OS- LIBRARY UNIVERSITY OF CALIFORNIA, Received. Accessions No. .^4^^2^ Shelf No. SUG-AK ANALYSIS. FOR REFINERIES, SUGAR-HOUSES, EXPERIMENTAL STATIONS, ETG., AND AS A HANDBOOK OF INSTRUCTION IN SCHOOLS OF CHEMICAL TECHNOLOGY. BY FEEDINAND Gk WIECHMANN, PH.D., i Instructor in Chemical Physics and Chemical Philosophy, School of Mines, Columbia College ; Consulting Chemist to the Havemeyers and Elder Sugar Refining Company, Brooklyn, N. TJHI7EESITY NEW YORK: JOHN WILEY & SONS, 53 EAST TENTH STREET. 1890. COPYRIGHT, 1890, BY JOHN WILEY & SONS. ROBERT DRUMMOND, FERRIS BROS., Electrotyper, Printers Pearl Street, 326 Pearl g^ York - New York. INSCRIBED TO HIS TEACHER CHARLES F. CHANDLER, PH.D., PROFESSOR OF CHEMISTRY, COLUMBIA COLLEGE, AS A SLIGHT TOKEN OF SINCERE GRATITUDE, ESTEEM AND REGARD. THE AUTHOR. //- PREFACE. IT lias been the aim of the writer to prepare a concise yet thorough treatise on Sugar Analysis that should prove of service to the practising chemist as well as to the student of this branch of analytical chemistry. Within the past few years numerous changes have been made in the older methods of sugar-analysis, new methods have been devised, and many researches of im- portance to sugar-chemistry have been accomplished. The. current literature of the day devoted to sugar and its interests, abounds in matter pertinent to the subject. A great number of these investigations have, however, appeared only in foreign journals and have therefore not been accessible to all ; moreover, they occur scattered through so many different publications that a critical study of the same involves no inconsiderable outlay of time and labor. A work that should give a general survey of this field seemed therefore both desirable and timely, and it has been with the aim indicated in view, that this publication was undertaken. The greatest difficulty encountered was the making of a proper choice from the wealth of material at hand. The schemes selected and here offered, embrace those methods of analysis which, after careful investigation, and, in many cases, after prolonged trial in practice, have seemed to the writer best adapted to the requirements of a technical laboratory. iii IV PREFACE. A glance at the Table of Contents will show at once the plan and scope of this manual. Instead of taking up for discussion, as is usually done, the different products met with in sugar-laboratories, such as raw sugars, refined sugars, liquors, molasses, etc., and describing for each in turn the determination of their constituents, it has been deemed more expedient to dis- cuss the methods of determining the individual constitu- ents, as sucrose, invert-sugar, water, ash, etc., independ- ently of the products in which they may occur, and then to add such comments and suggestions as certain contin- gencies would seem to call for. By the adoption of this plan numerous repetitions have been avoided. Wherever feasible, examples have been inserted in the text to aid in the understanding of the principles dis- cussed, and of the calculations explained. Numerous references are given throughout; these will, it is hoped, incite to a study of the original memoirs. The tables have been selected with the greatest of care, prompted by a desire to introduce only the most accu- rate. To ensure uniformity of basis, several of these tables have been calculated expressly for this issue. The publication of the formulae by which the different tables were obtained, should prove a welcome feature to the student. A list of books and of periodical literature bearing on Sugar Analysis is appended. Asterisks attached to titles show that the publications so marked were consulted in the preparation of these pages, and indicate the obligations of SCHOOL OF MINES, THE AUTHOR. COLUMBIA COLLEGE, 1890. TABLE OF CONTENTS. CHAPTER I. Polarization 1 Polariscopes: construction adjustment examination quartz-plates polariscope-tubes 3 Hydrometers : varieties used range of scales 13 Methods of Testing Hydrometers : by means of : pyknometer solutions of chemically pure sugar polariscope 15 Graduation of Flasks : in true cubic centimetres Mohr's method 18 Verification of Graduated Glass Vessels, in true Cubic Centimetres. 19 Thermometers : examination conversion formulae 20 Balances : requirements examination 21 Weights ; verification 22 CHAPTER II. Sampling Sugars and Molasses : manner of sampling percentage of cargo sampled representative sample 23 Determination of Color of Sugar and Sugar Solutions : Dutch standards colorimeters , 25 Determination of Density of Solutions : by : specific-gravity flask pipette and beaker hydrometers glass spheres hydrostatic balance. 