pestle so that the fine lumps of clay may be broken up and caused to remain suspended in the water. This treatment with the pestle should be done in such a way as to avoid as far as possible all grinding of the particles, the object being merely to pulverize the minute aggregations of clay and extremely fine particles which always form on drying a sample of soil after removing it from the field. Measurement of the Particles: To determine the size of par- ticles in suspension, a small glass tubs is applied to the surface of the liquid in such a way as to take up a single drop which is transferred to a glass slide. This drop will contain the smallest particles in the liquid. To obtain a sample of the coarsest particles, the liquid is allowed to stand long enough to form a very slight sediment, and a portion of this sediment is collected with a glass tube. To determine the diameter of the particles in a sediment, it is stirred vigorously with a little water and the pipette at once applied to the surface of the water. On decanting the greater part of the sediment, the large particles remain at the bottom of the beaker and may be easily examined. Time: The time required to make the separations, above described, is about two hours for each, so that an analysis includ- ing the siftings, is made in five or six hours, exclusive of the time necessary for collecting the dust and separating the clay, for which a subsidence of 24 hours is allowed. xxii. SOIL 165 \\'i only of relative value. For this determination a Hilgard "sieve cylinder," which can be obtained from dealers in chemical apparatus, is used. It is a metal cylinder, open at the top and closed at the bottom by a fine wn The cylinder rests in a ring 2 cm high provided at the sides with holes which allow free access of water when immersed in a beaker containing water. The wire screeen is cov- -ivd inside with a fine, circular linen cloth. The cylinder is 16 cm deep x 4 cm in diameter, so that its contents amount to 200 cubic centimeters. 166 METHODS OP ANALYSIS Before the test moisten the linen cloth, and weigh the appara- tus together with a small porcelain dish in which it stands. Then fill the cylinder up to the rim with the air-dry soil, adding it gradually with continual shaking until no further settling is noticeable. Then level with a spatula and weigh again. Place the cylinder in a good sized beaker, containing enough water at room temperature to submerge the sieve bottom of the cylinder to the -extent of 5 to 10 millimeters, and cover the entire apparatus with a glass bell jar to prevent evaporation. The time required to reach the maximum water absorption will vary with the nature of the soil. As soon as moisture appears at the surface, take out the cylinder, allow it to drain for a few moments, wipe the outside, place it in the porcelain dish originally used, and weigh. Put the cylinder back in the water for some time and weigh again, repeating this procedure until the weight is constant, or nearly so. Calculate the increase in weight as the percentage on the weight of the air-dry soil. 10. STATEMENT OF ANALYSIS Calculate all the results of the chemical analysis as percent- ages of the soil dried to constant weight at the temperature of boiling water, and report in the order given. Under "physical analysis" express the results as percentages on the air-dry soil. CHEMICAL ANALYSIS % on Moisture- free Soil Insoluble residue Lime (CaO) Carbon dioxide (CO,) Potash (K 2 0) Soda (Na 2 0) Iron and aluminum oxides (Fe 2 3 & A1 2 3 ) Manganese oxide (Mn 8 4 ) Phosphoric acid (P 2 3 ) Sulphuric acid (S0 3 ) Volatile matter Humus Total nitrogen Water soluble xxn. SOIL 167 PHYSICAL ANALYSIS % on Air- Dried Soil Hygroscopic moisture Water capacity Temperature of absorption (C.) Coarse sand. 1.0 0.5 mm Medium sand, 0.5 0.25 mm. Fine sand, 0.250.05 mm Silt, 0.050.01 mm Dust, less than 0.01 mm XXIII. APPARATUS In addition to the data given in this chapter, many articles and arrangements of apparatus will be found described in con- nection with the directions for particular determinations. 1. BALANCES Analytical balances of the standard grade and sensibility should be employed. Pulp balances should be rugged in con- struction and sensible to 2 milligrams. 2. BEET RASP A rasp of the Keil-Dolle type is employed for the samples handled in the beet laboratory. This rasp removes a true radial segment from each beet and at the same time reduces it to a very fine pulp suitable for analysis by the cold water method. It has been found by a great number of tests that the portion of the beet removed by a rasp of this kind is on the average a very accu- rate sample of the whole beet. Special directions regarding the care and use of this rasp will be found in detail in Chap. XII, 2 and 3. 3. CAPSULES AND COVERS FOR ANALYSIS OF BEETS Metal cups, so-called "capsules," are employed in the deter- mination of sugar in the beet by the cold water digestion method. They are all adjusted to the same tare by grinding or by adding solder, and should be made of Monel metal (or nickel), as other common metals will be attacked by the lead acetate solution and the tare will, as a result, change rapidly. The capsules should be about 3 in. dia. x 3 in. high, or of about 350 ml capacity. The cover consists of an aluminum disc, 4^ in. dia. x % in. thick, which has a hole 1-% in. in diameter at the center, and over XXIII. APPARATUS 169 it is stretched a rubber envelope. When the cover is placed on the capsule, the rubber is pressed with the thumbs downward through the central opening. On releasing the pressure a slight vacuum is created, which holds the cover on firmly ; this makes an air-tight joint which prevents evaporation, and also loss of the contents if the capsule is accidentally knocked over. 4. CARBONATOR For carbonating saccharate, a carbonator of familiar construc- tion is employed. It should have means for injecting steam and carbon dioxide gas, which, for convenience and to avoid local over- heating of the juice, should preferably be introduced through connections at the bottom rather than through pipes running down through the liquid. 5. COOLER The laboratory cooler is a working model of the factory coolers. No particular description is necessary. See section 17 for the speeds of the various pulleys. Care should be taken to avoid wet- ting the bolter screen. When it becomes stopped up, the bolter should be removed and the screen cleaned by washing it first with hydrochloric acid, then with water, and drying in a warm place. 6. DISHES FOR MOISTURE DETERMINATIONS Aluminum dishes 2 in. dia. x I 1 /-.* in. high should be employed for dry substance determinations in general ; for dried pulp alu- minum dishes 3 in. dia. x "< in. high should be used. Each dish should have a loosely fitting aluminum cover provided with a knob of the same material, and both the dish and the cover should be numbered with a die. 7. DRYING OVENS Electric ovens, even those of the best make, fall far short of the requirement of uniform temperature, as one will commonly find variations of 10 20 not only at different levels but also at different points on the same shelf. They are accordingly not to be recommended except possibly for drying empty dishes. 170 METHODS OF ANALYSIS A double walled oven of suitable construction, the jacket of which is filled with a boiling glycerin solution, will give a tem- perature which is uniform within 2 to 3 degrees in all parts of the oven, provided the dishes are placed on shelves and not directly on the bottom of the oven. This type of oven is accordingly recommended for dry substance determinations. The glycerin solution should be of such a strength that the required temperature (commonly 100 105) will be maintained in the interior of the oven. For 630 mm barometric pressure (5000 feet elevation) a mixture of about 3 parts of glycerin and 1 part of water, which has a density of about 42 Brix, will give approximately the desired concentration. The boiling point of the glycerin solution should be kept constant by means of a reflux condenser. It will occasionally be necessary to add a little water ta replace the water which is lost by evaporation and is not caught by the condenser. 8. EVAPORATOR An open evaporator heated by a steam chamber at the bot- tom is the type of laboratory evaporator recommended and commonly employed. 9. GRINDING MACHINERY For grinding cossettes employ an Enterprise Meat Chopper No. 41, with a plate containing % inch perforations, and running at the rate of 300 R. P. M. For grinding pulp use a second machine of the same description. For preparing for analysis samples of material such as lime- stone, boiler house ashes, etc., a combination of a jaw crusher with a disc pulverizer is very satisfactory. Material of great hardness, such as coke, must not be ground in a disc pulverizer on account of the contamination which will affect the sample. Large samples of coal are ground in a pebble mill, by means of which they may be ground to the necessary fineness during a long period of time without important loss of moisture. The mill for this purpose has a cast iron jar 18 x 18Vi> in., which should revolve at the rate of 40 50 R. P. M., and should contain 100 pounds of smooth, best grade flint pebbles. Inspect the contents occasionally for the presence of broken pebbles, which should be removed and discarded. XXIII. APPARATUS 171 10.. HYDROMETERS. Laboratory Brix hydrometers should have a total length of about 12 inches and a range of 6 Brix each, starting at 6 and up to and including 72 78. The scale should be graduated in one-tenths of one degree Brix and should cover a distance of not less than 4 1 /4 inches on the stem. Baume hydrometers, for testing molasses, should have enclosed thermometers, should have ranges of 30 40 and 40 50 degrees Baume, a total length of 13 inches, a scale length of 4% inches, and should be graduated in one-tenths of one degree Baume. The standard temperature for both Brix and Baume hydrometers is 20. All laboratory hydrometers must be verified as described in Chap. XXIV, 3, and any more than 0.1 degree in error at any point must be rejected or readjusted. 11. HYDROMETER JARS The hydrometer jars used with the laboratory Brix hydro- meters should be 12 inches long and 2 inches in diameter (inside dimensions) . 12. PLATINUM, CARE OF In making ignitions or fusions in platinum vessels by means of the Bunsen burner, only the upper non-luminous cone of the flame should be employed, and not the inner cone, nor should a smoky flame be used, as the action of a flame containing free car- bon will result in the formation of a carbide of platinum, causing the metal to become brittle. At the best a tarnish will gradually develop, which should be removed by gentle rubbing with moist sea sand, the grains of which are rounded and do not scratch the metal. Platinum ware should be kept polished in this manner, as the tarnish increases more rapidly upon already tarnished surface*, and will eventually lead to corrosion and cracking. Platinum surfaces may also be cleansed by fusing borax upon them and by digestion with nitric acid. The following precautions should be observed in the use of platinum utensils: (a) Platinum is insoluble in any single acid, but is readily Milublr in a mixture of hydrochloric and nitric acids (aqua regia). (b) Fusions in which the hydroxides of sodium, potassium, or barium are used should not be performed in platinum. 172 METHODS OF ANALYSIS (c) All metals which may be reduced in a fusion espe- cially compounds of lead, bismuth, tin, and other metals easily reduced and melted and all metallic compounds with reducing agents form fusible alloys with ignited platinum. Mercury, lead, bismuth, tin, antimony, zinc, etc., are liable to be rapidly reduced and immediately melt away platinum in contact with them. (d) Free chlorine and bromine attack platinum at ordinary temperature, and free sulphur, phosphorus, arsenic, and iodine attack ignited platinum. Operations in which these elements are set free should not be performed in platinum. Hence the fusion of sulphides, sulphates, and phosphates with reducing agents should be avoided, and care should be exercised in igniting phosphates in the presence of carbon from burnt filters. 13. POLARISCOPES (SACCHARIMETERS) No detailed explanation of the theory and construction of polariscopes will be given here, as this subject will be found treated at length in the various textbooks. See for example Browne's "Handbook of Sugar Analysis" and Circular 44, " Polarimetry, " of the Bureau of Standards. While the sugar chemist is advised to let the optical parts of the instrument alone as far as possible, it is desirable that he have a full understanding of the principles relating to the construction and use of saccharimeters. A few points are discussed below to which it is desired to direct special attention. (a) SPECIFICATIONS The type of polariscope to be preferred for general laboratory control work is the double field, single compensation, 400 mm tube length, mounted on a trestle support. The *report of the com- mittee of the American Chemical Society covers in great detail the desirable features of a commercial saccharimeter. (b) SACCHARIMETRIC SCALE AND NORMAL WEIGHT The 100 degree point is defined as the scale reading given by the polarization of the "normal weight" of pure sucrose, weighed in air with brass weights, and dissolved in water and made up to a volume of 100 ml at 20, the temperature of the solution and of the optical parts of the instrument during polariza- tion being 20. The "normal weight" at present most commonly in use, and the standard employed in this book, is 26 grams. See also Chap. XXIV, 7 (a). *Jour. Ind. & Eng. Chem, 12, 440. XXIII. APPARATUS 173 (c) VERIFICATION OF SCALE See Chap. XXIV, 7 (a). When the accuracy of the scale has once been established, it suffices for ordinary purposes to keep the instrument in adjustment at the zero point and to check it occasionally with standard quartz plates. The Chief or Assistant Chemist should check the setting of the zero point at least twice a shift, and oftener if it appears desirable. (d) EFFECT OF TEMPERATURE ON POLARIZATION The polarization of a pure .sugar solution decreases by about .03% for each degree increase in temperature. If the solution, when made up to volume and polarized at a given temperature (t), shows a polarization of S t , the polarization of 20 (S 20 ) is given by the following formula : S 2ft = S t + .0003 S t (t 20) If the solution is made up to volume at 20 but is polarized in a glass tube at some other temperature, the temperature coefficient in the formula becomes .0006 instead of .0003 ; plainly this pro- cedure will only increase the liability of error. On the other hand if the solution is both made up and polarized at 20 while the polariscope is at some other temperature, the temperature coef- ficient is that for the instrument alone, which is given by Schonrock as ..000148 for the ordinary quartz wedge saccharimeter with nickelin scale, and as .000138 if the scale is of glass. In the case of an impure sugar solution, the temperature coefficient is equal to the algebraic sum of the various influences, including those of the associated impurities, and may be more or less than the value for pure sugar, which it is therefore unsafe to apply in the polarization of an impure solution. According to *Browne the temperature coefficient for the direct polarization of beet molasses is almost negligible, and for raw beet sugars is about the same as for pure sucrose. While work of the highest precision demands the use of a constant temperature room which can be kept at exactly 20, sufficiently accurate results for ordinary control work are obtained by making up and polarizing the solutions at room temperature. It follows, however, that the room temperature should be kept as close to 20 as the heating and ventilating arrangements will *Jour. Ind. & Eng. Chem., 1, 567. 