26 Determination of Alkalinity 30 Determination of Acidity 31 Test for Sulphurous Oxide in Sugar 32 CHAPTER III. Determination of Sucrose in the Absence of other optically active Substances 33 Optical Analysis : with balance without balance 33 Quotient of Purity, or Exponent: determination by: drying to con- stant weight aid of hydrometer Ventzke's method Casarnajor's method true and apparent quotient of purity calculation to dry 38 substance Gravimetric Analysis 42 v VI TABLE OF CONTENTS. CHAPTER IV. Determination of Sucrose in the Presence of other optically active Substances 44 Clerget's Inversion Method 44 Sucrose in the Presence of Raffi nose : German government method- correction for temperature of observation reference-list to other methods , : 46 Sucrose in the Presence of Dextrose : qualitative tests quantitative methods : hot polarization gravimetric 49 Sieben's Process for Destruction of Lamilose 59 Determination of Sucrose, Dextrose, and La3vulose : Winter's method gravimetric method , 61 CHAPTER V. Invert-Sugar 64 Qualitative Examination 64 Quantitative Determination : formula for Fehling's solution 65 Volumetric Methods: Soxhlet's Fehling's dextrose solution for standardizing Fehling's solution 65 Gravimetric Methods : Meissl-Herzfeld Bodenbender and Scheller. . . 69 Soldaini's Solution 74 CHAPTER VI. Water : determination by drying in : air-bath inert gas vacuum 76 Ash : methods of determination Scheibler's Von Lippmann's carbon- ization 77 Quantitative Analysis of Sugar-Ash 79 Suspended Impurities : determination of : total inorganic organic.. 80 Determination of Woody Fibre 82 Detection of the Sugar-Mite 82 CHAPTER VII. Organic Non-Sugar : determination by basic acetate of lead 83 Classification of Organic Bodies accompanying Sucrose : organic acids nitrogenous substances non-nitrogenous substances 84 Schemes for Analysis of the Organic Acids : non-volatile acids- rare non-volatile acids volatile acids approximate determination of organic acids : non-volatile and volatile 85 Determination of Total Nitrogen 95 Non-Nitrogenous Organic Substances 96 Determination of Pure Cellulose. . 96 TABLE OF CONTENTS. Vli CHAPTER VIII. Notes on the Reporting of Sugar- Analyses : forms of reports inter- pretation of analyses nature of reducing sugar 98 Rendement : determination by the Payen-Scheibler process 102 Calculation of Reudement: United States of America England- France Germany 105 Duty : United States of America 106 Calculation of the Weight of Solids and Liquids from their Specific Gravity : weight in pounds per cubic foot weight of a gallon in pounds 107 CHAPTER IX. Synonyms : English German French , 108 References to Literature on Sugar Analysis : books periodicals 110 Tables 113 Index 183 SUGAR ANALYSIS CHAPTEE I. POLARIZATION POLARISCOPES HYDROMETERS FLASKS THERMOMETERS BALANCES WEIGHTS. Polarization. If a ray of light strikes a glass mirror and makes an angle of about 55 with the normal of the mirror, the ray is not only reflected, but is endowed with certain properties, and is said to be polarized. In Fig. 1, ab is the incident ray, be the polarized ray. A plane conceived as passed through abc is called the plane of polarization. . If a polarized ray is allowed to fall upon a yp second mirror, parallel to the first, it is again / reflected at the angle above mentioned. If this second mirror is turned around be, its inclina- tion to the horizontal being preserved un- changed, the intensity of the reflected ray FIG.I. continuously diminishes until, when the rotation has been carried through 90, the light is extinguished com- pletely. If the rotation be carried beyond this point the mirror becomes again illumined ; and when it has been turned through 180, the reflection is again at its maxi- mum of brightness. In other words, the intensity of the reflected light is greatest when the incident ray and the 2 SUGAR ANALYSIS. polarized ray, after reflection from the second mirror, are in the same plane, and least, when these rays are in planes at ri2;ht angles to each other. o o Polarization of light can also be produced by other means : by repeated single refractions, or by double re- fraction in certain crystals Iceland-spar, for instance. If a plate of quartz, cut at right angles to its prin- cipal axis, is inserted between two mirrors placed as above described, and traversed by a polarized ray, the image of the quartz will appear in color in the upper mirror. The color of the image changes with the turning of the mir- ror ; the order in which the colors appear is the same as found in the solar spectrum : red, yellow, green, blue, and violet. This phenomenon is termed circular polarization. It depends on the property possessed by quartz of rotating to a different degree the planes of polarization of the various colored rays which compose white light. One variety of quartz shows these colors in the order named when the mirror is turned to the right ; a second variety of the mineral exhibits the colors in this sequence only when the rotation of the mirror is to the left. These varieties of quartz are respectively termed right-rotating and left-rotating, or dextrogyrate and laevogyrate. Among other bodies which share with quartz the property of circular polarization are the sugars when in solution. Some of the sugars are dextro-rotatory: for instance, sucrose, dextrose, and raffinose; others rotate the plane of polarized light to the left, as Isevulose and sorbinose. The extent to which the plane of polarized light is turned by quartz, by a sugar solution, or any other opti- SUGAR ANALYSIS. 3 cally active substance, depends on the thickness of the layer which the polarized ray has to traverse. The thicker the plate or the longer the column of solution, the greater the rotation of the ray. Whereas in the case of a quartz-plate the thickness of the plate is the only factor to be considered, in sugar solutions the concen- tration of the solution, i.e., the amount of sugar in the solution, must be taken into account. Polariseopes. Basing on this property of circular polarization, instruments have been constructed by which the strength of solutions containing optically active sub- stances can be determined. They are called polariscopes or polarimeters. Polariseopes intended for general scien- tific work are provided with a circular disk, graduated in such a manner that the angle of rotation can be con- veniently read. Instruments intended for some special purpose, as, for instance, for sugar analysis, are generally provided with a scale which, if certain directions have been followed in the preparation of the solution, will at once indicate in percentage the amount of the optically active substance present. Polariseopes designed especially for sugar analysis are termed saccharimeters. The principle on which these instruments are con- structed is briefly this : A ray of light is polarized by passing through a prism, called the polarizer, and gener- ally made of Iceland-spar; the ray is then made to traverse a column of sugar solution of known length. Emerging from this, it passes through a second prism of Iceland-spar, the analyzer, which corresponds to the sec- ond mirror in the apparatus previously described. It now only remains to ascertain the extent to which the plane of polarized light has been rotated by the sugar 4 SUGAR ANALYSIS. solution. The arrangements by which this is effected differ in the various forms of saccharimeters, but in the more modern instruments it is generally accomplished by allowing the light on its emergence from the analyzer to pass through a layer of quartz, the thickness of which (capable of accurate measurement) can be so regulated as to exactly compensate the rotation produced by the sugar solution. It is assumed that the rotatory dispersion of sugar corresponds to that of quartz. The field of vision of a saccharimeter is either one of color, or else exhibits, when correctly set at zero, a uni- form faint tint ; polariscopes showing the latter are known as half-shade instruments, and can be used by color-blind persons, as well as by others. The arrangement of the optical parts of a saccha- rimeter is shown in the accompanying Figs. 2 and 3. BZS7D 1 2 Fig. 2. Solei I- Ventzke-Scheibler Polariscope. 1. Magnifying-glass for reading scale. 2. Telescope for observing field of vision. 3. Nicol prism, analyzer. 4. Quartz-wedge, fixed, bearing vernier. "i 5. Quartz-wedge, movable, bearing scale. I Rotation 6. Quartz-plate. \ Dextr - rotator y if 4 and 5 a laevo-rotatory. [Compensator. ' 1 Lsevo-rotatory if 4 and 5 are dextro-rotatory, j 7. Double quartz-plate (dextro- and laevo-rotatory). 8. Nicol prism, polarizer. 9. Quartz-plate, dextro- or leevo-rotatory. > , , 10. Nicol prism. SUGAR ANALYSIS. 10 11 5 6 Fig. 3. Double-wedge Compensator Polariscope, Schmidt and Haensch Construction. 1. Eye-piece. 2. Objective. 3. Nicol prism, analyzer. 4. Quartz-wedge."! 5. Quartz- wedge. [Constituting the Double- 6. Quartz-wedge. [ wedge Compensator- 7. Quartz- wedge. J 8. Lens. 9. Nicol prism. 