174 METHODS OF ANALYSIS permit. The accuracy can be increased by making up and polariz- ing the solutions at 20, in which case, if the room temperature is not .20, the only correction is that due to the temperature coefficient of the saccharimeter, which, as given above, is not great and is a fairly definite figure for any single instrument; this pro- cedure is not adapted for a large volume of work but is applicable in special cases. As the specific rotation of inverted solutions varies greatly with the temperature, all such solutions must be made up and polarized at exactly 20. (e) INSTALLATION The saccharimeter should be installed in a "polariscope box" of the customary construction, which should have a partition at the rear with a small hole at the proper height for illuminating the instrument without allowing bright light to strike the ob- server's eye, should be painted a dead black on the inside, and should be provided with a dark curtain at the front, open end to exclude outside light. The location should be free from excessive heat or cold drafts, and as little subject as possible to undue varia- tions in temperature. ( f ) ILLUMINATION A Mazda C stereopticon lamp is the most satisfactory source of illumination. A finely frosted glass plate should be fastened so as to cover the opening in the partition of the polariscope box and the lamp should be placed as close behind this as possible. The lamp should be clamped on a firm bracket, or support, which has means for vertical and lateral adjustment. To avoid shifting of the zero point it is essential that the instrument be kept in alignment with the source of illumination, and for this purpose not only should the lamp be firmly mounted but the polariscope should also be kept in a fixed position by means of bolts or strips of wood, etc. Particular care should be taken to adjust the position of the lamp so that the brightest portion is in alignment with the optical axis of the saccharimeter. Electric lamps will darken with use, and, when this has taken place to such an extent that the illumination is insufficient, they should be discarded. The instrument should never be placed so close to the source of light as to permit overheating to take place and hence possible xxra. APPARATUS 175 damage to the optical parts. The rule is that the polariseope should be placed at such a distance from the source of light that the image of the latter is clearly defined upon the analyzer dia- phragm; this is best accomplished by fastening a needle or other sharp pointed object at the source of light (the frosted glass plate) and changing the position of the instrument until a clear inverted image of the point is obtained upon a piece of white paper placed before the analyzer diaphragm. The distance of Schmidt & Haensch instruments from the source of light is given by the manufacturers as 150 millimeters ; it is also directed by them that, in the case of their 1909 model instrument provided with the "Blendrohr," when the light filter is in place the sleeve containing the condensing lens must be drawn out to the extent of 8.9 mm, i. e., up to the engraved mark, and the distance of the condensing lens from the source of light must then be adjusted to 150 mm. (g) LIGHT FILTER It is important that a light filter be constantly used. A com- mon arrangement consists of a cell containing a solution of potas- sium dichromate. If "a" is the length of the cell in centimeters and "b" is the percentage strength of the dichromate solution, the proper value of the latter is found from the formula For example, if the cell is 3 cm long, a 3% solution must be used. In some instruments a glass plate is employed as a light filter, and in one make of saccharimeter means are provided by which a light filter of this kind may readily be thrown in or out of the optical system; in this case readings should always be made with the light filter in place except in the case of a very dark solution which contains enough coloring matter to serve as its own light filter. (h) TUBES AND COVER GLASSES In filling a tube for polarization, it is customary to rinse it first two or three times with the solution, then to fill it, put the cover glass in place, and attach the cap. The caps should not be screwed on too tight, as the strain on the glass thereby created may cause optical rotation. Metal tubes are satisfactory for ordinary work, but they should be examined and tested frequently to see that they do not 176 METHODS OF ANALYSIS become bent. See Chap. XXIV, 7 (b). Glass tubes are free from this drawback. Cover glasses must be kept clean and dry. It is impossible to do accurate work with smeary cover glasses. Scratched glasses should be discarded. (i) CARE AND ADJUSTMENT OF POLARISCOPES As an almost inflexible rule, the adjusting of the polariscope should be limited to the setting of the zero point, as mentioned under (b), and to careful cleaning of the splash glasses and ex- posed lenses. The half-shadow angle, which is fixed, or not readily adjust- able, in most commercial saccharimeters, represents a compromise between maximum sensibility and sufficient illumination for polar- izing dark solutions; a decrease of the half-shadow angle results in increased sensibility but in decreased illumination. It varies from about 6 to 9 angular degrees in most commercial instruments, and may be determined by measuring the interval in sugar degrees between the points of maximum light extinction on each side of the zero point, and then multiplying by .3466 to convert to angular degrees. If it is necessary to change the half -shadow angle, this may be do>ne, in instruments provided with the Lippich polarizing system, by rotating the large polarizing Nicol to a new position, and then, with the quartz wedge scale set at zero, rotating the analyzer till the two halves of the field show equality of brightness, or very nearly so; the zero point may then be adjusted, if neces- sary, by the usual arrangement for changing the position of the vernier. 14. PRESSES Hydraulic presses, operated at a standard pressure, must be employed to obtain the juice from ground beets or cossettes for the determination of apparent purity. The standard pressure to be used upon the ground material is 240 Ibs. per sq. in., and the corresponding gage pressure for different types of presses is calculated as follows: Let a = diameter of ram in inches b = inside diameter of basket in inches (if round) c =.area of basket in square indies (if square or rect- angular) XXIII. APPARATUS 177 P = gage pressure in pounds per square inch. 240 Ir 306 c Then I = or P = ; a- M ~ < E. g., if a = 4 and b = 10, P = 1500. In obtaining the dimen- sions, measure the rani at the eup leather across the entire effective surface. As the percentage of sugar in the juice obtained from pulp at different pressures does not vary noticeably, a hand operated lard press is satisfactory for this purpose. 15. RADIATOR FOR VOLATILIZING LIQUIDS AND SOLIDS The radiator described by Hillebrand in U. S. Geological Survey Bulletin 700, "The Analysis of Silicate and Carbonate Rocks," page 33, is frequently recommended in this book and will be found greatly superior to the hot plate or sand bath for evapo- rating such liquids as sulphuric acid rapidly without loss by decrepitation. 16. REFRACTOMETERS The refractometer used in sugar work is of the Abbe type and is provided with a dry substance scale based on the Deter- minations of Schonrock. The standard temperature for the use of the instrument is 20. No special directions for the use of the instrument beyond those given in Chap. I, 2 (b) and XXIV, 8, are probably necessary. 17. SPEEDS OF LABORATORY MACHINERY The following resume of the speeds at which +he laboratory machinery should be operated will be found convenient for reference : R, P. M. Beet Rasp (Keil disc) 600-700 Case Crusher 450-500 Cooler, Laboratory Propeller 200 Bolter 40 Conveyor (auger type) 35 *Bureau of Standards Circular 44, "Polarimetry," 2nd ed., p. 134. 178 METHODS OF ANALYSIS R. P. M. Curtis Vacuum Pump and Air Compressor 1 ... 250 (at least) Enterprise Meat Chopper No. 41 300 Hydraulic Press (Hydraulic Press Mfg. Co.), countershaft 80 Her Disc Pulverizer 350-450 McCool Disc Pulverizer 300 Pebble Mill (jar 18y 2 x 18 in.) 40-50 Samson Crusher . 500 18. THERMOMETERS The Centigrade scale alone should be employed. The only exception to this is the use of the Fahrenheit scale in recording boiler house temperatures. Unless otherwise expressly stated, all temperatures in this book are in degrees Centigrade. For deter- mining the temperature correction in the apparent purity deter- mination, a small floating thermometer, with enclosed paper scale, of 30 range, is recommended. Clerget thermometers, for inver- sion readings, must be of special construction and accurate within 0.1 at the 20 point. 19. VOLUMETRIC APPARATUS All flasks, burettes, pipettes, and other volumetric apparatus should be standardized as described in Chap. XXIV, 2. "Sugar" flasks should be made heavier than the ordinary standard to save breakage, but the 100 ml flasks used for inversions should have sufficiently thin walls so that the solutions will reach the neces- sary temperature in the time required. XXIV. STANDARDIZATION AND VERIFICATION OF LABORATORY APPARATUS 1. GENERAL All kinds of laboratory apparatus used for quantitative measurements must be carefully verified before use. Sacchari- meters, refractometers, and weights should be checked at frequent intervals. It should also be remembered that glass apparatus will gradually undergo a slight change in capacity until it has had several years' seasoning. Tolerances: The "specifications for laboratory apparatus" give the limits of error allowable for each class of apparatus. 2. VOLUMETRIC APPARATUS (a) GENERAL Units of Capacity: The liter, defined as the volume occupied by a quantity of pure water at 4 C. having a mass of one kilo- gram, and the one-thousandth part of the liter, called the milli- liter (cubic centimeter), are the units of capacity. Standard Temperature: The standard temperature for the use of glass volumetric apparatus is 20 C. The apparent weight in air of one liter of water at 20 C. (weighed with brass weights in air at 76 cm barometric pressure and 50% relative humidity) is 997.18 grams. At 63 cm barometric pressure (5,000 feet elevation) the apparent weight is 997.36 grams; the difference is so small that it may be disregarded in ordinary work. Tables 35 47 of Bureau of Standards Circular 19, 5th ed., "Standard Density and Volumetric Tables," will be found useful in calibrating volumetric glassware. 180 METHODS OF ANALYSIS Reading: In adjusting the meniscus to the graduation mark, the lowest point of the curve when viewed against a white surface should just touch the level of the mark. (b) FLASKS Clean and dry the flask thoroughly, and standardize by one of the following methods : (1) Weigh the flask first empty and then filled with recently boiled, distilled water. Both the flask and the water should be at room temperature, and the temperature of the water should be accurately determined with a thermometer. Adjust the flask according to the tables in Bureau of Standards Circular 19. For example, a 100 ml flask must be graduated to hold 100 .340 = 99.66 grams of water at 23 C. (See Table 38 of the Circular) (2) Fill the flask from a standardized pipette or burette, using clean water at room temperature. The pipette or burette employed for this purpose should be carefully standardized under definite conditions of manipulation and used under the same con- ditions. If the outflow is sufficiently ^restricted by the size of the orifice in the tip, no period of drainage need be allowed ; other- wise a definite period of drainage, e. g., 15 seconds, should be used. In either case the water remaining in the tip should not be blown out, but the emptying should be completed by t touching the tip to the wet surface of the receiving vessel. (3') Employ a flask standardized by weight as under (1). Fill the clean, dry flask with clean mercury at room temperature, and transfer the latter with the aid of a small funnel to the flasks' of the same capacity to be tested (previously cleaned and dried). Return the mercury occasionally to the standard flask to make sure that there has been no -loss or alteration in volume due to change of temperature in handling. This method ip convenient and safe only for flasks of small capacity. ( c ) PIPETTES Verify pipettes by weighing the water delivered. Use distilled water at room temperature, and obtain the capacity from the tables in Bureau of Standards Circular 19. If the graduation mark is found incorrect, make a new temporary mark and test again, re- *See Bureau of Standards Circular 9, 8th ed., p. 17, "Testing of Glass Volumetric Apparatus." tLoc. cit., p. 26. XXIV. STANDARDIZATION OF APPARATUS 181 peat ing this procedure until the correct point for the graduation is found. Pipettes should be standardized under the conditions under which they are to he used. Pipettes for analytical work of high precision should be standardized as described under "Flasks" (2). Pipettes for routine sugar laboratory work must necessarily have uo<;d sized orifices, but in use the tip is immediately touched to the wet surface of the receiving vessel to complete the emptying, without allowing any period of drainage. (d) BURETTES AND AUTOMATIC PIPETTES Burettes: Calibrate burettes in a similar manner to pipettes by weighing the water discharged. Empty them slowly and check at several different points in the scale, as well as for the largest amount which they will deliver. Burettes may also be verified by connecting them with a ''standardizing pipette" by means of which successive portions of water of 5 ml each can be drawn off and measured. M insuring Pipettes: Check measuring pipettes, so-called Mohr pipettes, in a similar manner to burettes. Automatic Pipettes: The 177 ml automatic pipettes should deliver 177 ml of water within an accuracy of 0.25 ml. Orsat Burettes: Check Orsat burettes at the 100 ml point and at intermediate points up to about the 35 ml graduation mark. If the ratios of the smaller capacities to the total capacity are correct the burette may be used without error, even if the measure- ments do not represent true milliliters. (e) ETCHING GRADUATION MARKS Stopper the flask, or other piece of glassware, and immerse the neck in melted paraffin. After the paraffin has hardened place the flask in a suitable apparatus, by menus of which it can be rotated evenly about its axis and