10. Lens. 11. Lens. The scales of saccharimeters are constructed by ascer- taining, the number of degrees, minutes, and seconds which a definite amount by weight of pure sugar dis- solved in water and made up to 100 cubic centimetres will rotate the polarized ray. This is marked as 100, and the scale is then divided into one hundred parts. If the same weight of an impure sugar is brought into solution and polarized under the same conditions, the reading in the polariscope of course at once expresses percentage of the active substance present. The scales of different saccharinieters have their 100 mark correspond to different weights of pure sugar. In the Duboscq instrument it is 16.192 grammes, in Wild's apparatus it is 40.000 grammes, and in the Ventzke-Soleil 26.048 grammes. These values are termed the "normal weights" of the respective instru- ments. SUGAR ANALYSIS. EQUIVALENCE IN DEGREES OF DIFFERENT SACCHARIMETERS. Grammes of Sugar in 100 Cubic Centimetres. 1 scale of Mitscherlich = 0.750 1, " Soleil-Duboscq = 0.1619 1 " Yentzke-Soleil = 0.26048 1 " " Wild (sugar scale) = 0.100 1 " " Laurent and Duboscq (shadow) = 0.1619 One-degree on the Scale of Corresponds to Corresponds to Corresponds to Corresponds to Mitscherlich Mitscherlich. Soleil-Ventzke. 2.870 Soleil-Duboscq. 4. 6^S Wild . Soleil-Ventzke o. 346 I 608 2.64-8 ' ( v^.^u 0.215 0.620 I .610 ^Vild (sugar scale) .... o i^^ o. 384. 618 EQUIVALENCE IN CIRCULAR DEGREES. J 1 Soleil-Duboscq = 0.2167 J 1 " " = 0.2450 J 1 Soleil-Ventzke = 0.3455 J 1 " " = 0.3906 circular degree D. J. D. J. The letters J and D represent certain rays of light. The former signifies the mean yellow or transition tint, the latter the sodium ray. The amount of rotation which the plane of polarization experiences, called the angle of rotation, varies with the wave-length of the ray : it is least for the red, and greatest for the violet ray. In saccharimeters using white light (gas or lainp) r this value is generally given for the transition-tint, which means the color complementary to mean yellow light. In order to adjust a polariscope, first obtain by the telescope a sharp and clearly-defined view of the field. SUGAR ANALYSIS. 7 Then turn the screw attached to the quartz-wedge until both halves of the field are, in color instruments, of the same tint; or if the polariscope is a half-shade apparatus, until both halves of the field are equally illumined. If the instrument is provided with double-wedge compensation, the red scale is first set exactly at zero, and the manipulation is then carried out as described above. When this has been done the position of the scale is carefully read through the magnifying-glass. The zero of the scale should be, exactly in line with the zero mark on the vernier; if this is not the case, they must be brought into the -required position by a slight turning of the screw-micrometer provided for the purpose. Care must be taken that the screw in connection with the analyzer be not mistaken for. the other screw, or the whole apparatus will be thrown out of order. If it is impossible to obtain a uniform shade or tint on both sides of the centre line of the field, the polarizer and the analyzer must be brought into adjustment. This is done by removing the movable and the sta- tionary quartz-wedges, as well as the compensation quartz-plate; the cover is then closed, and the key hav- ing been inserted in the screw-head connected with the analyzer (this screw-head is generally placed on the right- hand side of the polariscope), the key is turned until the tint in both halves of the field is uniform. The wedges and the plate which had been removed are then replaced, and the zero-point accurately ad- justed. When the instrument has been correctly set at zero, SUGAR ANALYSIS. a quartz-plate of known value, preferably one approxi- mating the average test of the sugar solutions to be examined, is inserted in the instrument, and the correct- ness of that part of the scale ascertained. The zero-point should be determined before every observation ; where press of work renders this impracti- cable, the observation should be insisted on at least twice daily in the morning before a polarization is made, and again in the middle of the day. When a solution is introduced for reading, the tele- scope must first be properly focussed, as before stated, to insure a clear and sharply defined view of the field. If the scale stood at zero before the tube filled with the solution was introduced, a glance through the glass will after its introduction show the halves of the field to be of different colors; or, if a half-shade polariscope is used, one half of the field will appear dark and the other light. The screw attached to the quartz-wedge is then turned until equality in tint or shade shall have been restored to the whole field. It then only remains to read the scale. Most instru- ments have the degrees divided into tenths. First it must be determined how many whole degrees the zero of the scale is removed from the zero of the vernier. When this has been ascertained, attention must be given to the tenths of a degree indicated. The number of divisions marking tenths on the vernier are counted until one is found which coincides perfectly with a division on the movable scale, that is to say, which appears to form a continuation of that line. This division repre- SUGAR ANALYSIS. sents the number of tenths indicated. The accompany- ing figure, for instance, shows 30.7 degrees. \ } 2( u ) 30 1 1 1 1 1 f f P P If 40 / 111 ] Ml 1 II ill A 1 1 1 1 1 I I I I I lit 11 1 1 Fig. 4. The sources of error in saccharimeters are numerous and therefore every instrument before being placed in use, should be carefully examined. The principal difficulties that may be encountered are the following : The scale may be too long or too short. Adjust the zero-point exactly. Make 100 c.c. of a sugar solution by dissolving the normal weight of chemically pure sugar* in water, and polarize. This solution should read 100 degrees (per cent) on the scale if the instrument is correct. If it does not read 100, the instrument should be rejected. The scale may be right in some places, and wrong in others. This is the case when the surfaces of the quartz- wedges are not perfectly plane. In half-shade polari- scopes provided with double compensation wedges, this cannot occur, as any inequality would be noticed at once. In other polariscopes, the scale may be examined by pure sugar solutions of different densities, by means of the " control tube" of Schmidt and Haensch, or by quartz-plates. The following figures, taken from a table calculated by Schmitz, show the number of grammes of pure sugar which must be made up to 100 c.c. aqueous solution in * For preparation of chemically pure sugar see page 17. 10 SUGAR ANALYSIS. order to show the corresponding degree on a polariscope having ,2 6. 04 8 grammes for its normal weight: Polariscope Degrees. Grammes C. P. Sugar in 100 c.c. solution. Polariscope Degrees. Grammes C. P. Sugar in 100 c.c. solution. Polariscope Degrees. Grammes C. P. Sugar in 100 c.c. solution. I . 0.260 35 9-W 69 17-954 2 0.519 36 9-357 70 18.216 3 0.779 37 9.618 71 18.476 4 1.039 38 9.878 72 18.738 5 1.298 39 10.138 73 18.998 6 1.558 40 10.398 74 19.259- 7 I.8l7^ 4i 10.659 75 19.519 8 2.078 42 lo.gig 76 19.781 9 2,337 43 11.180 77 20.042 10 2-597 44 11.440 78 20.302 ii 2.857 45 11.70; 79 20.564 12 3.H7 46 11.961 80 20.824 13 3.376 47 12.222 8r", 21.085 14 3.637 48 12.482 824^ 21.346 15 3.896 49 12.743 83 21.608 16 4.156 50 I3.003 84 21.868 17 4.416 51 13.264 85 22.130 18 4.676 52 13.524 86 22.391 19 4.936 53 13.784 87 22.652 20 5.196 54 14.044 88 22.912 21 5.456 55 14.305 89 23.174 22 5.7i6 56 14.566 V 90 23.435 23 5.976 57 14.826, 9 1 23.696 24 6.236 58 15.087 92 23-957 25 6.496 59 15-347 93 24.219 / 26 6.756 60 15.608 94 24.480 < 27 7.016 - 61 15.868* 95 24.742 28 7.276 62 16.130. 96 25.002 29 7.536 63 16.390 97 25.265 30 7.796 64 16.651 98 25.525 3 1 8.056. 65 16.912 99 25-787 32 8.316. 66 17.173 IOO 26.048 33 8.577 67 17-433 34 8.837 68 17.694 This method of testing requires a separate solution for each degree of the scale which is to be examined. If the weights necessary to this mode of examination are not available, the tests can be made by dissolving the normal weight of chemically pure sugar in different vol- umes of water at the normal temperature. Thus with a SUGAR ANALYSIS. 11 / German saccharimeter 26.048 grammes of such sugar will, when dissolved in 100 c.c. water polarize 100.00 degrees. " 105 " " " 95.23 " " 110 " " " 90.90 " " 115 " " 86.95 " 120 " " " 83.33 " If a control- tube is used, but few solutions are needed, as this tube is so arranged that it can be lengthened or shortened at will. A funnel receives the superfluous solution when the tube is shortened, and a scale attached, shows the length of the column in millimetres. A simple calculation gives the reading which will be shown by the polariscope if this is correct. If quartz-plates are used to test the accuracy of dif- ferent parts of the scale, care must be taken that the sur- faces of the plates are perfectly plane, that they are inserted in the optical axis of the instrument and at right angles to it. The quartz-plates themselves should, before being used to control polariscopos, be examined as to their accuracy. One of the ways of ascertaining their value, that is to say, the amount by which they rotate a plane of polarized light, is to measure their thickness.