the graduation can be marked by a stylus attached to the apparatus. Then dip the flask in a hydrofluoric acid mixture, such as "Diamond Ink." After a few minutes wash off the acid and remove the paraffin with gasoline or by other suitable means. The graduation mark should be fine, exactly perpendicular to the axis, and should appear as a single ^traijrht line when viewed without parallax. Where it is necessary to regraduate a flask or piece of volu- metric apparatus which already has an incorrectly placed gradua- 182 METHODS OF ANALYSIS tion mark, errors due to confusion of the two marks will be avoided by the use of a *colored mark applied as follows: Mix ceramic green 728 D (Roessler & Hasslacher Chemical Co.) intimately with a vehicle made up of 4 parts of copaiba balsam, 1 part of clove oil, and 1 part of lavender oil, using just enough of the vehicle so that the mixture will run slowly from a pen. After marking, heat with a flame the region where the mark has been made until the color begins to glow, being careful not to heat to the softening point of the glass. Allow to cool a little, then reheat until the markings, not the glass, again begin to glow. 3. HYDROMETERS (a) BRIX HYDROMETERS, GENERAL Standard Temperature: Brix hydrometers indicate, in a solu- tion of pure sugar at 20, the direct percentage of sugar. The limit of error at any point on the scale should not exceed 0.1 Brix. Cleansing: Wash the hydrometers thoroughly with soap and water, rinse, and dry with a clean linen cloth. In order to make the liquid adhere readily, dip the stems in strong alcohol, and wipe immediately with a soft, clean, linen cloth. Points to be Checked: Check at least two points on every hydrometer, one near each end of the scale, and preferably an additional point at the middle. Test Liquid: Use a sulphuric acid solution in every case for the test liquid. (b) PYCNOMETER METHOD A 50 ml pycnometer of the Bureau of Chemistry type (E. & A. Cat. No. 1086) is preferable. First determine the capacity of the pycnometer by weighing it empty, and filled with recently boiled, distilled water at 20. Make at least three or four such determinations, which should agree closely. Then rinse and fill the pycnometer with the test solution, also at exactly 20, and weigh, making at least two such determinations. In obtaining these pycnometer weights, it is unnecessary to weigh to any greater degree of precision than the nearest milligram. *Bock, Jour. Am. Chem. Soc., XLI, 359. XXIV. STANDARDIZATION OF APPARATUS 183 Calculate the density of the test solution as follows: Divide the apparent weight of the test solution by the apparent weight of the water, to obtain the " apparent specific gravity." Convert the latter to "true specific gravity" by the following formula, which gives results correct within four units in the fifth decimal place, equivalent to less than .01 Brix. Let D = true sp. gr. D'= apparent sp. gr. Then D = D' .001 (D' 1) Tlx-n find the equivalent degree Brix from the 20/20 column in Table 1. EXAMPLE Weight of w r ater in pycnometer 50.014 g Weight of test solution in pycnometer 66.043 g J11 = 1.32049 50.014 1.32049 .001 (1.32049 1) -= 1.32049 .00032 = 1.32017 From the table, 1.32017 sp. gr. at 20 720 C. is equivalent to 65.25 Brix. Reading of Hydrometer: Use a cylinder provided with an overflow as shown in fig. 3, p. 12, Bureau of Standards Circular 16. Provide also a stirrer consisting of a glass rod slightly longer than the cylinder and bent into a spiral at the bottom. Fill the cylinder with the test solution at a temperature of 20 C. Immerse the hydrometer carefully slightly beyond (about y 4 inch) the point where it floats naturally, and then allow it to float freely until it has assumed the temperature of the liquid, the hydrometer, stir the liquid, and observe the temperature. If this is not exactly 20, bring it to this temperature, then im- merse the hydrometer as before. If the room temperature varies much from 20, changes in temperature may be avoided by keep- ing the hydrometers immersed in a large jar of water at 20 and transferring them immediately, after wiping, to the cylinder con- taining the test solution. Make all readings at 20, as the tempera- ture corrections prescribed for sugar solutions will not be the same for sulphuric acid solutions. To eliminate the effect on the reading of the formation of surface films of impurities, pour into the funnel sufficient of the 184 METHOI>S OP ANALYSIS test solution (at 20 C.) to cause the liquid to overflow through the spout. Then read the hydrometer. Test the completeness of the surface cleansing by repeating the operation; the readings will approach a constant value as the surface becomes normal. Do not take the reading until the liquid and hydrometer are free from air bubbles and at rest. When the reading is taken, the hydrometer must not be in contact with the bottom or walls of the cylinder. Read the scale by bringing the eye upon a level with the surface of the solution so that the latter appears as a straight line and not an ellipse, and note where the border line forming the bottom of the meniscus intersects the scale. The reading in a sulphuric acid solution also theoretically requires a correction due to the difference in surface tension between sulphuric acid and sugar solutions. This varies with the diameter of the stem of the hydrometer and the density of the solution, but for sugar hydrometers of the customary sizes and ranges the correction is so small that it may be disregarded. (c) COMPARISON METHOD Hydrometers may also be tested by comparison with standard hydrometers certified by the Bureau of Standards. Use a cylinder large enough to hold the standard hydrometer and the hydrometer to be tested at the same time, and employ a sulphuric acid solution at room temperature as the liquid. Overflowing to remove surface contamination is unnecessary, since the effect of the latter on two hydrometers of similar dimen- sions will be the same. Immerse and read the hydrometers otherwise as described before. Until standard hydrometers are several years old, they are liable to change slightly in reading as the result of seasoning. Standard hydrometers should therefore be verified at least once a year by the pycnometer method until they have had several years' seasoning, or in case of doubt should be returned to the Bureau of Standards for re-test. (d) BAUME HYDROMETERS Verify Baume hydrometers, for testing molasses, in a similar manner to Brix hydrometers. Use Table 1 for obtaining the density in degrees Baume from the specific gravity at 20/20 C. of the test solution, after converting the apparent specific gravity XXIV. STANDARDIZATION OP APPARATUS 185 at 20/20 to true specific gravity at 20/20 by the formula previously given. This^ Baume scale is based on a modulus of 145 and specific gravity at 20/20 C. Check the enclosed ther- mometer as well as the areometric scale. 4. THERMOMETERS Verify thermometers by comparison with suitable standards. Use water for temperatures up to its boiling point, and oil for higher ranges. 5. GRADUATION MARKS The following methods may be found useful for making the graduation marks distinct on thermometers and volumetric glass- ware : (a) Dip in a solution of asphaltum, wipe off the excess with a smooth piece of paper, and bake at a temperature sufficiently high to harden the asphaltum. (b) Rub with a soft graphite pencil. (c) Fill with a paste made by mixing lamp black and turpentine. (d) Apply a mixture of oil and white lead, rub softly witli tissue paper, then apply dry, powdered zinc oxide and again rub gently with the tissue paper. 6. WEIGHTS Verify weights by comparison with suitable standards. The present standard saccharimetric normal weight is 26 grams. Check normal weights, including multiples and fractions, and counter- weighted dishes at frequent intervals. 7. POLARISCOPES AND POLARISCOPE TUBES (a) POLARISCOPES Verify polariscopes from time to time with quartz plates which have been standardized by the Bureau of Standards, or have been carefully compared with such standard plates. Polari- scopes which are sent to the Bureau of Standards will be tested by them at several points on the scale and a certificate of correc- tions furnished. 186 METHODS OF ANALYSIS See Chap. XXIII, 13 (b) for the definition of the 100 degree point of the saccharimetric scale. The sugar scale now employed by the Bureau of Standards in standardizing saccharimeters and quartz plates is the Bates-Jackson scale, which differs by about 0.1 at the 100 point from, the Herzfeld-Schonrock scale, the standard formerly in use. Pure sugar which polarizes 100.0 on the former scale will polarize 100.1 on the latter. (b) POLABISCOPE TUBES Verify the length of polariscope tubes by measurement. Test for eccentricity of mounting of the caps by placing the tube, with the caps on, in the trough of a polariscope and, while revolving it, viewing the opening through the tube with reference to the polari- scope field; if the tube has been properly centered and the caps are free from eccentricity, the tube opening will remain in the center of the field and show no movement during rotation. Test for plane parallelism of the ends of the tube and of cover glasses by repeating the experiment with the cover glasses in position and the tube filled with water ; take readings also at different positions during rotation to make sure that any lack of plane parallelism causes no optical activity. Test metal tubes, which may become bent, frequently in this manner. (See Browne's "Handbook of Sugar Analysis," pp. 154-5.) 8. REFRACTOMETERS Test at the zero point with distilled water, and at other points with standard plates or solutions made up by weight from sugar of accurately determined polarization. 9. CALORIMETERS Determine the water equivalent with the standard heat sam- ples of the Bureau of Standards (benzoic acid, naphthalene, and sugar). All thermometers used in calorimetric work should be certified by the Bureau of Standards and the necessary corrections should be employed. 10. BIBLIOGRAPHY Refer to the following publications of the Bureau of Standards : Circular 3 "Design and Test of Standards of Mass." Circular 8 "Testing of Thermometers." XXIV. STANDARDIZATION OF APPARATUS 187 Circular 9 ''Testing of Glass Volumetric Apparatus. " Circular 11 "Standardization of Bomb Calorimeters." Circular 12 "Verification of Polariscopic Apparatus." Circular 16 "Testing of Hydrometers." Circular 19 "Standard Density and Volumetric Tables." Circular 25 "Standard Analyzed Samples." Circular 44 " Polarimetry. " Miscellaneous "Tables of Equivalents of the U. S. Customary and Metric Weights and Measures." XXV. REAGENTS This chapter covers the preparation and standardization of reagents which have a general application. Reagents used for special determinations will be found described in connection with the particular determinations. 1. ACETIC ACID, DILUTE, FOR LIME CAKE ANALYSIS Mix 15 ml of the 99% acetic acid with 1 liter of water. 2. ACETIC ACID, DILUTE, FOR SACCHARATE CAKE ANALYSIS Dilute 1 part of the 99% acetic acid with 4 parts of water. 3. ALPHA-NAPHTHOL Dissolve 5 grams of alpha-naphthol in 100 ml of 95% alcohol. This solution should give the reactions described in Chap. I, 13. If the sensibility of the alpha-naphthol is poor, the strength of the solution may be increased to 10 or 20%, if necessary. As this solution does not keep well, and is liable to become contaminated, it should be made .up in small quantities. 4. ALUMINA CREAM (a) Method I: Add a slight excess of ammonium hydroxide to a cold saturated solution of alum; then bring to a faint acid reaction with a portion of the original alum solution retained for the purpose. (b) Method II: A preparation free from dissolved salts is obtained as follows. Add a slight excess of ammonium hydroxide to a cold saturated solution of alum, allow the precipitate to settle and wash by decantation with water until the wash water gives XXV. REAGENTS 189 only a faint reaction for sulphates with barium chloride solution. Pour off the excess of water until the cream has the proper consistency. 5. AMMONIUM CARBONATE Dissolve 1 part of the crystallized salt in a mixture of 3 parts of water and 1 part of ammonium hydroxide. 6. AMMONIUM OXALATE Dissolve 1 part of the crystallized salt in 24 parts of water. 7. BARIUM CHLORIDE, GENERAL REAGENT Dissolve 1 part of the crystallized salt in 10 parts of water. 8. BARIUM CHLORIDE SOLUTION, FOR STANDARDIZ- ING SOAP SOLUTION Dissolve 4.3574 grams of the C. P. crystallized salt (BaCl 2 .2H 2 O) in water and make up to 1 liter. This solution Ins a value of 1 ml = .001 g *CaO. In case of doubt as to the purity of the barium chloride, the value may be accurately de- termined by precipitating with an excess of dilute sulphuric acid i ud weighing the barium sulphate. Before finishing the ignition add a few drops of sulphuric acid so that any barium present as <; -rinded barium chloride will be converted to sulphate. 9. FEHLING'S SOLUTION Fehling's Solution (Soxhlet's Modification) consists of the following two solutions which are mixed in equal volumes immedi- ately before use. (a) Copper Sulphate Solution: Dissolve 34.639 grams of C. P. crystallized copper sulphate in water, and dilute to a volume of 500 ml. (b) Alkaline Tartrate Solution: Dissolve 173 grams of C. P. vodium potassium tartrate (Rochelle salt) and 50 grams of sodium hydroxide in water, and dilute to a volume of 500 ml. Do not n-e the commercial grade of Rochelle salt. 190 METHODS OP ANALYSIS 10. HYDROCHLORIC ACID FOR INVERSIONS Dilute the ordinary C. P. acid to a density of 24.824.9 Brix at 20. (1.1029 sp. gr. at 20/4 or 1.1049 sp. gr. at 20 720. ) 11. INDICATORS (a) Cochineal: Digest, with frequent agitation, 3 grams of pulverized cochineal in a mixture of 50 ml of strong alcohol and 200 ml of water for 1 or 2 days at ordinary temperature, and then filter. (b) Methyl Orcvnge: Dissolve 1 part of the dye in 1000 parts of water. (c) Methyl Red: Dissolve 1 gram of methyl red (dimethyl- amino-azo-benzene-ortho-carbonic acid) in 100 ml of 95% alcohol. (d) Phenolphthalein : Dissolve 5 grams of the powder in 500600 ml of 95% ethyl alcohol or refined methyl alcohol (Colum- bian Spirit), and dilute tr>yv TVRTX LSlvl-A. 1 2 3 4 5 6 7 8 9 PM 10 jL>xviyv 15.0 .032 .063 .095 .126 .158 .189 .221 .252 .284 315 15.0 .2 .031 .062 .093 .124 .155 .186 .217 .248 .280 .311 .2 .4 .031 .061 .092 .123 .153 .184 .214 .245 .276 .306 .4 .6 .030 .060 .091 .121 .151 .181 .212 .242 .272 .302 .6 .8 .030 .060 .089 .119 .149 .179 .209 .238 .268 .298 .8 16.0 .029 .059 .088 .118 .147 .176 .206 .235 .265 .294 16.0 .2 .029 .058 .087 .116 .145 .174 .203 .232 .261 .290 .2 .4 .029 .057 .086 .115 .143 .172 .201 .229 .258 .286 4 .6 .028 .057 .085 .113 .141 .170 .198 .226 .255 .283 .6 .8 .028 .056 .084 .112 .140 .168 .195 .223 .251 .279 .8 17.0 .028 .055 .083 .110 .138 .165 .193 .221 .248 .276 17.0 .2 .027 .054 .082 .109 .136 .163 .191 .218 .245 .272 .2 .4 .027 .054 .081 .108 .134 .161 .188 .215 .242 .269 .4 .6 .027 .053 .080 .106 .133 .159 .186 .213 .239 .266 .6 .8 .026 .052 .079 .105 .131 .157 .184 .210 .236 .262 .8 18.0 .026 .052 .078 .104 .130 .156 .182 .207 .233 .259 18.0 .2 .026 .051 .077 .103 .128 .154 .179 .205 .231 .256 .2 .4 .025 .051 .076 .101 .127 .152 .177 .203 .228 .253 .4 .6 .025 .050 .075 .100 .125 .150 .175 .200 .225 .250 .6 .8 .025 .049 .074 .099 .124 .148 .173 .198 .223 .247 .8 19.0 .024 .049 .073 .098 .122 .147 .171 .196 .220 .245 19.0 .2 .024 .048 .073 .097 .121 .145 .169 .194 .218 .242 .2 .4 .024 .048 .072 .096 .120 .144 .167 .191 .215 .239 .4 .6 .024 .047 .071 .095 .118 .142 .166 .189 .213 .237 .6 .8 .023 .047 .070 .094 .117 .140 .164 .187 .211 .234 .8 1 2 3 4 5 6 7 8 9 10 . ,, No. of ml of soap soln. Formula: "CaO to 100 Brae" ' 2x . 997 2 x BrixxD' 20 Where D' is the apparent sp. gr. at 3- (ratio of weights in air). 226 METHODS OP ANALYSIS TABLE 15 GaO BY SOAP SOLUTION IN THICK JUICE, MASSECUITE, MOLASSES, ETC. Calculated for the employment of 10 ml of approximately 23 Brix material, and soap solu- tion of the strength, 1 mU.OOl g CaO. An example will make clear the use of the table: 10 ml of diluted molasses of 23.7 Brix required 8.4 ml of soap solution. From the table, on the line opposite 23.7 in the Brix column, .308 + (.154 x.l) =.308 + .015 = .323, which is the "CaO to 100 Brix." NUMBER OF MILLILITERS OF SOAP SOLUTION BRIX BRIX 1 2 3 4 5 6 7 8 9 10 20.0 .046 093 .139 .185 .231 .278 .324 .370 .417 .463 20.0 .1 .046 .092 .138 .184 .230 .276 .322 .368 .414 .461 .1 .2 .046 .092 .137 .183 .229 .275 .321 .366 .412 .458 2 .3 .046 .091 .137 .182 .228 .273 .319 .364 .410 .456 '.3 .4 .045 .091 .136 .181 .227 .272 .317 .363 .408 .453 .4 20.5 .045 .090 .135 .180 .225 .270 .316 .361 .406 .451 20.5 .6 .045 .090 .135 .179 .224 .269 .314 .359 .404 .448 .6 .7 .045 .089 .134 .178 .223 .268 .312 .357 .401 .446 .7 .8 .044 .089 .133 .177 .222 .266 .311 .355 .399 .444 .8 .9 .044 .088 .132 .177 .221 .265 .309 .353 .397 .441 .9 21.0 .044 .088 .132 .176 .220 .263 .307 .351 .395 .439 21.0 .1 .044 .087 .131 .175 .218 .262 .306 .349 .393 .437 .1 .2 .043 .087 .130 .174 .217 .261 .304 .348 .391 .435 .2 .3 .043 .086 .130 .173 .216 .259 .303 .346 .389 .432 .3 .4 .043 .086 .129 .172 .215 .258 .301 .344 .387 .430 .4 21.5 .043 .086 .128 .171 .214 .257 .300 .342 .385 .428 21.5 .6 .043 .085 .128 .170 .213 .256 .298 .341 .383 .426 .6 .7 .042 .085 .127 .169 .212 .254 .297 .339 .381 .424 M . i .8 .042 .084 .126 .169 .211 .253 .295 .337 .379 .422 .8 .9 .042 .084 .126 .168 .210 .252 .294 .336 .378 .420 .9 22.0 .042 .083 .125 .167 .209 .250 .292 .334 .376 .417 22.0 .1 .042 .083 .125 .166 .208 .249 .291 .332 .374 .415 .1 .2 .041 .083 .124 .165 .207 .248 .289 .331 .372 .413 .2 .3 .041 .082 .123 .165 .206 .247 .288 .329 .370 .411 .3 .4 .041 .082 .123 .164 .205 .246 .287 .327 .368 .409 .4 22.5 .041 .081 .122 .163 .204 .244 .285 .326 .367 .407 22.5 .6 .041 .081 .122 .162 .203 .243 .284 .324 .365 .405 .6 .7 .040 .081 .121 .161 .202 .242 .282 .323 .363 .403 .7 .8 .040 .080 .120 .161 .201 .241 .281 .321 .361 .401 .8 .9 .040 .080 .120 .160 .200 .240 .280 .320 .360 .400 .9 23.0 .040 .080 .119 .159 .199 .239 .278 .318 .358 .398 23.0 .1 .040 .079 .119 .158 .198 .237 .277 .317 .356 .396 .1 .2 .039 .079 .118 .158 .197 .236 .276 .315 .355 .394 .2 .3 .039 .078 .118 .157 .196 .235 .274 .314 .353 .392 .3 .4 .039 .078 .117 .156 .195 .234 .273 .312 .351 .390 .4 1 2 3 4 5 6 7 8 9 10 XXVII. TABLES 227 TABLE 15 Continued NUMBER OF MILLILITERS OF SOAP SOLUTION BRIX BRIX 1 2 3 4 5 6 7 8 9 10 23.5 .039 .078 .117 .155 .194 .233 .272 .311 .350 .388 23.5 .6 .039 .077 .116 .155 .193 .232 .271 .309 .348 .387 .6 .7 .038 .077 .115 .154 .192 .231 .269 .308 .346 .385 .7 .8 .038 .077 .115 .153 .192 .230 .268 .306 .345 .383 .8 .9 .038 .076 .114 .152 .191 .229 .267 .305 .343 .381 .9 24.0 .038 .076 .114 .152 .190 .228 .266 .304 .342 .379 24.0 .1 .038 .076 .113 .151 .189 .227 .264 .302 .340 .378 .1 .2 .038 .075 .113 .150 .188 .226 .263 .301 .339 .376 .2 .3 .037 .075 .112 .150 .187 .225 .262 .299 .337 .374 .3 .4 .037 .075 .112 .149 .186 .224 .261 .298 .335 .373 .4 24i5 .037 .074 .111 .148 .185 .223 .260 .297 .334 .371 24.5 .6 .037 .074 .111 .148 .185 .222 .259 .295 .332 .369 .6 .7 .037 .074 .110 .147 .184 .221 .257 .294 .331 .368 .7 .8 .037 .073 .110 .146 .183 .220 .256 .293 .329 .366 .8 .9 .036 .073 .109 .146 .182 .219 .255 .292 .328 .364 .9 25.0 .036 .073 .109 .145 .181 .218 .254 .290 .327 .363 25.0 .1 .036 '.072 .108 .144 .181 .217 .253 .289 .325 .361 .1 .2 .036 .072 .108 .144 .180 .216 .252 .288 .324 .360 .2 .3 .036 .072 .107 .143 .179 .215 .251 .286 .322 .358 .3 .4 .036 .071 .107 .143 .178 .214 .250 .285 .321 .356 .4 25.5 .035 .071 .106 .142 .177 .213 .248 .284 .319 .355 25.5 .6 .035 .071 .106 .141 .177 .212 .247 .283 .318 .353 .6 .7 .035 .070 .106 .141 .176 .211 .246 .282 .317 .352 .7 .8 .035 .070 .105 .140 .175 .210 .245 .280 .315 .350 .8 .9 .035 .070 .105 .140 .174 .209 .244 .279 .314 .349 .9 1 2 3 4 5 6 7 8 9 10 Formula: "CaO to 100 Brix" No. of ml of soap soln. 2x.9972xBnxxD' 20 Where D' is the apparent sp. gr. at ^ (ratio of weights in air). 228 METHODS OF ANALYSIS TABLE 16 TABLE FOR USE IN DRY SUBSTANCE DETERMINATIONS ON PULP SOLD See Chap. VI, 3 (b) for the derivation and use of this table. Acidity of Pulp Grams Lime to be Added Weight to be Subtracted Acidity of Pulp Grams Lime to be Added Weight to be Subtracted .100 .0100 .0068 .600 .0600 .0407 .110 .0110 .0075 .610 .0610 .0414 .120 .0120 .0081 .620 .0620 .0420 .130 .0130 .0088 .630 .0630 .0427 .140 .0140 .0095 .640 .0640 .0434 .150 .0150 .0102 .650 .0650 .0441 .160 .0160 .0109 .660 .0660 .0448 .170 .0170 .0116 .670 .0670 .0454 .180 .0180 .0122 .680 .0680 .0461 .190 .0190 .0129 .690 .0690 .0468 .200 .0200 .0136 .700 .0700 .0475 .210 .0210 .0143 .710 .0710 .0482 .220 .0220 ..0149 .720 .0720 .0488 .230 .0230 .0156 .730 .0730 .0495 .240 .0240 .0162 .740 .0740 .0502 .250 .0250 .0169 .750 .0750 .0509 .260 .0260 .0176 .760 .0760 .0516 .270 .0270 .0183 .770 .0770 .0522 .280 .0280 .0190 .780 .0780 .052.9 .290 .0290 .0196 .790 .0790 .0536 a .300 .0300 .0203 .800 .0800 .0543 .310 .0310 .0210 .810 .0810 .0550 .320 .0320 .0217 .820 .0820 .0557 .330 .0330 .0224 .830 .0830 .0564 .340 .0340 .0230 .840 .0840 .0571 .350 .0350 .0237 .850 .0850 .0578 .360 .0360 .0244 .860 .0860 .0585 .370 .0370 .0251 .870 .0870 .0592 .380 .0380 .0258 .880 .0880 .0598 .390 .0390 .0204 .890 .0890 .0605 .400 .0400 .0271 .900 .0900 .0612 .410 .0410 .0278 .910 .0910 .0619 .420 .0420 .0285 .920 .0920 .0626 .430 .0430 .0291 .930 .0930 .0632 .440 .0440 .0298 .940 .0940 .0639 .450 .0450 .0305 .950 .0950 .0646 .460 .0460 .0312 .960 .0960 .0653 .470 .0470 .0319 .970 .0970 .0660 .480 ."0480 .0325 .980 .0980 .0666 .490 .0490 .0332 .990 .0990 .0673 .500 .0500 .0339 1.000 .1000 .0680 .510 .0510 .0346 1.010 .1010 .0687 .520 .0520 .0353 1.020 .1020 .0694 .530 .05'0 .0359 1.030 .1030 .0700 .540 .0540 .0366 1.040 .1040 .0707 .550 .0550 .0373 1.050 .1050 .0714 .560 .0560 .0380 1.060 .1060 .0721 .570 .0570 .0387 1.070 .1070 .0728 .580 .0580 .0393 1.080 .1080 .0734 .590 .0590 .0400 1.090 .1090 07-41 XXVII. TABLES 229 TABLE 17 B. T. U. LOST IN DRY FLUE GAS PER POUND OF COAL CONTAINING 57% CARBON Based on percentage of CO? in the flue gas, temperature, F., of flue gas (T), and tempera- ture, F., of boiler room (t). %co, T t 250 255 260 265 270 275 280 285 290 295 6.0 1401 1429 1457 1485 1513 1541 1569 1597 1625 1653 6.1 1379 1406 1434 1462 1489 1517 1544 1572 1599 1627 6.2 1357 1384 1411 1438 1466 1493 1520 1547 1574 1601 6.3 1336 1363 1389 1416 1443 1470 1496 1523 1550 1577 6.4 1316 1342 1369 1395 1421 1448 1474 1500 1527 1553 6.5 1296 1322 1348 1374 1400 1426 1452 1478 U03 1529 6.6 1277 1303 1328 1354 1379 1405 1430 1456 1481 1507 6.7 1259 1284 1309 1335 1360 1385 1410 1435 1460 1486 6.8 1241 1266 1291 1315 1340 1365 1390 1415 . 1439 1464 6.9 1223 1247 1272 1296 1321 1345 1370 1394 1419 1443 7.0 1206 1230 1254 1278 1302 1326 1350 1375 1399 1423 7.1 1189 1213 1237 1261 1285 1308 1332 1356 1380 1404 7.2 1173 1197 1220 1244 1267 1291 1314 1338 1362 1386 7.3 1158 1181 1204 1227 1250 1273 1297 1320 1343 1366 7.4 1143 1165 1188 1211 1234 1257 1280 1302 1325 1348 7.5 1128 1150 1173 1195 1218 1241 1263 1286 1308 1331 7.6 1114 1136 1158 1180 1203 1225 1247 1269 1292 1314 7.7 1100 1121 1143 1165 1187 1209 1231 1253 1275 1297 7.8 1086 1108 1129 1151 1173 1194 1216 1238 1260 1281 7.9 1073 1094 1115 1137 1158 1180 1201 1223 1244 1266 .- 8.0 1060 1081 1102 1123 1144 1165 1187 1208 1229 1250 8.1 1047 1068 1089 1110 1131 1152 1172 1193 1214 1235, 8.2 1034 1055 1076 1097 1117 1138 1159 1179 1200 1221 8.3 1022 1043 1063 1084 1104 1125 1145 1166 1186 1206 , 8.4 :. M'- 1011 1031 1051 1071 1092 1112 1132 1152 1172 1193 8.5 1001 1021 1041 1061 1081 1101 1121 1141 1161 1181 8.6 988 1008 1027 1047 1067 1087 1107 1126 1146 1166 8.7 977 997 1016 1036 1055 1075 1094 1114 1133 1153 8.8 966 986 1005 1024 1044 1063 1082 1102 1121 1140 8.9 956 975 994 1013 1032 1051 1070 1090 1109 1128 9.0 946 965 984 1003 1022 1041 1059 1078 1097 1116 9.1 936 955 973 992 1011 1030 1048 1067 1086 1104 9.2 926 945 963 982 1000 1019 1037 1056 1074 1093 93 918 936 955 973 991 1010 1028 1047 1065 1083 9.4 908 926 944 962 981 999 1017 1035 1053 1071 9.5 898 915 933 951 969 987 1005 1023 1041 1059 9.6 889 906 924 942 960 977 995 1013 1031 1048 9.7 880 897 915 932 950 968 985 1003 1020 1038 9.8 S71 889 906 924 941 958 976 993 1011 1028 9.9 863 880 897 915 932 949 966 984 1001 1018 10 854 871 888 905 922 939 956 974 991 1001 10.1 846 863 880 897 914 931 948 965 981 99S 10.2 838 855 872 888 905 922 939 955 972 989 10.3 831 848 864 881 897 914 931 947 964 980 10.4 823 839 856 872 889 905 922 938 955 971 230 METHODS OP ANALYSIS TABLE 17 Continued %C0 2 T t 300 305 310 315 320 325 330 335 340 345 6.0 1681 1709 1737 1765 1793 1821 1849 1877 1905 1933 6.1 1655 1682 1710 1737 1764 1793 1820 1847 1875 1903 6.2 1628 1655 1683 1710 1737 1764 1791 1818 1846 1873 6.3 1603 1630 1657 1683 1710 1737 1764 1790 1817 1844 6.4 1579 1606 1632 1658 1684 1711 1737 1763 1790 1816 6.5 1555 1581 1607 1633 1659 1685 1711 1737 1763 1789 6.6 1532 1558 1583 1609 1635 1660 1686 1711 1737 1762 6.7 1511 1536 1561 1586 1611 1637 1662 1687 1712 1737 6.8 1489 1514 1539 1564 1588 1613 1638 1663 1688 1712 6.9 1468 1492 1517 1541 1565 1590 1614 1639 1663 1688 7.0 1447 1471 1495 1519 1543 1567 1591 1616 1640 1664 7.1 1427 1451 1475 1499 1523 1546 1570 1594 1618 1641 7.2 1409 1432 1455 1478 1502 1525 1549 1572 1596 1619 7.3 1389 1412 1435 1458 1482 1505 1528 1551 1574 1598 7.4 1371 1394 1417 1440 1462 1485 1508 1531 1554 1577 7.5 1353 1376 1398 1421 1444 1466 1489 1511 1534 1556 7.6 1336 1358 1381 1403 1425 1448 1470 1492 1514 1537 7.7 1319 1341 1363 1385 1407 1429 1451 1473 1495 1517 7.8 1303 1325 1347 1368 1390 1412 1433 1455 1477 1499 7.9 1287 1308 1330 1351 1373 1394 1416 1437 1459 1480 8.0 1272 1293 1314 1335 1356 1378 1399 1420 1441 1462 8.1 1256 1277 1298 1319 1340 1361 1382 1403 1424 1445 8.2 1241 1262 1283 1303 1324 1345 1366 1386 1407 1428 8.3 1227 1247 ' 1268 1288 1309 1329 1350 1370 1391 1411 8.4 1213 1233 1253 1273 1294 1314 1334 1354 1374 1395 8.5 1201 1221 1241 1261 1281 1301 1321 1341 1361 1381 8.6 1186 1205 1225 1245 1265 1284 1304 1324 1344 1363 8.7 1172 1192 1211 1231 1251 1270 1290 1309 1329 1348 8.8 1160 1179 1198 1218 1237 1256 1275 1295 1314 1334 8.9 1147 1166 1185 1204 1223 1242 1262 1281 1300 1319 9.0 1135 1154 1173 1192 1211 1230 1249 1267 1286 1305 9.1 1123 1142 1161 1179 1198 1217 1235 1254 1273 1291 9.2 1111 1130 1148 1167 1185 1204 1222 1241 1259 1278 9.3 1102 1120 1138 1157 1175 1194 1212 1230 1249 1267 9.4 1089 1108 1126 1144 1162 1180 1198 1216 1235 1253 9.5 1077 1095 1113 1131 1149 1167 1185 1203 1221 1239 9.6 1066 1083 1102 1120 1137 1155 1173 1191 1208 1226 9.7 1055 1073 1090 1108 1125 1143 1160 1178 1196 1213 9.8 1045 1063 1080 1098 1115 1133 1150 1168 1185 1202 9.9 1035 1053 1070 1087 1104 1122 1139 1156 1173 1191 10.0 1025 1042 1059 1076 1093 1110 1127 1144 1161 1179 10.1 1015 1032 1049 1066 1083 1100 1117 1134 1151 1168 10.2 1006 1022 1039 1056 1073 1089 1106 1123 1140 1156 10.3 997 1014 1030 1047 1064 1080 1097 1113 1130 1147 10.4 988 1004 1021 1037 1053 1070 1086 1103 1119 1136 XXVII. TABLES TABLE 17 Continued 231 %co, T t 350 355 360 365 370 375 380 385 390 395 6.0 1961 1989 2107 2045 2073 2102 2136 2158 2186 2214 6.1 1931 1958 1986 2013 2041 2068 2096 2124 2151 2179 6.2 1900 1927 1954 1981 2008 2036 2063 2089 2117 2144 6.3 1871 1897 1924 1951 1978 2004 2031 2058 2084 2111 6.4 1842 1869 1895 1921 1948 1974 2000 2027 2053 2079 6.5 1815 1841 1866 1892 1918 1944 1970 1996 2022 2048 0.6 1788 1814 1839 1865 1890 1916 1941 1967 1992 2018 6.7 1762 1788 1813 1838 1863 1888 1913 1939 1964 1989 6.8 1737 1762 1787 1812 1836 1861 1886 1911 1936 1960 6.9 1712 1737 1761 1786 1810 1835 1859 1883 1908 1932 7.0 1688 1712 1736 1760 1785 1809 1833 1857 1881 1905 71 1665 1689 1713 1737 1760 1784 1808 1832 1855 :879 7.2 1643 1666 1690 1713 1737 1760 1784 1807 1831 1854 7.3 1621 1644 1667 1690 1713 1737 1760 1783 1806 1829 7.4 1600 1622 1645 1668 1691 1714 1737 1759 1782 1805 7.5 1579 1602 1624 1647 1669 1692 1714 1737 1759 1782 7.6 1559 1581 1603 1626 1648 1670 1692 1715 1737 1759 7.7 1539 1561 1583 1605 1627 1649 1671 1693 1715 1737 7.8 1520 1542 1564 1585 1607 1629 1651 1672 1694 1716 7.9 1502 1523 1544 1566 1587 1609 1630 1652 1673 1695 8.0 1483 1505 1526 1547 1568 1589 1610 1632 1653 1674 81 1466 1487 1507 1528 1549 1570 1591 1612 1633 1654 8.2 1448 1469 1490 1510 1531 1552 1572 1593 1614 1634 8.3 1431 1452 1472 1493 1513 1534 1554 1575 1595 1615 8.4 1415 1435 1455 1476 1496 1516 1536 1556 1577 1597 8.5 1401 1421 1441 1461 1481 1501 1521 1541 1561 1581 8.6 1383 1403 1423 1442 1462 1482 1502 1521 1541 1561 8.7 1368 1387 1407 1426 1446 1466 1485 1505 1524 1544 8.8 1353 1372 1392 1411 1431 1450 1469 1488 1508 1527 8.9 1338 1357 1376 1395 1414 1434 1456 1472 1490 1510 9.0 1324 1343 1362 1381 1400 1419 1438 1457 1475 1494 9.1 1310 1329 1348 1366 1385 1404 1422 1441 1460 1479 9.2 1296 1315 1333 1352 1370 1389 1408 1426 1445 1463 9.3 1285 1304 1322 1341 1359 1377 1396 1414 1432 1451 9.4 1271 1289 1307 1325 1343 1362 1380 1398 1416 1434 9.5 1257 1274 1291 1310 1328 1346 1364 1382 1400 1418 9.6 1 24 J 1262 1279 1297 1315 1333 1351 1368 1386 1404 9.7 1231 1248 1264 1282 1299 1317 1334 1352 1369 1387 9.8 1220 1237 1255 1272 1289 1307 1324 1342 1359 1377 9.9 1208 1225 1242 1260 1277 1294 1311 1329 1346 1363 10.0 1196 1213 1230 1247 1264 1281 1298 1315 1332 1349 10.1 1185 1202 1218 1235 1252 1269 1286 1303 1320 1337 10 2 1173 1190 1207 1223 1240 1257 1274 1291 1307 1324 10 3 1163 1180 1196 1213 1230 1246 1263 1279 1296 1313 10 4 1162 1169 1185 1202 1218 1235 1251 1267 1284 1300 232 METHODS OF ANALYSIS TABLE 17 Continued %CO 2 T t 400 405 410 415 420 425 430 435 440 445 6.0 2242 2270 2298 2326 2354 2382 2410 2438 2466 2494 6.1 2206 2234 2262 2289 2317 2344 2372 2399 2427 2455 6.2 2171 2198 2225 2253 2280 2307 2334 2361 2383 2415 6.3 2138 2165 2191 2218 2245 2272 2298 2325 2352 2378 6.4 2106 2132 2158 2185 2211 2237 2264 2290 2316 2342 6.5 2074 2100 2126 2152 2178 2204 2230 2256 2281 2307 6.6 2043 2069 2094 2120 2146 2171 2197 2222 2248 2273 6.7 2014 2039 2064 2090 2115 2140 2165 2190 2215 2241 6.8 1985 2010 2035 2060 2085 2109 2134 2159 2184 2209 6.9 1957 1981 2005 2030 2055 2079 2104 2128 2152 2177 7.0 1929 1953 1977 2002 2026 2050 2074 2098 2122 2146 7.1 1903 1927 1951 1974 1998 2022 2046 2069 2093 2117 7.2 1877 1901 1924 1948 1971 1995 2018 2042 2065 2089 7.3 1852 1875 1899 1922 1945 1968 1991 2014 2038 2061 7.4 1828 1851 1874 1897 1919 