* This measurement is effected most accurately by means of a spheroineter. This consists of a movable screw supported in the centre of three arms, upon which the apparatus rests. The screw is provided at its lower end with a steel point ; near its upper end there is fast- ened a circular plate of metal, the circumference of which is divided into several hundred equal divisions. Fastened * Open to objections, because the specific rotatory power of quartz is not a constant value. Zeitschrift des Vereines fur Rubenzucker-Industrie. Vol. 12 SUGAR ANALYSIS. to one of the supporting arms is a metal bar, also bearing a graduation ; its graduated edge is placed at right angles to the circular disk. Parallel to the latter, and attached to the bar, is a sliding-scale which can be set and fastened at any desired height. The graduation of the sliding-scale is so made, that nine of its divisions correspond to ten divisions on the disk. When the thickness of a plate of quartz, for instance, is to be measured, the screw is first adjusted in such a manner that it shall just touch the perfectly level surface on which the apparatus has been placed. The sliding-scale is next fastened on the bar exactly on a level with the circular disk. Suppose the latter to bear five hundred equal divi- sions, and the graduated bar to be divided into halves of a millimetre. The threads of the screw are so cut that one complete revolution of the screw, indicated by the graduated disk fastened to it, raises the screw through one half of a millimetre. To effect the measurement the screw is first raised sufficiently so as to allow the quartz- plate to be slipped beneath it ; when this has been done, the screw is carefully lowered until contact is secured between its point and the quartz-plate. From the num- ber of revolutions through which the screw has been turned, the thickness of the quartz-plate is determined ; with a spherometer graduated as here assumed, the meas- urement will be exact to the one ten-thousandth part of a millimetre. Besides giving attention to the points already referred to, care must be taken that the Nicol prisms and the lenses are not dusty, and that the illumination is perfect. SUGAR ANALYSIS. 13 The light must be steady and of an unvarying intensity, as the field of vision is materially affected by the flicker- ing of the flame. The end of the instrument must not be placed too near the light, as the heat affects the cement which holds the prisms in position. The polariscope-tubes must be of exactly the pre- scribed length, as the amount of deviation of the polarized ray produced by an optically active substance depends, among other conditions, on the length of the column of the substance which it traverses. The length of tubes can readily be determined by measuring them with a metal rod made of the standard length. The ends of the pol- arization-tubes must be ground perfectly plane-parallel. Another point to be borne in mind is the fact that the glass covers of the polarization-tubes may be optically active, either by nature of the glass, by being screwed down too tight, or by not having both surfaces perfectly parallel. The latter difficulty can be readily recognized by taking a glass cover between two fingers and rotating it rapidly, at the same time looking through it at some fixed object. If the latter seems to be moving, the glass is not plane-parallel, and should be rejected. Hydrometers The hydrometers used in the analysis of saccharine solutions embrace specific-gravity hydrome- ters and instruments graduated according to an arbitrary scale. To the latter belong the Baume hydrometers, and the Brix or Balling spindles. The degrees of a Brix hy- drometer indicate percentage by weight of sugar, when immersed in a solution of pure sugar. The suggestion has been made to replace the Saurae" scale by a scale graduated in the so-called densimetrio degrees. 14 SUGAR ANALYSIS. These values are found by taking the specific gravity corresponding to any given Baurne degree, ignoring the unit, and dividing the decimals by 100. Example. Baum Degrees. Densities. Densimetric Degrees. 1. 