1942 1965 1988 2011 2034 7.5 1805 1827 1850 1872 1895 1917 1940 1962 1985 2068 7.6 1782 1804 1826 1848 1871 1893 1915 1937 1960 1982 7.7 1759 1781 1803 1825 1847 1869 1891 1913 1935 1957 7.8 1737 1759 1781 1803 1824 1846 1868 1890 1911 1933 7.9 1716 1737 1759 1780 1802 1823 1845 1866 1888 1909 8.0 1695 1716 1738 1759 1780 1801 1822 1844 1865 1886 8.1 1675 1696 1717 1738 1759 1780 1801 1821 1842 1863 8.2 1655 1676 1697 1717 1738 1759 1779 1800 1821 1841 8.3 1636 1656 1677 1697 1718 1738 1759 1779 1799 1820 8.4 1617 1637 1657 1678 1698 1718 1738 1758 1779 1799 8.5 1601 1621 1641 1661 1681 1701 1721 1741 1761 1781 8.6 1581 1601 1620 1640 1660 1680 1699 1719 1739 1759 8.7 1563 1583 1602 1622 1641 1661 1680 1700 1720 1739 8.8 1546 1566 1585 1604 1624 1643 1662 1682 1701 1720 8.9 1529 1548 1567 1586 1605 1625 1644 1663 1682 1701 9.0 1513 1532 1551 1570 1589 1608 1627 1646 1665 1683 9.1 1497 1516 1535 1553 1572 1591 1610 1628 1647 1666 9.2 1482 1500 1519 1537 1556 1574 1593 1611 1630 1648 9.3 1469 1487 1506 1524 1543 1561 1579 1598 1616 1634 9.4 1452 1470 1488 1507 1525 1543 1561 1579 1597 1615 9.5 1436 1454 1472 1490 1508 1526 1544 1562 1580 1598 9.6 1422 1439 1457 1475 1493 1510 1528 1546 1564 1582 9.7 1405 1422 1440 1457 1475 1492 1510 1528 1545 1563 9.8 1394 1411 1429 1446 1464 1481 1499 1516 1533 1551 9.9 1380 1398 1415 1432 1449 1467 1484 1501 1518 1536 10.0 1366 1383 1401 1418 1435 1452 1469 1486 1503 1520 10.1 1354 1371 1388 1405 1422 1439 1455 1472 1489 1506 10.2 1341 1358 1374 1391 1408 1425 1441 1458 1475 1492 10.3 1329 1346 1363 1379 1396 1412 1429 1446 1462 1479 10.4 1317 1333 1350 1366 1383 1399 1416 1432 1448 1465 XXVII. TABLES TABLE 17 Continued 233 % co, T t 450 455 460 465 470 475 480 485 490 495 6.0 2522 2550 2578 2606 2634 2662 2690 2718 2746 2774 61 2482 2510 2537 2565 2593 2620 2648 2675 2703 2730 6.2 2443 2470 2497 2524 2551 2578 2605 2633 2660 2687 6.3 2305 2432 2459 2485 2512 2539 2566 2592 2619 2646 6.4 2369 2395 2421 2448 2474 2500 2527 2553 2579 2606 6.5 2333 2357 2385 2411 2437 2463 2489 2515 2541 2567 6.6 2299 2324 2356 2375 2401 2427 2452 2478 2508 2529 6.7 2266 2291 2316 2341 2366 2392 2417 2442 2467 2492 6.8 2233 2258 2283 2308 2333 2357 2382 2407 2432 2457 6.9 2201 2226 2250 2275 2299 2324 2348 2373 2397 2422 7.0 2170 2194 2219 2243 2267 2291 2315 2339 2363 2387 7.1 2141 2165 2188 2212 2236 22CO 2284 2307 2331 2355 7.2 2112 2136 2159 2183 2206 2229 2253 2276 2300 2323 7.3 2084 2107 2130 2153 2176 2200 2223 2246 2269 2292 7.4 2057 2079 2102 2125 2148 2171 2194 2216 2239 2262 7.5 2030 2053 2075 2098 2120 2143 2165 2188 2211 2233 7.6 2004 2027 2049 2071 2093 2116 2138 2160 2182 2205 7.7 1979 2001 2023 2045 2067 2089 2111 2133 2155 2177 7.8 1955 1976 1998 2020 2042 2063 2085 2107 2128 2150 7.9 1931 1952 1973 1995 2016 2038 2059 2081 2102 2124 8.0 1907 1928 1950 1971 1992 2013 2034 2055 2077 2098 8.1 1884 1905 1926 1947 1968 1989 2010 2031 2052 2072 8.2 1862 1883 1903 1924 1945 1966 1986 2007 2028 2048 8.3 1840 1861 1881 1901 1922 1943 1963 1984 2004 2024 8.4 1819 1839 1860 1880 1900 1920 1940 1961 1981 2001 8.5 1801 1821 1841 1861 1881 1901 1921 1941 1961 1981 8.6 1778 1798 1818 1838 1857 1877 1897 1917 1936 1956 8.7 1759 1778 1797 1817 1837 1856 1876 1895 1915 1934 8.8 1740 1759 1778 1798 1817 1836 1856 1875 1894 1914 8.9 1720 1739 1758 1777 1797 1816 1835 1854 1873 1892 9.0 1702 1721 1740 1759 1778 1797 1816 1835 1854 1873 91 1684 1703 1722 1741 1759 1778 1797 1815 1834 1853 9.2 1667 1685 1704 1722 1741 1759 1778 1796 1815 1833 9.3 1653 1671 1690 1708 1726 1745 1763 1781 1800 1818 9.4 1634 1652 1670 1688 1707 1725 1743 1761 1779 1797 9.5 1616 1633 1651 1669 1687 1705 1723 1741 1759 1777 9.6 1599 1617 1635 1653 1670 1688 1706 1724 1741 1759 9.7 1580 1598 1615 1633 1650 1668 1685 1703 1720 1738 9.8 1568 1586 1603 1621 1638 1655 1673 1690 1708 1725 9.9 1553 1570 1587 1605 1622 1639 1657 1674 1691 1708 10.0 1537 1554 1571 1588 1606 1623 1640 1657 1674 1691 10.1 1523 1540 1557 1574 1591 1608 1625 1642 1659 1676 10 2 1508 1525 1542 1559 1575 1592 1609 1626 1642 1659 10 3 1495 1512 1529 1545 1562 1578 1595 1612 1628 1645 10.4 1481 1498 1514 1531 1547 1564 1580 1597 1613 1630 234 METHODS OP ANALYSIS TABLE 17 Continued T t 07 ro. /O ^^2 500 505 510 515 520 525 530 535 540 545 550 6.0 2803 2830 2858 2886 2914 2942 2970 2998 3026 3054 3082 6.1 2758 2786 2813 2841 2868 2896 2923 2651 2979 3006 3034 6.2 2714 2741 2768 2795 2823 2850 2877 2904 2931 2958 2985 6.3 2673 2699 2726 2753 2779 2806 2833 2860 2886 2913 2940 6.4 2632 2658 2685 2711 2737 2764 2790 2816 2843 2869 2891 6.5 2593 2618 2644 2670 2696 2722 2748 2774 2800 2825 2850 6.6 2554 2580 2605 2631 2656 2682 2707 2733 2759 2784 2810 6.7 2517 2543 2568 2593 2618 2643 2669 2694 2719 2744 2769 8.8 2482 2506 2531 2556 2581 2606 2630 2655 2680 2705 2730 6.9 2446 2470 2495 2519 2544 2568 2593 2617 2642 2666 2691 7.0 2412 2436 2460 2484 2508 2532 2556 2580 2604 2629 2653 7.1 2379 2403 2426 2450 2474 2498 2521 2545 2569 2593 2617 7.2 2347 2370 2394 2417 2441 2464 2488 2511 2535 2558 2581 7.3 2315 2339 2362 2385 2408 2431 2454 2477 2501 2524 2547 7.4 2285 2208 2331 2354 2376 2399 2422 2445 2468 2491 2514 7.5 2256 2278 2301 2324 2346 2369 2391 2414 2436 2459 2481 7.6 2227 2249 2271 2294 2316 2338 2361 2383 2405 2427 2450 7.7 2199 2221 2243 2264 2287 2309 2331 2353 2375 2397 2419 7.8 2172 2194 2215 2237 2259 2280 2302 2324 2346 2367 2389 7.9 2145 2166 2188 2209 2231 2252 2274 2295 2317 2338 2360 8.0 2119 2140 2161 2183 2204 2225 2246 2267 2282 2310 2331 8.1 2094 2115 2136 2156 2177 2198 2119 2240 2261 2282 2303 8.2 2069 2089 2110 2131 2152 2172 2193 2114 2234 2255 2276 8.3 2045 2065 2086 2106 2127 2147 2168 2188 2209 2229 2249 8.4 2021 2041 2062 2082 2102 2122 2142 2163 2183 2203 2223 8.5 2001 2021 2041 2061 2081 2101 2121 2141 2161 2181 2201 8.6 1976 1996 2015 2035 2055 2075 2095 2114 2134 2154 2174 8.7 1953 1974 1993 2013 2032 2052 2071 2091 2110 2130 2149 8.8 1933 1952 1972 1991 2010 2030 2049 2068 2088 2107 2126 8.9 1911 1930 1950 1969 1988 2007 2026 2045 2064 2083 2103 9.0 1892 1910 1929 1948 1967 1986 2005 2024 2043 2081 2100 9.1 1872 1890 1909 1928 1946 1965 1984 2002 2021 2040 2059 9.2 1852 1871 1889 1908 1926 1945 1963 1982 2000 2019 2037 9.3 1837 1855 1873 1892 1910 1928 1947 1965 1983 2002 2020 9.4 1816 1834 1852 1870 1888 1906 1924 1942 1961 1979 1997 9.5 1795 1813 1831 1849 1867 1885 1903 1921 1939 1957 1974 9.6 1777 1795 1813 1830 1848 1866 1884 1901 1919 1937 1955 9.7 1756 1773 1791 1808 1826 1843 1861 1878 1896 1913 1931 9.8 1743 1760 1777 1795 1812 1830 1847 1864 1882 1899 1917 9.9 1726 1743 1760 1777 1795 1812 1821 1846 1863 1880 1898 10.0 1708 1725 1742 1759 1776 1793 1810 1828 1845 1862 1879 10.1 1693 1709 1726 1743 1760 1777 1794 1811 1828 1845 1862 10.2 1676 1693 1710 1726 1743 1760 1777 1793 1810 1827 1844 10.3 1662 1678 1695 1711 1728 1745 1761 1778 1795 1811 1828 10.4 1646 1662 1679 1695 1712 1728 1745 1761 1778 1794 1810 XXVII. TABLES 235 TABLE 17 Continued %co, T t 250 255 260 265 270 275 280 285 290 295 10.5 815 832 848 864 881 891 913 930 946 962 10.6 808 824 840 856 873 889 905 921 937 953 10.7 801 817 833 849 865 881 897 913 929 945 10.8 794 810 826 842 857 873 889 905 921 937 10.9 787 803 818 834 850 866 881 897 913 929 11.0 780 796 811 827 842 858 874 889 905 920 11.1 773 788 804 819 835 859 866 881 897 912 11.2 766 782 797 812 828 843 858 874 889 904 11.3 760 775 790 806 821 836 851 866 882 897 11.4 754 709 785 803 815 830 846 861 876 891 11.5 748 763 778 793 808 823 838 853 868 883 11 6 742 757 772 787 801 816 831 846 861 876 11.7 736 751 765 780 795 810 824 839 854 868 11.8 730 745 759 774 788 803 818 832 847 861 11.9 724 738 753 767 782 796 810 825 839 854 12.0 719 733 748 762 776 791 805 820 834 848 12.1 713 727 742 756 770 784 799 813 827 841 12.2 707 721 735 749 764 778 792 806 820 834 12.3 702 716 730 744 758 772 786 800 814 828 12.4 696 710 724 738 757 766 780 794 807 821 12.5 691 705 719 732 746 760 774 788 802 815 12.6 686 700 713 727 741 755 768 782 796 809 12.7 680 694 707 721 734 748 762 775 789 802 12.8 675 689 702 716 729 743 756 770 783 797 12.9 670 683 697 710 724 737 750 764 777 791 13.0 665 678 692 705 718 732 745 758 771 786 13.1 660 673 686 700 713 726 739 752 766 779 13.2 656 669 682 695 708 722 735 748 761 774 13.3 651 664 677 690 703 716 729 742 755 768 13.4 646 659 672 685 698 711 724 737 749 762 13.5 642 655 668 681 693 706 719 732 745 758 13.6 637 650 663 675 688 701 714 726 739 752 13.7 633 646 658 671 684 696 709 722 734 747 13.8 628 641 653 666 678 691 703 716 729 741 13.9 624 636 649 661 674 686 699 711 724 736 14.0 620 632 645 657 670 682 694 707 719 732 14.1 616 628 641 653 665 678 690 702 715 727 14.2 612 624 636 649 661 673 685 698 710 722 14.3 608 620 632 644 657 669 681 693 705 717 14.4 604 616 628 640 652 664 676 689 701 713 14.5 600 612 624 636 648 660 672 684 696 708 14.6 596 608 620 632 644 656 668 679 691 703 14.7 592 604 616 628 639 651 663 675 687 699 14.8 588 600 612 623 635 647 659 670 682 694 14.9 585 597 508 620 632 643 655 667 679 690 1.5.0 581 593 604 616 627 639 651 662 674 686 236 METHODS OF ANALYSIS TABLE 17 Continued %CO 2 T-t 300 305 310 315 320 325 330 335 340 345 10.5 979 995 1011 1027 1044 1060 1076 1092 1109 1125 10.6 970 986 1002 1018 1034 1050 1067 1083 1099 1115 10.7 961 977 993 1009 1025 1041 1057 1073 1089 1105 10.8 953 969 984 1000 1016 1032 1048 1064 1080 1095 10.9 944 960 976 991 1007 1023 1039 1054 1070 1086 11.0 936 952 967 983 998 1014 1030 1045 1061 1076 11.1 928 943 959 974 989 1005 1020 1036 1051 1067 11.2 920 935 950 966 981 996 1012 1027 1042 1058 11.3 912 927 942 958 973 988 1003 1018 1034 1049 11.4 906 921 936 951 966 981 996 1012 1027 1042 11.5 898 913 928 943 958 973 988 1002 1017 1032 11.6 890 905 920 935 950 965 979 994 1009 1024 11.7 883 898 913 927 942 957 972 986 1001 1016 11.8 876 891 905 920 935 949 964 978 993 1008 11.9 868 882 897 911 926 940 954 969 983 998 12.0 863 887 891 906 920 935 949 963 978 992 12.1 856 870 884 898 913 927 941 955 970 984 12.2 849 863 877 891 905 919 933 948 962 976 12.3 842 856 870 884 898 913 927 941 955 969 12.4 835 849 863 877 891 905 919 933 947 961 12.5 829 843 857 871 884 898 912 926 940 954 12.6 823 837 851 864 878 892 906 919 933 947 12.7 816 830 843 857 870 884 898 911 925 938 12.8 810 824 837 851 864 878 891 905 918 932 12.9 804 817 831 844 858 871 884 898 911 925 13.0 798 811 825 838 851 865 878 891 904 918 13.1 792 805 819 832 845 858 871 885 898 911 13.2 787 800 813 826 840 853 866 879 892 905 13.3 781 794 807 820 833 846 859 872 885 898 13.4 775 .788 801 814 827 840 853 866 879 892 13.5 770 783 796 809 822 835 847 860 873 886 13.6 765 777 790 803 816 828 841 854 867 879 13.7 760 772 785 797 810 823 835 848 861 873 13.8 754 766 779 791 804 817 829 842 854 867 13.9 749 761 774 786 799 811 824 836 849 861 14.0 744 756 769 781 794 806 818 831 843 856 14.1 739 752 764 776 788 801 813 825 838 850 14.2 734 747 759 771 783 796 808 820 832 845 14.3 730 742 754 766 778 790 803 815 827 839 14.4 725 737 749 761 773 785 797 . 809 821 834 14.5 720 732 744 756 768 780 792 804 816 828 14.6 715 727 739 751 763 775 787 799 811 822 14.7 711 722 734 746 758 770 782 793 805 817 14.8 706 717 729 741 753 764 776 788 800 811 14.9 702 714 725 737 749 760 772 784 795 807 15.0 697 709 720 732 744 755 767 779 790 802 XXVII. TABLES 237 TABLE 17 Continued %co, T t 350 355 360 365 370 375 380 385 390 395 10.5 1142 1158 1174 1191 1207 1223 1239 1256 1272 1288 10.6 1131 1147 1164 1179 1196 1212 1228 1244 1260 1277 10.7 1121 1137 1153 1169 1185 1202 1217 1234 1249 1266 10.8 1111 1127 1143 1159 1175 1191 1207 1222 1238 1254 10.9 1102 1117 .1133 1149 1165 1180 1196 1212 1226 1243 11.0 1092 1108 1123 1139 1154 1170 1186 1201 1217 1232 11.1 1082 1098 1113 1129 1144 1160 1175 1190 1206 1221 11.2 1073 1088 1104 1119 1134 1150 1165 1180 1196 1211 11.3 1064 1079 1094 1109 1125 1140 1155 1170 1186 1201 11.4 1057 1072 1087 1102 1117 1132 1147 1162 1178 1193 11.5 1047 1062 1077 1092 , 1107 1122 1137 1152 1167 1182 11.6 1039 1054 1068 1083 1098 1113 1128 1143 1158 1172 11.7 1030 1045 1060 1075 1089 1104 1119 1133 1148 1163 11.8 1022 1037 1051 1066 1081 1095 1110 1124 1139 1154 11.9 1012 1026 1041 1055 1070 1084 1099 1113 1127 1142 12.0 1006 1021 1035 1050 1064 1078 1093 1107 1121 1136 12.1 998 1012 1027 1041 1055 1070 1084 1098 1113 1127 12.2 990 1004 1018 1032 1047 1061 1075 1089 1103 1117 12.3 983 997 1011 1025 1039 1053 1067 1081 1095 1109 12.4 975 989 1002 1016 1030 1044 1058 1072 1086 1100 12.5 967 981 995 1009 1023 1037 1050 1064 1078 1092 12.6 960 974 988 1002 1015 1029 1043 1056 1070 1084 12.7 952 966 979 993 1006 1020 1034 1047 1061 1074 12.8 945 959 972 986 999 1013 1026 1046 1053 1067 12.9 938 951 965 978 992 1005 1018 1032 1045 1059 13.0 931 944 958 971 984 998 1011 1024 1037 1051 13.1 924 937 951 964 977 990 1003 1017 1030 1043 13.2 918 931 944 958 971 984 997 1010 1023 1036 13.3 911 924 937 950 963 977 990 1003 1016 1029 13.4 905 918 930 943 956 969 982 995 1008 1021 13.5 899 912 924 937 950 963 976 989 1002 1014 13.6 892 905 918 930 943 956 969 981 994 1007 13.7 886 899 911 924 937 949 962 975 987 1000 13.8 879 x'.rj 905 ' 917 930 942 955 967 980 993 13.9 874 sst) 899 911 924 936 949 961 974 986 14.0 868 880 893 905 918 930 942 955 967 980 14 1 862 875 887 899 912 924 936 949 961 973 14.2 857 869 881 894 906 918 930 942 955 967 14 3 851 863 876 888 900 912 924 936 948 961 14.4 s4C> 858 870 SS'J 894 906 918 930 942 954 14.5 840 852 864 876 sss 900 912 924 936 948 14.6 834 846 s 858 870 SS2 894 906 918 930 942 1 1 7 829 841 853 864 876 888 900 912 924 935 14.8 823 835 847 858 870 882 894 906 917 929 14.9 819 830 842 854 866 877 889 901 912 924 15.0 813 825 837 848 860 872 883 x'..-> 906 918 238 METHODS OF ANALYSIS TABLE 17 Continued %C0 2 T t 400 405 410 415 420 425 430 435 440 445 10.5 1305 1321 1337 1354 1370 1386 1403 1419 1435 1451 10.6 1293 1309 1325 1341 1357 1374 1390 1406 1422 1438 10.7 1282 1298 1314 1330 1346 1362 1378 1394 1410 1426 10.8 1270 1286 1302 1318 1334 1349 1365 1381 1397 1413 10.9 1259 1275 1290 1306 1322 1338 1353 1369 1385 1400 11.0 1248 1264 1279 1295 1310 1326 1342 1357 1373 1385 11.1 1237 1252 1268 1283 1299 1314 1330 1345 1360 1376 11.2 1226 1242 1257 1272 1288 1303 1318 1334 1349 1364 11.3 1216 1231 1246 1262 1277 1292 1307 1322 1338 1353 11.4 1208 1223 1238 1253 1268 1283 1298 1313 1328 1344 11.5 1197 1212 1227 1242 1257 1272 1287 1302 1317 1332 11.6 1187 1202 1217 1232 1247 1261 1276 1291 1306 1321 11.7 1178 1192 1207 1222 1236 1251 1266 1281 1295 1310 11.8 1168 1183 1198 1212 1228 1241 1256 1271 1285 1300 11.9 1156 1171 1185 1199 1214 1228 1243 1257 1271 1286 12.0 1150 1164 1179 1193 1208 1222 1236 1251 1265 1279 12.1 1141 1155 1169 1184 1198 1212 1226 1241 1255 1269 12.2 1132 1146 1160 1174 1188 1202 1216 1231 1245 1259 12.3 1123 1137 1151 1165 1179 1193 1207 1221 1236 1250 12.4 1114 1128 1142 1156 1170 1184 1197 1211 1225 1239 12.5 1108 1119 1133 1147 1161 1175 1189 1202 1216 1230 12.6 1098 1111 1125 1139 1152 1166 1180 1194 1207 1221 12.7 1088 1102 1115 1129 1142 1156 1170 1183 1197 1210 12.8 1080 1094 1107 1121 1134 1148 1161 1175 1183 1202 12.9 1072 1085 1099 1112 1126 1139 1152 1166 1179 1193 13.0 1064 1077 1091 1104 1117 1131 1144 1157 1170 1184 13.1 1056 1070 1083 1096 1109 1122 1136 1149 1162 1175 13.2 1049 1062 1076 1089 1102 1115 1128 1141 1154 1167 13.3 1042 1055 1038 1081 1094 1107 1120 1133 1148 1159 13.4 1034 1047 1060 1073 1086 1099 1111 1124 1137 1150 13.5 1027 1040 1053 1056 1079 1091 1109 1117 1130 1143 13.6 1020 1032 1015 1058 1071 1083 1096 1109 1122 1134 13.7 1013 1025 1038 1050 1063 1076 1088 1101 1114 1126 13.8 1005 1018 1030 1043 1055 1068 1081 1093 1106 1118 13.9 999 1011 1023 1036 1049 1061 1074 1086 1099 1111 14.0 992 1004 1017 1029 1042 1054 1066 1079 1091 1104 14.1 986 998 1010 1023 1035 1047 1060 1072 1084 1096 14.2 979 991 1004 1016 1028 1040 1053 1065 1077 1089 14.3 973 985 997 1001 1029 1074 1046 1058 1070 1082 14.4 966 978 991 1003 1015 1027 1039 1051 1063 1075 14.5 960 972 984 996 1008 1020 1032 1044 1056 1068 14.6 954 966 977 989 1001 1013 1025 1037 1049 1061 14.7 947 959 971 983 995 1007 1018 1030 1042 1054 14.8 941 953 964 976 988 1000 1011 1023 1035 1047 14.9 936 947 959 971 982 994 1006 1018 1029 1041 15.0 930 941 953 964 976 988 999 1011 1023 1034 XXVII. TABLES 239 TABLE 17 Continued %co, T t 450 455 460 465 470 475 480 485 490 495 10.5 1468 1484 1500 1517 1533 1549 1566 1582 1598 1615 10.6 1454 1471 1487 1503 1519 1535 1551 1568 1584 1600 10.7 1442 1458 1474 1490 1506 1522 1538 1554 1570 1586 10.8 1429 L446 1461 1476 1492 1508 1524 1540 1556 1572 10.9 1416 1432 1448 1463 1479 1495 1511 1526 1542 1558 11.0 1404 1420 1435 1451 1466 1482 1498 1513 1529 1544 11.1 1391 1407 1422 1438 1453 1469 1484 1500 1515 1531 11 2 1380 1395 1410 1426 1441 1456 1472 1487 1502 1518 11 3 1369 1383 1398 1414 1429 1444 1459 1474 1490 1505 11.4 1359 1374 1389 1404 1419 1434 1449 1464 1479 1494 11.5 1347 1362 1377 1392 1407 1422 1437 1152 1467 1482 11.6 1336 1350 1365 1380 1395 1410 1425 1439 1454 1469 11.7 1325 1340 1354 1369 1384 1398 1413 1428 1443 1457 11.8 1314 1329 1344 1358 1373 1387 1402 1417 1431 1446 11 9 1300 1315 1329 1343 1358 1372 1387 1401 1416 1430 12.0 1294 1308 1323 1337 1351 1366 1380 1394 1409 1423 12 1 1283 1298 1312 1326 1340 1355 1369 1383 1397 1412 12 2 1273 1287 1301 1315 1330 1344 1358 1372 1386 1400 12.3 1264 1278 1292 1306 1320 1334 1348 1362 1376 1390 12 4 1253 1267 1281 1295 1309 1323 1337 1351 1365 1379 12.5 1244 1258 1271 1285 1299 1313 1327 1341 1354 1368 12.6 1235 1249 1262 1276 1290 1303 1317 1331 1345 1358 12.7 1224 1238 1251 1265 1278 1292 1306 1319 1333 1346 12.8 1215 1229 1242 1256 1269 1283 1296 1310 1323 1337 12.9 1206 1219 1233 1246 1260 1273 1286 1300 1313 1327 13.0 1197 1210 1224 1237 1250 1264 1277 12fiO 1303 1317 1 13.1 1188 1202 1215 1228 1241 1254 1268 1281 1294 1307 13.2 1180 1194 1207 1220 1233 1246 1259 1272 1285 1298 13.3 1172 1185 1198 1211 1224 1237 1250 1263 1276 1289 13.4 1163 1176 1189 1202 1215 1228 1241 1254 1267 1280 13.5 1156 1168 1181 1194 1207 1220 1233 1245 1258 1271 13.6 1147 1160 1173 1185 1198 1211 1224 1236 1249 1262 13 7 1139 1152 1164 1177 1190 1202 1215 1228 1240 1253 13.8 1131 1143 1156 1169 1181 1194 1206 1219 1231 1244 13 9 1124 1136 1149 1161 1174 1186 1199 1211 1224 1236 14.0 1116 1128 1141 1153 1166 1178 1190 1203 1215 1228 14 1 1109 1121 1133 1146 1158 1170 1183 1195 1207 1220 14 2 1102 1114 1126 1138 1151 1163 1175 1187 1200 1212 14.3 1094 1107 1119 1131 1143 1155 1167 1179 1192 1204 14.4 1087 1099 1111 1123 1136 1148 1160 1172 1184 1196 14 5 1080 1092 1104 1116 1128 1140 1152 1164 1176 1188 14 6 1073 1085 1097 1109 1120 1132 1144 1156 1168 1180 14.7 1066 1078 1089 1101 1113 1125 1137 1149 1160 1172 14.8 1058 1070 1082 1094 1105 1117 1129 1141 1152 1164 14.9 1053 1064 1076 1088 1099 1111 1123 1134 1146 1158 15.0 1046 1057 1069 1081 1092 1104 1116 1127 1139 1150 240 METHODS OF ANALYSIS TABLE 17 Continued %C0 2 T t 500 505 510 515 520 525 530 535 540 545 550 10.5 1631 1647 1664 1680 1696 1712 1729 1745 1761 1778 1794 10.6 1616 1632 1648 1664 1681 1697 1713 1729 1745 1761 1778 10.7 1602 1618 1634 1650 1666 1682 1698 1714 1730 1746 1762 10.8 1588 1603 1619 1635 1651 1667 1683 1699 1714 1730 1746 10.9 1574 1589 1605 1621 1636 1652 1668 1684 1699 1715 1731 11.0 1560 1576 1591 1607 1622 1638 1654 1669 1685 1700 1716 11.1 1546 1561 1577 1592 1608 1623 1639 1654 1670 1685 1701 11.2 1533 1548 1564 1579 1594 1610 1625 1640 1656 1671 1686 11.3 1520 1535 1550 1566 1581 1596 1611 1626 1642 1657 1672 11.4 1510 1525 1540 1555 1570 1585 1600 1615 1630 1645 1660 11.5 1497 1511 1526 1541 1556 1571 1586 1601 1616 1631 1646 11.6 1484 1499 1514 1529 1543 1558 1573 1588 1608 1618 1632 11.7 1472 1487 1501 1516 1531 1546 1560 1575 1590 1604 1619 11.8 1461 1475 1490 1504 1519 1534 1548 1563 1577 1592 1607 11.9 1444 1459 1473 1488 1502 1516 1531 1546 1560 1575 1589 12.0 1438 1452 1466 1481 1495 1509 1524 1538 1552 1567 1581 12.1 1426 1440 1455 1469 1483 1497 1512 1526 1540 1554 1569 12.2 1415 1429 1443 1457 1472 1485 1499 1514 1528 1542 1556 12.3 1404 1418 1432 1446 1460 1474 1488 1502 1516 1530 1544 12.4 1393 1406 1420 1434 1440 1462 1476 1490 1504 1518 1532 12.5 1382 1396 1410 1423 1437 1451 1465 1479 1493 1506 1520 12.6 1372 1386 1399 1413 1427 1441 1454 1468 1482 1495 1509 12.7 1360 1374 1387 1401 1414 1428 1442 1455 1469 1482 1496 12.8 1350 1364 1377 1389 1404 1417 1431 1445 1459 1472 1485 12.9 1340 1353 1367 1380 1394 1407 1420 1434 1447 1461 1474 13.0 1330 1343 1357 1370 1383 1397 1410 1423 1436 1450 1463 13.1 1321 1334 1347 1360 1373 1387 1400 1413 1426 1439 1453 13.2 1312 1325 1338 1351 1364 1377 1390 1403 1416 1429 1443 13.3 1302 1315 1328 1341 1354 1367 1380 1393 1406 1419 1432 13.4 1293 1305 1318 1331 1344 1357 1370 1383 1396 1409 1422 13.5 1284 1297 1310 1323 1335 1348 1361 1374 1387 1400 1412 13.6 1275 1287 1300 1313 1326 1338 1351 1364 1377 1389 1402 13.7 1266 1278 1291 1303 1316 1329 1341 1354 1367 1379 1392 13.8 1257 1269 1282 1294 1307 1319 1332 1344 1357 1370 1382 13.9 1249 1261 1273 1286 1298 1311 1323 1336 1348 1361 1373 14.0 1240 1252 1265 1277 1290 1302 1314 1327 1339 1352 1364 14.1 1232 1244 1257 1269 1281 1294 1306 1318 1331 1343 1355 14.2 1224 1236 1248 1261 1273 1285 1297 1310 1322 1334 1346 14.3 1216 1228 1240 1252 1264 1277 1289 1301 1313 1325 1338 14.4 1208 1220 1232 1244 1256 1268 1280 1293 1305 1317 1329 14.5 1200 1211 1223 1285 1247 1259 1271 1283 1295 1307 1319 14.6 1192 1204 1216 1228 1240 1252 1264 1275 1287 1299 1311 14.7 1184 1196 1208 1220 1231 1243 1255 1267 1279 1291 1303 14.8 1176 1188 1200 1211 1223 1235 1247 1258 1270 1282 1294 14.9 1170 1181 1193 1205 1216 1228 1240 1251 1263 1275 1286 15.0 1162 1176 1185 1197 1200 1220 1232 1243 1255 1267 1278 XXVI I. TABI.KS 241 TABLE 17 Continued Derivation The flue gas is assumed to contain 80.5% nitrogen and no carbon monoxide, heat is taken as 0.24. Let a -% CO, in flue gas b = % oxygen in flue gas c =% nitrogen in flue gas (80.5) W =lbs. of dry flue gas per Ib. of carbon burned L =B. T. U. lost in dry flue gas, per Ib. of carbon burned L' =B. T. U. lost in dry flue gas, per Ib. of coal burned The specific Then W lla+8b+7c 3a L =0.24 W (T - t) L'=.57L MOISTURE FACTOR' TABLE 18 FOR COMPUTING LOSS OF HEAT IN FLUE GAS DUE TO MOISTURE Based on Coal Containing 6% Hydrogen If F = moisture factor as found in this table, F' = temperature factor as found in Table 18-A, A = B. T. U. in coal as fired, and Li = total loss of heat due to moisture, FxF / % MOISTURE IN COAL .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 10 64.0 64.1 64.2 64.3 64.4 64.5 64.6 64.7 64.8 64.9 i 11 65.0 65.1 65.2 65.3 65.4 65.5 65.6 65.7 65.8 65.9 12 66.0 66.1 66.2 66.3 66.4 66.5 66.6 66.6 66.8 66.9 13 67.0 67.1 67.2 67.3 67.4 67.5 67.6 67.7 67.8 67.9 14 68.0 68. 68.2 68.2 68.4 68.5 68.6 68.7 68.8 68.9 15 69.0 69. 69.2 69.3 69.4 69.5 69.6 69.7 69.8 69.9 16 70.0 70. 70.2 70.3 70.4 70.5 70.6 70.7 70.8 70.9 17 71.0 71. 71.2 71.3 71.4 71.5 71.6 71.7 71.8 71.9 18 72.0 72. 72.2 72.3 72.4 72.5 72.6 72.7 72.8 72.9 19 73.0 73. 73.2 73.3 73.4 73.5 73.6 73.7 73.8 73.9 20 74.0 74. 74.2 74.3 74.4 74.5 74.6 74.7 74.8 74.9 21 75.0 75.1 75.2 75.3 75.4 75.5 75.6 75.7 75.8 75.9 22 76.0 76.1 76.2 76.3 76.4 76.5 76.6 76.7 76.8 76.9 23 77.0 77.1 77.2 77.3 77.4 77.5 77.6 77.7 77.8 77.9 24 78.0 78.1 78.2 78.3 78.4 78.5 78.6 78.7 78.8 78.9 25 79.0 79.1 79.2 79.3 79.4 79.5 79.6 79.7 79.8 79.9 Derivation Let M -moisture in coal H = hydrogen in coal F = moisture factor ThenF -M+9 H-M+54 242 METHODS OF ANALYSIS TABLE 18-A 'TEMPERATURE FACTOR" FOR COMPUTING LOSS OF HEAT IN FLUE GAS DUE TO MOISTURE, Based on boiling point of water of 202 F. (at 5000 feet elevation) The use of this factor is described in the explanation under Table 18. TEMP. TEMPERATURE (F.) OF BOILER ROOM TEMP. (F.) OF (F.) OF FT TTF OA<3 FT TTF nAQ JL AJ \J J-j \jr/VO 30 40 50 60 70 80 90 100 J~ J-J\J 1-J \_T/\O 330 1209 1199 1189 1179 1169 1159 1149 1139 330 340 1213 1203 1193 1183 1173 1163 1153 1143 340 350 1218 1208 1198 1188 1178 1168 1158 1148 350 360 1223 1213 1203 1193 1183 1173 1163 1153 360 370 1228 1218 1208 1198 1188 1178 1168 1158 370 380 1232 1222 1212 1202 1192 1182 1172 1162 380 390 1237 1227 1217 1207 1197 1187 1177 1167 390 400 1242 1232 1222 1212 1202 1192 1182 1172 400 410 1246 1236 1226 1216 1206 1196 1186 1176 410 420 1251 1241 1231 1221 1211 1201 1191 1181 420 430 1256 1246 1236 1226 1216 1206 1196 1186 430 440 1260 1250 1240 1230 1220 1210 1200 1190 440 450 1265 1255 1245 1235 1225 1215 1205 1195 450 460 1270 1260 1250 1240 1230 1220 1210 1200 460 470 1275 1265 1255 1245 1235 1225 1215 1206 470 480 1279 1269 1259 1249 1239 1229 1219 1209 480 490 1284 1274 1264 1254 1244 1234 1224 1214 490 500 1289 1279 1269 1259 1249 1239 1229 1219 500 510 1293 1283 1273 1263 1253 1243 1233 1223 510 520 1298 1288 1278 1268 1258 1248 1238 1228 520 530 1303 1293 1283 1273 1263 1253 1243 1233 530 540 1307 1297 1287 1277 1267 1257 1247 1237 540 550 1312 1302 1292 1282 1272 1262 1252 1242 550 560 1317 1307 1297 1287 1277 1267 1257 1247 560 570 1322 1312 1302 1292 1282 1272 1262 1252 570 580 1326 1316 1306 1296 1286 1276 1266 1256 580 590 1331 1321 1311 1301 1291 1281 1271 1261 590 600 1336 1326 1316 1306 1296 1286 1276 1266 600 610 1340 1330 1320 1310 1300 1290 1280 1270 610 620 1345 1335 1325 1315 1305 1295 1285 1275 620 630 1350 1340 1330 1320 1310 1300 1290 1280 630 640 1354 1344 1334 1324 1314 1304 1294 1284 640 650 1359 1349 1339 1329 1319 1309 1299 1289 650 30 40 50 60 70 80 90 100 Derivation If T =temp. (F.) of flue gas, t =temp. (F.) of boiler room, w =boiling point of water (202 F at 5000 feet elevation), and F'=factor in table, Then F' = (w-t)+976.6 + .47 (T-w) XXVII. TABLES 243 TABLE 19 CaO IN MILK OF LIME OF VARIOUS DENSITIES (15C.) Blattner's Table Milk of lime made up with sweet water will show only about 85 per cent, of the CaO given by this table. Degrees Brix Specific Gravity Grams CaO per Liter %CaO by Weight Degrees Brix Specific Gravity Grams CaO per Liter %CaO by Weight 25 1.107 135 12.2 36 .160 203 17.5 26 1.111 141 12.6 37 .165 209 17.9 27 1.116 147 13.2 38 .170 215 18.4 28 1.120 153 13.7 39 .175 221 18.8 29 1 125 159 14.1 40 .180 228 19.3 30 1.130 165 14.6 41 .185 235 19.8 31 1.135 171 15.1 42 .190 242 20.3 32 1.140 177 15.5 43 .195 248 20.8 33 1.145 183 16.0 44 .200 255 21.3 34 1.150 189 16.4 45 .205 262 21.7 35 1.155 195 16.9 46 .210 269 22.2 244 METHODS OF ANALYSIS TABLE 20 EQUIVALENTS OF NORMAL SOLUTIONS SUBSTANCE FORMULA MOLECULAR OR ATOMIC WEIGHT NORMAL COEFFICIENTS g per Liter 1 ml=g Ammonia NHa 17.032 17.032 .01703 Ammonium sulphocyanate NHO 248.20 *248.20 *. 24820 Sulphuric acid H..SO 4 98.076 49.038 .04904 *As oxidizing or reducing agent. XXVII. TABLES 245 TABLE 21 PERCENTAGE OF AVAILABLE GRANULATED ON DRY SUBSTANCE OF SUGAR SOLUTIONS (MOLASSES PURITY OF 60) Pur- .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 Pur- ity ity 60 0.0 .25 '.5 .75 1.0 1 25 1.5 1.75 2.0 2.25 60 61 2.5 2.75 3.0 3.25 3.5 3.75 4.0 4.25 4.5 4.75 61 62 5.0 5.25 5.5 o . 75 6.0 6.25 6.5 6.75 7.0 7.25 62 63 7.5 7.75 8.0 8.25 8.5 8.75 9.0 9.25 9.5 9.75 63 64 10.0 10.25 10.5 10.75 11.0 11.25 11.5 11.75 12.0 12.25 64 65 12.5 12.75 13.0 13.25 13.5 13.75 14.0 14.25 14.5 14.75 65 66 15.0 15.25 15.5 15.75 16.0 16.25 16.5 16.75 17.0 17.25 66 67 17.5 17.75 18.0 18.25 18.5 18.75 19.0 19.25 19.5 19.75 67 68 20.0 20.25 20.5 20.75 21.0 21.25 21.5 21.75 22.0 22.25 68 69 22.5 22.75 23.0 23.25 23.5 23.75 24.0 24.25 24.5 24.75 69 70 25.0 25.25 25.5 25.75 26.0 26.25 26.5 26.75 27.0 27.25 70 71 27.5 27.75 28.0 28.25 28.5 28.75 29.0 29.25 29.5 29.75 71 72 30.0 30.25 30.5 30.75 31.0 31.25 31.5 31.75 32.0 32.25 72 73 32.5 32.75 33.0 33.25 33.5 33.75 34.0 34.25 34.5 34.75 73 74 35.0 35.25 35.5 35.75 36.0 36.25 36.5 36.75 37.0 37.25 74 75 37.5 37.75 38.0 38.25 38.5 38.75 39.0 39.25 39.5 39.75 75 76 40.0 40.25 40.5 40.75 41.0 41.25 41.5 41.75 42.0 42.25 76 77 42.5 42.75 43.0 43.25 43.5 43.75 44.0 44.25 44.5 44.75 77 78 45.0 45.25 45.5 45.75 46.0 46.25 46.5 46.75 47.0 47.25 78 79 47.5 47.75 48.0 48.25 48.5 48.75 49.0 49.25 49.5 49.75 79 80 50.0 50.25 50.5 50 75 51.0 51.25 51.5 51.75 52.0 52.25 80 81 52.5 52.75 53.0 53.25 53 5 53.75 54.0 54.25 54.5 54.75 81 82 55.0 55.25 55.5 55.75 56.0 56.25 56.5 56 75 57.0 57.25 82 83 57.5 57.75 58.0 58.25 58.5 58.75 59.0 59.25 59.5 59.75 83 84 60.0 60.25 60.5 60.75 61.0 61.25 61.5 61.75 62.0 62.25 84 85 62.5 62.75 63.0 63.25 63.5 63.75 64.0 64.25 64.5 64.75 85 86 65.0 65.25 65.5 65.75 66.0 66.25 66.5 66.75 67.0 67.25 86 87 67.5 67.75 68.0 68.25 68.5 68.75 69.0 69.25 69.5 69.75 87 88 70.0 70.25 70.5 70.75 71.0 71.25 71.5 71.75 72.0 72.25 88 89 72.5 72.75 73.0 73.25 73.5 73.75 74.0 74.25 74.5 74.75 89 90 75.0 75.25 75.5 75.75 76.0 76.25 76.5 76.75 77.0 77.25 90 91 77.5 77.75 78.0 78.25 78.5 78 75 79.0 79.25 79.5 79.75 91 92 SO.O 80.25 80.5 80.75 81.0 81.25 81.5 81.75 82.0 82.25 92 93 82.5 82.75 83.0 83.25 83.5 83.75 84.0 84.25 84.5 84.75 93 94 85.0 85.25 85.5 85.75 86.0 86.25 86.5 86.75 87 87.25 94 95 87.5 87.75 88.0 88.25 88.5 88.75 89.0 89.25 89.5 89:75 95 96 90.0 90.25 90.5 90.75 91.0 91.25 91.5 91.75 92.0 92.25 96 97 92.5 92.75 93.0 93.25 93.5 93.75 94.0 94.25 94.5 94.75 97 98 95.0 95.25 95.5 95.75 96.0 96.25 96.5 96.75 97.0 97.25 98 99 97.5 97.75 98.0 98.25 98.5 98.75 99.0 99.25 99.5 99.75 99 .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 DERIVATION: If P -purity and F -granulated factor, F-2.5 (P-60). 246 METHODS OF ANALYSIS TABLE 22 PERCENTAGE OF AVAILABLE GRANULATED ON TOTAL SUGAR OF SUGAR SO- LUTIONS (MOLASSES PURITY OF 60) This table should not be confused with Table 21, which is the one mostly employed in taking stock. Table 22 is intended for use where the polarization and purity of a product are known. E. g., if a lot of 10,000 Ibs. of raw sugar has a polarization of 96 . 7 and a purity of 97 . 1, the amount of sugar in the raw sugar is 10,000x96.7-^-100=9670 Ibs. The factor corresponding to 97.1 in Table 22 is 95 . 52. The "available granulated" is then, 9670 x95 . 52 -100 =9237 Ibs. Pur- .