0000 0.00 5 1.0356 3.56 10 1.0731 7.31 50 1.5161 5I.6I This scale has, however, not yet been adopted in general practice. The range of scale in each and all of these hydrom- eters of course varies greatly, according to the ideas and preference of the makers, and of those who use the in- struments. The following will be found to be convenient graduations for the ordinary requirements of refinery and laboratory : Specific-gravity Scale. Range from 1.095 to 1.106. The scale bears twelve full divisions, and these are di- vided into halves. Temperature of graduation, 17.5 C. The Brix Hydrometers. Range from to 28, and covering three instruments : the first from to 8, the second from 8 to 16, the third from 16 to 28. Each degree is divided into tenths. Tfye jBaume Hydrometers for Liquids hea/oier than Water. For general use in the refinery, a scale on a single instrument ranging from to 50, and divided into quar- ters or halves, will prove sufficient. For work at the "blow-ups" the range of scale is from 27 to 32, and each degree is divided into tenths. For the syrup-boiler a scale from 32 or from 38 to 44, also divided into tenths, is desirable. For laboratory work the range is SUGAR ANALYSIS. 15 from to 45, best carried over three or more instru- ments : for instance, from to 20, from 20 to 35, and from 35 to 45 ; the subdivision to be in tenths of a degree. It is a matter of great importance that the hydrome- ters used in analytical work be correct. Every instru- ment should be examined in at least three places, these being preferably chosen at points corresponding to the upper, the middle, and the lower part of the scale. If a correct instrument is at hand (ascertained to be correct by careful examination), other hydrometers of the same scale are readily tested by comparison with the standard hydrometer. If a standard is not available, the testing must be done in comparison with very accu- rate specific-gravity determinations, made by a balance. If the instrument tested is a specific-gravity hydrometer, the balance determinations are of course directly compared with its readings ; if it is a Brix or a Baume spindle, the corresponding specific-gravity values can be ascertained from Table I. Methods of Testing 1 Hydrometers. METHOD I. The balance determinations are made by weighing first a specific-gravity fiask or pyknometer,* perfectly clean and dry. The flask is then filled with distilled water at the temperature at which the hydrometer was graduated. This had best be 17. 5 C., and if the hydrometers are made to order, this temperature should be insisted on for the graduation. The weight of the flask filled with water up to the mark is next taken. A solution is then prepared by dis- * The neck where the mar is placed, should be narrow, and the flask should have a tightly-fitting stopper to prevent loss by evaporation. 16 SUGAR ANALYSIS. 1 1 solving pure sugar in water. The density of this solu- tion is such that it corresponds approximately to one of the points marked on the scale of the hydrometer which is being tested. The temperature of the solution is made to correspond exactly with the temperature at which the specific-gravity flask was previously filled, and the weight of this flask now filled with the sugar solution is accurate- ly determined. Subtracting the weight of the flask from these two weighings gives respectively the weight of equal volumes of water and of sugar solution. Dividing the latter value by the former, gives the specific gravity of the sugar solution. Example. Weight of specific-gravity flask + water, 40.0403 u u u * 15.0811 Weight of water in flask, 24.9592 Weight of specific-gravity flask + sugar solution, 42.5810 " " " " " " 15.0811 Weight of sugar solution in flask, 27.4999 27.4999 -f- 24.9592 = 1.1018 Specific gravity of sugar solution = 1.1018 Some of the sugar solution is poured into a glass cylinder, the temperature carefully brought to 17. 5 C., and the hydrometer, perfectly clean and dry, inserted. It should be allowed to glide down slowly into the solu- tion in order that no more of the stem shall be immersed than necessary. Care must also be taken that the instru- ment floats free, that is, does not come into contact with the sides. SUGAR ANALYSIS. 