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 Pur- ity ity 60 0.00 0.42 0.83 1.25 1.66 2.07 2.48 2.88 3.29 3.69 60 61 4.10 4.50 4.90 5.30 5.70 6.10 6.49 6.89 7.28 7.67 61 62 8.06 8.45 8.84 9.23 9.62 10.00 10.38 10.77 11.15 11.53 62 63 11.90 12.28 12.66 13.03 13.41 13.78 14.15 14.52 14.89 15.26 63 64 15.62 15.99 16.36 16.72 17.08 17.44 17.80 18.16 18.52 18.88 64 65 19.23 19.59 19.94 20.29 20.64 20.99 21.34 21.69 22.04 22.38 65 66 22.73 23.07 23.41 23.76 24.10 24.44 24.77 25.11 25.45 25.79 66 67 26.12 26.45 26.79 27.12 27.45 27.78 28.11 28.43 28.76 29.09 67 68 29.41 29.74 30.06 30.38 30.70 31.02 31.34 31.66 31.98 32.29 68 69 32.61 32.92 33.24 33.55 33.86 34.17 34.48 34.79 35.10 35.41 69 70 35.71 36.02 36.32 36.63 36.93 37.23 37.54 37.84 38.14 38.43 70 71 38.73 39.03 39.33 39.62 39.92 40.21 40.50 40.79 41.09 41.38 71 72 41.67 41.96 42.24 42.53 42.82 43.10 43.39 33.67 43.96 44.24 72 73 44.52 44.80 45.08 45.36 45.64 45.92 46.20 46.47 46.75 47.02 73 74 47.30 47.57 47.84 48.12 48.39 48.66 48.93 49.20 49.47 49.73 74 ',5 50.00 50.27 50.53 50.80 51.06 51.32 51.59 51.85 52.11 52.37 75 76 52.63 52.89 53.15 53.41 53.66 53.92 54.18 54.43 54.69 54.94 76 77 55.19 55.45 55.70 55.95 56.20 56.45 56.70 56.95 57.20 57.45 77 78 57.69 57.94 58.18 58.43 58.67 58.92 59.16 59.40 59.64 59.89 78 79 60.13 60.37 60.61 60.85 61.08 61.32 61.56 61.79 62.03 62.27 79 80 62.50 62.73 62.97 63.20 63.43 63.66 63.90 64.13 64.36 64.59 80 81 64.81 65.04 65.27 65.50 65.72 65.95 66.18 66.40 66.63 66.85 81 82 67.07 67.30 67.52 67.74 67.96 68.18 68.40 68.62 68.84 69.06 82 83 69.28 69.49 69.71 69.93 70.14 70.36 70.57 70.79 71.00 71.22 83 84 71.43 71.64 71.85 72.06 72.27 72.49 72.70 72.90 73.11 73.32 84 85 73.53 73.74 73.94 74.15 74.36 74.56 74.77 74.97 75.17 75.38 85 86 75.58 75.78 75.99 76.19 76.39 76.59 76.79 76.99 77.19 77.39 86 87 77.59 77.78 77.98 78.18 78.38 78.57 78.77 78.96 79.16 79.35 87 88 79.55 79.74 79.93 80.12 80.32 80.51 80.70 80.89 81.08 81.27 88 89 81.46 81.65 81.84 82.03 82.21 82.40 82.59 82.78 82.96 83.15 89 90 83.33 83.52 83.70 83.89 84.07 84.25 84.44 84.62 84.80 84.98 90 91 85.16 85.35 85.53 85.71 85.89 86.07 86.24 86.42 86.60 86.78 91 92 86.96 87.13 87.31 87.49 87.66 87.84 88.01 88.19 88.36 88.54 92 93 88.71 88.88 89.06 89.23 89.40 89.57 89.74 89.91 90.09 90.26 93 94 90.43 90.60 90.76 90.93 91.10 91.27 91.44 91.61 91.77 91.94 94 95 92.11 92.27 92.44 92.60 92.77 92.93 93.10 93.26 93.42 93.59 95 96 93.75 93.91 94.07 94.24 94.40 94.56 94.72 94.88 95.04 95.20 96 97 95.36 95.52 95.68 95.84 96.00 96.15 96.31 96.47 96.63 96.78 97 98 96.94 97.09 97.25 97.41 97.56 97.72 97.87 98.02 98.18 98.33 98 99 98.48 98.64 98.79 98.94 99.09 99.25 99.40 99.55 99.70 99.85 99 .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 DERIVATION: If P= purity and F' = granulated factor, F , 250 (P-60) XXVn. TABLES 247 TABLE 23 STANDARD BEET EXTRACTION Based on 0.60% total losses on beets, 40% elimination, and 57 apparent purity of molasses. % SUGAR IN COSSETTES Cos- . Cos- sette sette Pur. Pur. 13.0 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 79.0 ::> -2-2 75 27 75.32 75.38 75.42 75.48 75.52 75.57 75.62 75.67 79.0 79.1 75.35 75.41 75.45 75.52 75.56 75.61 75.66 75.71 75.76 75.80 79.1 79.2 75.47 75.52 75.57 75.63 75.68 75.73 75.77 75.82 75.88 75.92 79.2 79.3 75.59 75.64 75.69 75.76 75.80 75.85 75.91 75.95 76.00 76.04 79.3 79.4 75.71 75.76 75.80 75.87 75.92 75.97 76.02 76.06 76.12 76.16 79.4 79.5 75.84 75.89 75.94 76.00 76.05 76.10 76.16 76.19 76.25 76.29 79.5 79.6 75.95 76.00 76.04 76.11 76.16 76.21 76.26 76.30 76.35 76.40 79.6 79.7 76.06 76.11 76.16 76.22 76.27 76.32 76.37 76.41 76.47 76.51 79.7 79.8 7.'. Is 76.24 76.28 7f, :;o 76.40 76.45 76.50 76.54 76.60 76.64 79.8 7'.' '.' 76.32 76.37 76.42 76.48 76.53 76.58 76.64 76.67 76.73 76.77 79.9 Sll I) 76.43 76.48 76.53 76.60 76.64 76.70 76.75 76.79 76.85 76.88 80.0 80.1 76.55 76.60 76.64 76.71 76.76 76.81 76.87 76.90 76.96 77.00 80.1 80.2 76.66 76.71 76.76 76.83 76.88 76.93 76.98 77.02 77.08 77.12 80.2 80.3 :-, 7s 76.84 76.88 76.95 77.00 77.05 77.09 77 13 77.20 77.24 80.3 80.4 76.90 76.95 77.01 77.07 77.12 77.17 77.22 77.25 77.32 77.36 80.4 80.5 77.01 77.07 77.12 77.18 77.24 77.28 77.33 77.38 77.43 77.48 80.5 80.6 77.13 77.18 77.25 77.29 77.35 77.39 77.45 77.50 77.54 77.59 80.6 80.7 77.24 77.30 77.36 77.41 77.46 77.51 77.56 77.61 77.66 77.71 80.7 80.8 77.37 77.42 77.47 77.52 77.58 77.63 77.68. 77.72 77.77 77.82 80.8 80.9 77.48 77.53 77.59 77.64 77.69 77.74 77.79 77.84 77.89 77.94 80.9 81.0 77.60 77.65 77.70 77.75 77.81 77.86 77.91 77.96 78.t)0 78.05 81.0 81.1 77.71 77.76 77.82 77.87 77.92 77.97 78.02 78.07 78.12 78.17 81.1 81.2 77.82 77.88 77.93 77.98 78.04 78.09 78.14 78.19 78.23 78.28 81.2 81.3 77.95 78.00 78.06 78.11 78.16 78.21 78.26 78.31 78.36 78.41 81.3 81.4 78.05 78.11 78.16 78.21 78.27 78.32 78.37 78.42 78.46 78.51 81.4 81.5 78.17 78.22 78.28 78.33 78.38 78.43 78.48 78.53 78.58 78.63 81.5 81.6 78.28 78.34 78.39 78.44 78.50 78.55 78.60 78.65 78.69 78.75 81.6 81.7 78.40 78.45 78.51 78.55 78.61 78.66 78.71 78.76 78.81 78.86 81.7 81.8 78.51 78.56 78.62 78.67 78.73 78.78 78.83 78.88 78.93 78.98 81.8 81 9 78.63 78.68 78.74 78.78 78.84 78.89 78.94 78.99 79.04 79.09 81.9 82.0 78.74 78.79 78.85 78.90 78.96 79.01 79.06 79.01 79.16 79.20 82.0 82 1 78.85 78.91 78.96 79.01 79.07 79.12 79.17 79.22 79.27 79.32 82.1 VJ _' 78.97 79.02 79.08 79.13 79.19 79.24 79.28 79.34 79.39 79.44 82.2 82.3 79.08 79.14 79.19 79.24 79.30 79.35 79.40 79.45 79.50 79.55 82.3 82.4 79.20 79.25 79.31 79.36 79.42 79.47 79.52 79.57 79.62 79.67 82.4 82.5 79.30 79.36 79.41 79.46 79.52 79.57 79.62 79.67 79.72 79.77 82.5 82.6 79.42 79.47 79.53 79.59 79.64 79.69 79.74 79.79 79.84 79.89 82.6 82.7 79.52 79.58 79.64 79.68 79.77 79.82 79.87 79.92 79.97 80.02 82.7 82.8 79.65 79.70 79.76 79.81 79.87 79.92 79.97 80.02 80.07 80.12 82.8 82.9 79.75 79.81 79.86 79.91 79.97 80.02 80.07 80.12 80.17 80.22 82.9 13.0 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 248 METHODS OF ANALYSIS TABLE 23 Continued STANDARD BEET EXTRACTION % SUGAR IN COSSETTES Cos- Cos- setfe sette Pur Pur. 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 16.8 79.0 75.71 75.75 75.78 75.82 75.86 75.90 75.93 75.97 76.01 76.04 79.0 79.1 75.84 75.88 75.92 75.96 76.00 76.04 76.07 76.11 76.15 76.18 79.1 79.2 75.96 75.99 76.02 76.07 76.11 76.15 76.18 76.22 76.26 76.30 ,79.2 79.3 76.08 76.12 76.16 76.20 76.24 76.28 76.31 76.35 76.39 76.42 79.3 79.4 76.20 76.23 76.27 76.31 76.35 76.39 76.43 76.47 76.50 76.54 79.4 79.5 76.33 76.37 76.41 76.45 76.49 76.53 76.56 76.60 76.63 76.67 79.5 79.6 76.44 76.48 76.51 76.55 76.59 76.63 76.67 76.71 76.74 76.78 79.6 79.7 76.55 76.59 76.63 76.67 76.70 76.75 76.78 76.82 76.86 76.89 79.7 79.8 76.68 76.72 76.76 76.80 76.83 76.88 76.91 76.95 76.98 77.02 79.8 79.9 76.81 76.85 76.88 76.93 76.97 77.01 77.04 77.08 77.12 77.15 79.9 80.0 76.92 76.96 77.00 77.04 77.09 77.13 77.16 77.20 77.24 77.27 80.0 80.1 77.04 77.08 77 . 12 77.16 77.20 77.24 77.27 77.31 77.35 77.38 80.1 80.2 77.16 77.20 77.24 77.28 77.32 77.36 77.40 77.43 77.47 77.51 80.2 80.3 77.28 77.32 77.36 77.40 77.44 77.48 77.51 77.55 77.58 77.62 80.3 80.4 77.40 77.44 77.48 77.52 77.57 77.61 77.64 77.67 77.71 77.75 80.4 80.5 77.52 77.56 77.60 77.64 77.68 77.72 77.75 77.78 77.82 77.87 80.5 80.6 77.63 77.67 77.71 77.75 77.79 77.84 77.87 77.90 77.95 77.98 80.6 80.7 77 . 75 77.79 77.83 77.87 77.91 77.95 77.98 78.02 78.07 78.10 80.7 80.8 77.85 77.90 77.94 77.99 78.03 78.07 78.11 78.14 78.18 78.21 80.8 80.9 77.98 78.02 78.06 78.10 78.14 78.19 78.23 78.26 78.30 78.33 80.9 81.0 78.09 78.13 78.18 78.22 78.26 78.30 78.34 78.37 78.41 78.44 81.0 81.1 78.21 78.25 78.29 78.33 78.37 78.41 78.46 78.49 78.53 78.56 81.1 81.2 78.32 78.37 78.41 78.45 78.49 78.53 78.57 78.60 78.64 78.68 81.2 81.3 78.45 78.49 78.53 78.57 78.61 78.65 78.69 78.73 78.76 78.80 81.3 81.4 78.55 78.60 78.64 78.68 78.72 78.76 78.80 78.84 78.87 78.91 81.4 81.5 78.64 78.69 78.73 78.77 78.81 78.85 78.89 78.92 78.97 79.02 81.5 81.6 78.79 78.83 78.87 78.91 78.95 78.99 79.03 79.06 79.10 79.14 81.6 81.7 78.90 78.94 78.98 79.02 79.06 79.11 79.15 79.18 79.22 79.25 81.7 81.8 79.02 79.06 79.10 79.14 79.18 79.22 79.27 79.30 79.34 79.37 81.8 81.9 79.13 79.17 79.21 79.25 79.29 79.34 79.38 79.41 79.44 79.49 81.9 82.0 79.25 79.29 79.33 79.37 79.41 79.46 79.49 79.53 79.56 79.60 82.0 82.1 79.36 79.40 79.44 79.49 79.54 79.59 79.63 79.64 79.69 79.72 82.1 82.2 79.48 79.52 79.56 79.60 79.64 79.69 79.73 79.76 79.79 79.83 82.2 82.3 79.59 79.63 79.67 79.72 79.77 79.81 79.85 79.88 79.91 79 . 95 82.3 82.4 79.71 79.75 79.79 79.83 79.87 79.91 79.95 79.99 80.02 80.06 82.4 82.5 79.81 79.85 79.89 79.94 79.99 80.03 80.07 80.10 80.14 80.17 82.5 82.6 79.93 79.97 80.01 80.05 80.10 80.14 80.18 80.21 80.25* 80.29 82.6 82.7 80.03 80.07 80.12 80.16 80.20 80.24 80.29 80.32 80.36 80.39 82.7 82.8 80.16 80.20 80.24 80.28 80.32 80.37 80.41 80.44 80.48 80.52 82.8 82.9 80.26 80.31 80.35 80.39 80.43 80.47 80.52 80.55 80.59 80.62 82.9 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 16.8 XXVII. TABLES 249 TABLE 23 Continued STANDARD BEET EXTRACTION % SUGAR IN COSSETTES Cos- Cos- sett e sette Pur. Pur. 13.0 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 83.0 79.85 79.90 79.96 80.01 80.06 80.12 80.17 80.22 80.27 80.32 83.0 83.1 79.94 79.99 80.06 80.10 80.15 80.20 80.26 80.31 80.36 80.41 83.1 83 . 2 80.08 80.13 80.19 80.24 80.29 80.35 80.40 80.45 80.50 80.55 83.2 83.3 80.18 80.23 80.29 80.34 80.39 80.45 80.50 80.55 80.60 80 65 83.3 83 4 80.30 80.35 80.41 80.45 80.49 80.57 80.62 80.67 80.72 80.77 83.4 83.5 80.41 80.46 80.52 80.57 80.62 80.68 80.73 80.78 80.83 80.88 83.5 83.6 80.51 80.57 80.63 80.68 80.73 80.79 80.84 80.89 80.91 80.99 83.6 83.7 80.63 80.68 80.74 80.79 80.84 80.90 80.95 81.00 81.05 81.10 83.7 83.8 80.74 80.80 80.86 80.91 80.95 81.02 81.07 81.12 81.17 81.22 83.8 83.9 80.84 80.88 80.95 80.99 81.04 81.10 81.15 81.20 81.26 81.31 83.9 84.0 80.93 80.99 81.05 81.10 81.15 81.21 81.26 81.31 81.36 81.41 84.0 84.1 81.05 81.10 81.16 81.21 81.26 81.32 81.37 81.42 81.47 81.53 84.1 84.2 81.16 81.22 81.28 81.33 81.38 81.42 81.49 81.54 81.59 81.64 84.2 84.3 81.27 81.32 81.35 81.43 81.47 81.52 81.57 81.65 81.70 81.75 84.3 M 1 81.36. 81.42 81.48 81.53 81.59 81.64 81.69 81.74 81.79 81.85 84.4 84.5 81.48 81.53 81.59 81.64 81.70 81.75 81.80 81.85 81.90 81.95 84.5 M r, 81.58 81.64 81.70 81.75 81.81 81.86 81.91 81.96 82.01 82.06 84.6 84.7 81.70 81.75 81.81 81.86 81.92 81.97 82.03 82.08 82.13 82.18 84.7 M v 81.80 81.85 81.92 81.97 82.03 82.08 82.13 "82.18 82.23 82.28 84.8 84.9 81.91 81.96 82.02 82.07 82.13 82.18 82.24 82.29 82.34 82:39 84.9 85.0 82.00 82.06 82.12 82.17 82.23 82.28 82.33 82.38 82.43 82.48 85.0 85.1 82.11 82.16 82.22 82.27 82.33 82.39 82.44 82.49 82.54 82.59 85.1 85.2 82.22 82.28 82.34 82.39 82.45 82.50 82.55 82.60 82.66 82.71 85.2 85.3 82.33 82.38 82.44 82.49 82.55 82.60 82.65 82.70 82.75 82.80 85.3 85.4 82.43 82.49 82.55 82.60 82.65 82.71 82.76 82.81 82.86 82.91 85.4 v, :, 82.53 82.58 82.64 82.69 82.75 82.80 82.85 82.91 82.96 83.01 85.5 85.6 82.63 82.69 82.75 82.80 82.86 82.91 82.96 83.02 83.07 83.12 85.6 85.7 82.74 82.79 82.88 82.90 82.96 83.02 83.07 83.12 83.17 82.23 35.7 85.8 82.84 82.89 82.96 83.01 83.07 83.12 83.17 83.23 83.28 83.33 85.8 85.9 82.94 82.99 83.05 83.10 83.17 83.20 83.27 83.32 83.37 83.43 85.9 86.0 83 03 83 09 83.15 83.20 83.21 83.32 83.37 83.42 83.47 83.52 86.0 86.1 83.16 83.21 83.27 83.32 83.39 83.44 83.49 83.54 83.59 83.65 86.1 86.2 83.26 83.32 83.38 83.43 83.49 83.54 83.59 83.65 83.70 83.75 86.2 86.3 83.35 83.40 83.46 83.52 83.58 83.63 83.68 83.73 83.78 83.84 86.3 86.4 83.45 83.51 83.57 83.62 83.68 83 . 73 83.78 83.83 83.89 83.95 86.4 86.5 83.57 83.62 83.68 83.74 83.80 83.85 83.90 83.95 84.01 84.06 86.5 86.6 83.65 83.71 83.77 83.82 83.88 83.94 83.99 84.04 84.09 84.15 86.6 86.7 83.76 83.81 83.87 83.93 83.99 84.04 84.09 84.15 84.20 84.25 86.7 86.8 83.86 83.92 83.98 84.03 84.09 84.15 84.19 84.25 84.30 84.35 86.8 86.9 83.96 84.01 84.07 84.13 84.19 84.24 84.29 84.35 84.40 84.45 86.9 13.0 13.2 13.4 13.6 13.8 14.0 14.2 14.4 14.6 14.8 250 METHODS OF ANALYSIS TABLE 23 Continued STANDARD BEET EXTRACTION % SUGAR IN COSSETTES Cos- Cos- sette sette Pur. Pur. 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 16.8 83.0 80.36 80.40 80.44 80.49 80.54 80.58 80.63 80.67 80.69 80.72 83.0 83.1 80.46 80.50 80 . 54 80.58 80.63 80.67 80.71 80.74 80.79 80.82 83.1 83.2 80.59 80.63 80.67 80.72 80.76 80 80 80.84 80.88 80.92 80.95 83.2 83.3 80.70 80.74 80.78 80.82 80.86 80.91 80.95 80.98 81.03 81.07 83.3 83.4 80.80 80.85 80.89 80.94 80.99 81.03 81.07 81.10 81.14 81.18 83.4 83.5 80.93 80.97 81.01 81.05 81.09 81 . 14 81.18 81.21 81.26 81.30 83.5 83.6 81.03 81.07 81.12 81.16 81.20 81.24 81.28 81.31 81.36 81.40 83.6 83.7 81.15 81.19 81.23 81.27 81.32 81 . 37 81.41 81.44 81.48 81.52 83.7 83.8 81.26 81.30 81.35 81.39 81.44 81.48 81.52 81.55 81.59 81.63 83.8 83.9 81.35 81.39 81.43 81.48 81.53 81.57 81.61 81.64 81.68 81.71 83.9 84.0 81.46 81.50 81.54 81.58 81.62 81.67 81.71 81.74 81.79 81.82 84.0 84.1 81.57 81.61 81.65 81.70 81.75 81.78 81.81 81.85 81.89 81.93 84.1 84.2 81.68 81.73 81.77 81.81 81.85 81.90 81.94 81.98 82.02 82.06 84.2 84.3 81.79 81.83 81.87 81.91 81.95 82.00 82.04 82.08 82.12 82.16 84.3 84.4 81.88 81.93 81.97 82.02 82.06 82.10 82.15 82.18 82.22 82.25 84.4 84.5 82.00 82.04 82.09 82.14 82.18 82.22 82.26 82.30 82.34 82.37 84.5 84.6 82.11 82.16 82.21 82.26 82.29 82.32 82.36 82.40 82.44 82.48 84.6 84.7 82.23 82.27 82.31 82.36 82.39 82.44 82.49 82.53 82.57 82.59 84.7 84.8 82.33 82.38 82.42 82.47 82.51 82.55 82.59 82.63 82.65 82.70 84.8 84.9 82.43 82.48 82.52 82.56 82.60 82.65 82.69 82.73 82.77 82.81 84.9 85.0 82.53 82.57 82.62 82.66 82.70' 82.75 82.79 82.83 82.87 82.91 85.0 85.1 82.63 82.68 82.72 82.77 82.81 82.86 82.91 82.95 82.98 83.03 85.1 85.2 82.75 82.79 82.84 82.89 82.93 82.97 83.01 83.04 83.08 83.12 85.2 85.3 82.86 82.91 82.95 82.99 83.03 83.08 83.11 83.15 83.19 83.25 85.3 85.4 82.96 83.00 83.05 83.09 83.13 83.18 83.23 83.26 83.30 83.34 85.4 85.5 83.06 83.11 83.15 83.19 83.23 83.28 83.32 83.35 83.39 83.43 85.5 85.6 83.17 83.21 83.25 83.30 83.34 83.38 83.42 83.45 83.49 83.54 85.6 85.7 83.28 83.33 83.38 83.41 83.46 83.50 83.53 83.57 83.61 83.65 85.7 85.8 83.37 83.42 83.46 83.50 83.55 83.59 83.64 83.67 83.71 83.75 85.8 85.9 83.48 83.53 83.57 83.61 83.65 83.69 83.74 83.77 83.81 83.85 85.9 86.0 83.57 83.61 83.65 83.70 83.74 83.78 83.83 83.86 83.90 83.94 86.0 86.1 83.70 83.75 83.79 83.83 83.88 83.92 83.97 84.00 84.04 84.08 86.1 86.2 83.80 83.84 83.88 83.93 83.97 84.02 84.06 84.10 84.14 84.17 86.2 86.3 83.89 83.94 83.98 84.02 84.07 84.11 84.15 84.18 84.23 84.27 86.3 86.4 83.99 84.03 84.08 84.13 84.17 84.21 84.25 84.28 84.32 84.36 86.4 86.5 84.10 84.15 84.19 84.24 84.28 84.33 84.37 84.40 84.44 84.48 86.5 86.6 84.20 84.25 84.30 84.34 84.39 84.43 84.46 84.49 84.53 84.58 86.6 86.7 84.30 84.35 84.39 84.43 84.47 84.51 84.55 84.59 84.64 84.68 86.7 86.8 84.40 84.45 84.49 84.53 84.58 84.62 84.66 84.70 84.74 84.78 86.8 86.9 84.50 84.54 84.59 84.63 84.68 84.72 84.76 84.80 84.84 84.88 86.9 15.0 15.2 15.4 15.6 15.8 16.0 16.2 16.4 16.6 16.8 Derivation Let S = % sugar in cossettes, P= apparent purity of cossettes, and X=standard extraction. Also let J=apparent purity of purified juice, and G=granulated factor, % on sugar. Then J 100 P 4P+60 10,000 (J -57) 43 J X = G (S-.60) XXVII. TABLES 251 TABLE 24 STANDARD STEFFEN EXTRACTION Based on 58 tree purity of "molasses produced from Steffen," and a total loss of 5.25% of the original sugar in the molasses worked. True True Pur. of .0 .1 .2 .3 .4 .5 .6 .7 .8 .9 PIT. of Pert. Pfr'. Washeo Washed Cake Cake 80 81 62.04 64.06 62.24 64.26 62.45 64.46 62.65 64.66 62.85 64.85 63.05 65.05 63.26 65.25 63.46 65.44 63.66 65.64 63.86 65.83 80 81 82 66.03 66.22 66.42 66.61 66.80 67.00 67.19 67.38 67.57 67.76 82 83 67.95 68.13 68.33 68.53 68.71 68.89 69.08 69.27 69.46 69.64 83 84 69.84 70.01 70.20 70.38 70.57 70.75 70.93 71.11 71.30 71.48 84 85 71.67 71.84 72.02 72.20 72.38 72.56 72.74 72.91 73.10 73.26 85 86 73.45 73.62 73.80 73.98 74.15 74.33 74.50 74.67 74.85 75.02 86 87 75.20 75.37 75.54 75.71 75.89 76.06 76.23 76.40 76.57 76.73 87 88 76.91 77.08 77.24 77.41 77.58 77.75 77.91 78.08 78.25 78.41 88 89 78.58 78,75 78.91 79.07 79.24 79.40 79.56 79.72 79.89 80.04 89 90 80.21 80.38 80.53 80.70 80.85 81.01 81.17 81.34 81.49 81.64 90 91 81.81 81.97 82.12 82.29 82.44 82.59 82.75 82.91 83.06 83.22 91 92 83.38 83.52 83.68 83.83 83.99 84.14 84.29 84.45 84.60 84.75 92 93 84.90 85.05 85.20 85.36 85.50 85.65 85.80 85.95 86.10 86.25 93 94 86.40 86.54 86.69 86.84 86.99 87.13 87.28 87.42 87.57 87.72 94 95 87.86 88.01 88.15 88.30 88.44 88.58 88.73 88.87 89.01 89.16 95 .0 .1 .2 3 .4 .5 .6 .7 .8 .9 Derivation Let W =true purity of perfectly washed cake Y =standard Steffen extraction 9475 (W-58) 225.6 (W-58) Then Y 42 W W TABLE 25 SPECIFIC GRAVITY OF VARIOUS MATERIALS WEIGHT IN POUNDS OF ONE CUBIC FT. 40-42 37-40 40-50 50-52 Beets Beet pulp, fresh Beet pulp, fermented. . Coal (Colorado lignite) Coke Lime, burned Limestone Molasses Sugar, raw Sugar, white 27 50-60 90 90 50-55 55 TRUE SP. GR. Sugar 1 .591 Lime, burned 2 . 30-4 . 20 Limestone, usually . . 2 . 65-2 . 70 252 METHODS OF ANALYSIS TABLE 26 INTERNATIONAL ATOMIC WEIGHTS, 1920 Symbol Atomic Weight Symbol Atomic Weight Aluminum Al 27 1 M^olybdenum Mo 96 Antimony Sb ion 2 Neodymium Nd 144 3 Argon A 39 9 Neon Ne 20.2 Ars6nic A 74 96 Ni c k e l Ni 58 68 Barium Fla 137 37 Niton (radium emanation) . . Nt 222 4 Bismuth Bi 208 Nitrogen N 14 008 Boron B 10 9 Osmium Os 190 9 Bromine Br 79 92 Oxvffen o 16 00 Cadmium Cd 112 40 Palladium . Pd 106 7 Caesium Cs 132 81 Phosphorus p 31 04 Calcium On 40 07 Platinum Pt 195 2 Carbon c 12 005 Potassium K 39 10 Cerium CP 140 25 Praseodymium Pr 140 9 Chlorine Cl 35 46 Radium Ra 226 Chromium Cr 52 Rhodium Rh 102 9 Cobalt Co 58 97 Rubidium Rb 85 45 Columbium Cb 93 1 Ruthenium Ru 101 7 Copper Cu 63 57 Samarium Sa 150 4 Dysprosium Erbium r y 162.5 167 7 Scandium Selenium Sc Se 44.1 79 2 Europium Fluorine Eu F 152.0 19 Silicon Silver Si Ag 28.3 107.88 Gadolinium Gd 157 3 Sodium Na 23.00 Gallium Ga 70 1 Strontium Sr 87.63 Germanium Ge 72 5 Sulfur s 32.06 Glucinum Gl 9 1 Tantalum Ta 181.5 Gold Au 197 2 Tellurium Te 127.5 Helium He 4 00 Terbium Tb 159.2 Holmium Ho 163 5 Thallium Tl 204.0 Hydrogen H 1 008 Thorium Th 232.15 Indium In 114 8 Thulium Tm 168.5 Iodine I 126 92 Tin Sn 118.7 Iridium Ir 193 1 Titanium Ti 48.1 Iron FP 55 84 Tungsten .... W 184.0 Krypton Kr 82 92 Uranium U 238.2 Lanthanum . . . La 139 Vanadium . . V 51.0 Lead Pb 207 20 Xenon Xe 130.2 Lithium Li 6 94 Ytterbium (Neoytterbium) . Yb 173.5 Lutecium Lu 175 Yttrium Yt 89.33 Magnesium . . . Me 24 32 Zinc Zn 65.37 Manganese . . Mn 54 93 Zirconium Zr 90.6 Mercury Hg 200 6 INDEX Acetic acid, dilute for lime cake 188 for saccharate cake 1S8 Acid insoluble 92 Acid, standard 193 Air compressor 178 Air entering furnaces, temper- ature 75 Alkali, standard 193 Alkalinity 11 Alpha-naphthol 188 detection of sugar by 14, 37 Alumina cream 188 Aluminum... 108, 109, 118, 134, 136 discs 105, 168 dishes 169 Ammonia, determination 123 total nitrogen as 95 Ammonium carbonate 189 molybdate 112 nitrate 112 oxalate 189 Apparatus 168 standardization of 179 Apparent purity 6, 106 table of factors 214 Arsenic, in sulphur 150 Asbestos, preparation of 94 Ash 9, 128, 149, 156 lixiviated 10, 93, 107 sulphated 9 Ash analysis 107 aluminum 108, 109 calcium 109 carbonic acid 113 chlorine Ill hypothetical combinations . . . 113 iron '..108, 109 lixiviated ash 107 magnesium 109 phosphoric acid 112 potassium 110 silica and insoluble 107 sodium 110 statement of analysis 114 sulphuric acid 112 Ashes analysis 131 preparation of samples 74 sampling 73 Atomic weights, table 252 Bacteriological examination of water 139 Balances 168 Barium chloride, general re- agent 189 for standardizing soap solu- tion ."189 Barium oxide 199 Basic acetate separation 108 Battery supply water 141 Baume, of molasses 101 hydrometers 184 scale 185 table 201 test 101 Beets (see also "cossettes") detn. of purity 17, 106 detn. of sugar 17, 105, 106 preparation of sample 102 rasping of 103 Beet laboratory tests 102 Beet rasp, see "rasp." Beet tailings 18 Benzoic acid 193 Blow-up thick juice, see "thick juice." Boiler house control 72 bibliography 79 Boiler water 38, 84 Brix 1 direct method 1 double dilution method 2 table 201 Burettes 181 Calcium 109, 118, 134, 137, 143 detn. as oxide 135 detn. as sulphate 135 volumetric method 137 Calcium acetate 123 Calcium oxalate scale 104 Calorific value . . .130 254 IN DEX Calorimeters 130, 186 Campaign average samples. 140, 141 CaO by soap solution 13 tables 224, 226 CaO by titration 12 CaO, sugar-soluble 49 Capsules 168 covers 168 Carbon 124 fixed 129 Carbon dioxide, see "carbonic acid." Carbonator 169 Carbonic acid 113, 121, 138, 145, 161 Caustic soda 199 Chlorine, detn. 97, 111, 119, 143 Clerget formula 6 Coal 126 bibliography 132 preparation of samples. . .73, 126 sampling 72, 126 Coal analysis 128 ash .*. 128 calorific value 130 fixed carbon 129 moisture 128 sulphur 129 volatile matter 128 Cochineal 190 Coke 126 bibliography 132 preparation of samples 127 sampling 127 Coke analysis, see "coal analy- sis." Cold water digestion 103, 105 Combinations, hypothetical 99, 113, 145 Condensed waters 37, 84 Cooler 169, 177 solution for 47 tests 57 Copper, determination 9, 116 Cossettes 16 Cotton seed cake 157 analysis 158 moisture 158 prepn. of samples 157 protein 1 5S sampling 157 Crude fat ,...67, 155 Crude fiber 156 Crude potash 90 analysis, see "crude potash analysis." as sacked 85, 86< preparation of samples 90, 92 sampling 90 Crude potash analysis 92 acid insoluble 92> chlorine 97 complete analysis 97 general 92j hydrosulphuric acid 98 hypothetical combinations ... 99 lixiviated ash 93 moisture 92 nitrogen 95 potash 93 screen test 97 sulphuric acid 98 total alkali as CQ 2 97 water insoluble 93 Crude protein 151, 158 Crusher 170, 177, 178 Cupric oxide tables 223 Cuprous chloride 191 Deposits, see "scales." Desiccators 2, 33 Diatomaceous earth 147 apparent specific gravity 147 moisture i*<* organic matter 148 sampling 147 silica 148 Diffusion juice 18 Disc, Keil, see "Keil disc." Disc pulverizer 170, 178 Dishes, moisture 169 Dorr thickener additional tests 6u discharge 63 feed 60 overflow 60 Draft 75 Dried pulp (see also "pulp") as sacked 66 leaving dryers o5 moisture in 62, 65, 66, 67 weekly analysis of 66 INDEX 255 Dry substance (see also "mois- ture") ^. . . 2 by oven drying 3 by refractometer 3 in filter press cakes 3, 55, 87 in pulp sold 70 in remelt sugar ^9 in uncarbonated liquors 86 Drying ovens 128, 169 Dust box i^3 Enterprise meat chopper. .170, 178 Eschka mixture 129 Ether, purification of 155 Evaporator 1 1 thick juice, see "thick juice." thin juice, see "thin juice." Excess water 29 Extraction, standard, tables beet 247 ..Steffen 251 Fat, see "crude fat." Feeding stuffs, see "foods and feeding stuffs." Fehling's solution 18 6 Fiber, see "crude fiber." Filter cloth wash water 30 Filter press cake 26, 28, 46, 52, 55, 84, 66 (see also "lime cake," "sac- charate cake," etc.) First saturation juice 20 liquor 82 Fixed carbon 129 Flasks 178, 180 Flue gas analysis 75 tables 229, 241, 242j temperature 75 Flume pulp 20 Foods and feeding stuffs 151 ash 156 crude fat 155 crude fiber 156 crude protein 151 moisture 151 nitrogen free extract 156 preparation of sample 151 Formulas Clerget G hydraulic presses 176! raffinose 6 Gages, draft 75 Gas, carbonation 85 flue, see "flue gas." lime kiln 23 General methods 1 Glycerin 170 Gooch crucibles 94 Graduation marks 181, 185 Granulated, available, tables per cent on dry substance 245 per cent on sugar 246 Granulated sugar, see "white sugar." Graphite 124 Green syrup, see "high" and "low" green syrup. Grinding machinery 170 Heat balance 87 Heat losses, calcn. of 76 tables 229, 241, 242 High green syrup 32 High wash syrup 32} Hilgard sieve cylinder 165 Hot water digestion 17, 106 Humus 16l Hydrochloric acid 190 (see also "muriatic acid.") Hydrometers 171, 182 Hydrometer jars 171 Hydrosulphuric acid 98, 121 Hypothetical combinations 99, 113, 145 Ignition of precipitates 135 Indicators 190 Insecticides 200 Insoluble 116, 134, 136 acid 93 water 93 Inversion hydrochloric acid for 190 sugar by 4 256 INDEX Invert sugar 8 in thick juices 8, 221 in thin juices 9, 222 Iron 108, 109, 118, 134, 136, 143 Jar mill 170, 178 Keil disc ...103, 168, 177 Kieselguhr, see "diatomaceous earth." Lead acetate basic 190 dilute 105 neutral 190 table 217 Light filter 175 Lime (see also "calcium") cake, first presses 26 cake, second presses 28 kiln gas 23 milk of 25, 243 powder 48 salts, see "CaO by soap soln." sewer 28 to slacker 25 Limestone 133 general 133 preparation of sample 133 sampling 133 Limestone analysis 134, 136 calcium 134, 137 calculation of results 138 carbonic acid 138 gravimetric method 134 insoluble 134, 136 iron and aluminum 134, 136 magnesium 136 rapid method 136 sulphuric acid 13ft Liquor entering factory 82, 86' Liter 179 Lixiviated ash 10, 93, 107 Losses, see "heat losses." Low green syrup 35 Low wash syrup 35 Magnesia mixture 112 Magnesium. . .109, 118, 136, 138, 143 Main sewer 31 Marking glassware 181, 185 Massecuite 31, 34, 35 alkalinity of 12 Meat chopper 170, 178 Melted sugar (see also "melter"), 44, 45 Melter, sugar 36 Methyl orange 190 Methyl red 190 Milk of lime 25, 243 Milliliter 179 Miscellaneous 198 supplies 200 Moisture (see also "dry sub- stance") 2 in coal and coke 128 in cotton seed cake 158 in crude potash 92 in diatomaceous earth 148 in dried pulp 62, 65, 66, 67 in filter press cakes 3, 55, 87 in foods, etc 151 in remelt sugar 39 in soil 160 in sulphur 149 in white sugar 32, 198 Molasses 100 Baume 101 bought 100 in storage 101 produced 36, 39 sold 100 to pulp dryer 62 worked 39, 47, 80 Molybdate solution 112 Muriatic acid 199 Naphthol, see "alpha-naphthol." Nitric acid, standard 195 Nitrogen, determination . . . .95, 151 Nitrogen-free extract 156 Normal solutions, equivalents of 244 Normal weight 172 Oil determination 124 Organic coefficient 11 Organic matter 145, 148 Orsat apparatus 24, 181 reagents 191 Ovens, see "drying ovens." Oxalic acid 123 Oxygen 131 Pan storage tanks 31, 34 Pebble mill 170, 178 Percolation tests . . 33 INDEX 257 Perfectly washed cake ... 39, 53, 56 Phenolphthalein 190 Phosphoric acid 112, 121 Pipettes 180 automatic 105, 181 Platinic chloride solution 191 Platinum, care of 171 recovery 191 Polariscopes 172, 185 adjustment of 176 care of 176 cover glasses 175 illumination 174 installation 174 light filter 175 normal weight 172 scale 172, 186 specifications 172 temperature, effect of 173 tubes 175, 186 verification 173 Polarization 3 tables 218, 220 temperature, effect of 173 Potash bulbs 122 control (beet campaign) 80 control (potash campn.)..82, 141 crude, see "crude potash." determination, see "potas- sium." Potassium, detn 87, 93, 110, 118 Potassium chromate indicator. .144 hydroxide solution 191 permanganate 137 Precipitates, ignition of 135 Presses 176, 178 Protein, see "crude protein." Pulp (see also "dried pulp"). and pulp water 19 and pulp water, flume 20 dryer control 62 entering presses 64 entering silo 69 flume 20 leaving presses 65 silo control 69 sold 69, 228 water 19, 20 Pulverizer ..170, 178 Purity 6 apparent 6, 106 table of factors 214 true 8 Pyrogallol 191 Radiator, Hillebrand 177 'Raff inose 4, 6 formula 6 Rasp 102, 168, 177 care of 103 Raw massecuite, see "remelt massecuite." Raw sugar, see "remelt sugar." Reagents 188 Refractometers 3, 177, 186 Regular factory control 16 Remelt massecuite from crystallizer 35 from pan 34, 39 Remelt pan storage tanks 34 Remelt sugar 35, 39, 44 Saccharate cake cold 39, 52, 80 hot 39, 55, 80 perfectly washed 39, 53, 56 Saccharate milk 39, 56 Saccharimeters, see "polari- scopes." Sand, sea 192 Scales 115 aluminum 118 ammonia 123 calcium 118 carbon 124 carbonic acid 121 chlorine 119 copper 116 graphite 124 hydrosulphuric acid 121 insoluble 116 iron 118 magnesium 118 oil 124 oxalic acid 123 phosphoric acid 121 potassium 118 preparation of sample 115 qualitative examination 115 quantitative examination 116 sampling 115 258 INDEX silica 116 sodium 118 sugar 124 sulphuric acid 119 sulphurous acid 120 zinc 118 Screen tests 49, 97 Sea sand 192 Second saturation juice 21, 42 Sewer lime 28 main 31 Sieve cylinder 165 Sieve tests .49, 97 Silica 107, 116, 142, 148 Silver nitrate solution 144 Slacking test 49 Soap solution CaO by 13 standard 196 tables 224, 226 Soda ash 199 caustic 199 Sodium 110, 118 ammonium phosphate 193 carbonate 192, 193 (see also "soda ash") chloride 144 hydroxide, standard 195 oxalate 137 phosphate 193 thiosulphate 117 Soil 160 preparation of sample 160 sampling 160 Soil analysis 160 carbon dioxide 161 humus 161 inorganic constituents 161 mechanical analysis 162 moisture 160 nitrogen, total 160 statement of analysis 166 volatile matter 160 water capacity 165 water soluble 161 Solids, total 142 Solution for cooler . . 47 Specific gravity tables of sugar solutions 201 of various materials 251 Speeds of lab. machinery 177 Standard acid and alkali 193 Standardization of apparatus . . . 179 bibliography .186 Starch indicator 117 Steam calculation 87 Steffen process control 47 Storage tanks 31, 34, 101 Sugar (see also "white" and "remelt" sugar) by cold water digestion 105 by direct polarization 4 by hot water digestion ... 17, 106 by inversion 4 detection by alpha-naphthol . . 14, 37 in scales 124 Sugar melter 36 Sugar-soluble CaO 49 Sulphate cake 46 Sulphate control 42 Sulphated ash 9 Sulphates, see "sulphuric acid." Sulphides, see "hydrosulphuric acid." Sulphites, see "sulphurous acid." Sulphur 149 in coal 129 sampling 149 Sulphur analysis 149 arsenic 150 ash: 149 moisture 149 sulphur 149 Sulphuric acid detn. ...11, 98, 112, 119, 136, 144 standard 194 Sulphurous acid 120 Suspended matter 145 Sweet water 30 Tables 201 (see table of contents for list) Tailings, see "beet tailings." Temperature correction tables for Abbe refractometer 216 for Brix hydrometers. . .215, 216 INDEX 259 Temperature data ...40, 9, 67, 8G Thermometers 178, 185 Thick juice blow-up 23, 43 evaporator 22, 39 Thick liquor 83, 85, 86 Thin juice, evaporator 22 Thin liquor 83, 86 Third saturation juice 21, 43 Total solids 142 Total sulphates 142 True purity 8 Undetermined 40 Vacuum pump 178 Volatile matter 128 Volumetric apparatus 178, 179 Wash syrup, see "high" and "low" wash syrup. Wash water cold 51 hot 52 Waste water cold press 50 cooler 49 hot filter 61 total 50, 81 Water 139 bacteriological examination . .139 battery supply 141 boiler 38, 84 condensed 37, 84 distilled 197 from presses 63 from pulpefanger 63 quality of 7, 197 sampling 139, 140 Water analysis 141 calcium 143 carbonic acid 145 chlorine 143 example 145 hypothetical combinations . . 145 iron 143 magnesium 143 organic and volatile matter.. 145 silica 142 statement of analysis 146 sulphuric acid 144 suspended matter 145 total solids 142 total sulphates 142 Water capacity 165 Water insoluble 93 Water soluble 161 Weekly analysis of dried pulp . . 66 Weekly composite samples 38, 80, 86, 141 Weights 185 White massecuite 31, 39 White pan storage tanks 31 White sugar moisture in 32, 198 percolation tests of 33 sampling of 198 sulphuric acid in 44 Zinc, determination 118 Zinc nitrate solution . . . 197 YC 704(8 468640 '^S'^ UNIVERSITY OF CALIFORNIA LIBRARY