17 When the hydrometer has come to rest, a reading of the scale is made and compared with the specific gravity obtained by the balance. The indications of specific- gravity hydrometers should of course agree exactly with the balance determinations ; for Brix and for Baume in- struments the limit of agreement should be placed at 0.15. The cheaper Baume hydrometers, ranging from to 50, will, however, rarely agree closer than 0.25, and this degree of accuracy will suffice for the practical working purposes of the refinery. METHOD IL If the hydrometer is a specific-gravity hydrometer of limited range, it may be tested by immer- sion in solutions of chemically pure sugar ; these solutions are prepared as follows : * Sp. Gravity. 1.095 Grammes C. P. Sugar. 22.6 Grammes distilled Water at 17.5 C. 77.4 1.097 23.0 77.0 1.100 23.7 76.3 1.103 24.3 75.7 1.106 25.0 75.0 METHOD III. If a balance is not available, the test- ing of specific-gravity hydrometers may be accomplished by the aid of a polariscope. This method is also applica- ble to Brix and to Baume hydrometers if their degrees are translated into the corresponding specific-gravity values. Prepare pure sugar by washing best granulated or powdered block-sugar repeatedly with an 85 per cent alcohol. The washing should be done with a volume of alcohol equal to from three to five times the volume of * Based on the table given in Stammer's Lehrbuch der Zuckerfabrika- tion, 3d edition, p. 26 et seq. 18 SUGAR ANALYSIS. the sugar. The washed sugar must then be perfectly dried at the temperature of about 100 C., and kept in an air-tight jar. A solution of this sugar is made, the tem- perature taken, and the hydrometer inserted in it with all the care and precautions previously referred to. After the reading of the hydrometer has been noted, the solu- tion is polarized, and the polarization is multiplied by the factor (Table IV) corresponding to the specific gravity of the solution, corrected, if necessary, for temperature (Table II). If the hydrometer is correct (of course a correct polariscope is premised), the result of the multi- plication of the polarization by the factor must be 100. Example. Specific gravity of solution corrected for temperature, 1.096 Factor, 1.042 Polarization, ........ 96.0 96.0 X 1.042 = 100.0. Graduation of Flasks. T wo methods are used. The first, the scientifically correct one, is to graduate in true cubic centimetres. A true cubic centimetre represents the space occupied by 1 gramme of water weighed in vacuo at a temperature of 4 C. The second method, known as Mohr's, omits the reduction to volume at 4 C. and to weight in vacuo. METHOD I. To graduate a flask at any given tem- perature, ascertain from Table XVII the weight of 1 cubic centimetre of water, at that temperature. Then correct for weighing in air, that is to say, reduce the weighing in air to weighing in vacuo by assuming each gramme of water weighed in air to be 1 milligramme too SUGAR ANALYSIS. 19 light. * Tare the flask accurately, place the correct weights on one scale-pan, and weigh the corresponding weight of water into the flask. Example. To graduate a flask to hold exactly 100 cubic centimetres at 15 C. Table XVII shows that 1 cubic centimetre of water at 15 C. weighs 0.99916 grammes. Hence 100 X 0.99916 = 99.916 grammes. As the weighing is to be made in air, to reduce to weighing in vacuo, 99.916 X 0.001 = 0.099916 must be subtracted from the former figure : 99.916000 0.099916 99.816084 Therefore 99.8161 grammes of water at the tempera- ture of 15 C. must be weighed into the flask. METHOD II. The required number of grammes of water (at the temperature chosen) corresponding to the desired volume in cubic centimetres are weighed into the flask, and the resulting volume marked on the flask. These " cubic centimetres" are of course larger than the true cubic centimetres. Example. To graduate a flask to hold 50 cubic centi- metres at 15 C., 50 grammes of water at 15 C. are weighed into the flask, and the volume occupied is marked as 50 c.c. Verification of Graduated Glass Vessels, in true Cubic Centimetres Fill to the mark with distilled water of * This presupposes the use of brass weights. If the weight of water exceeds 100 grammes, 1.06 milligrammes instead of 1.00 milligramme must be taken in above calculation. 20 SUGAR ANALYSIS. the temperature at which the vessel was graduated, and weigh. Add to this weight 1 milligramme for each gramme of water weighed. The density of the water at the temperature of the experiment is to be found in Table XVII. If P = Corrected weight of the water, Q = Density of water at temperature of the ex- periment relative to water at 4 C., t = Temperature of the water in the experiment ; then the volume in cubic centimetres contained in the vessel at the temperature t is . A flask holds 50.072 grammes of water at 15 C. The weight in vacuo will be 50.072 + 0.050 50.122 grammes, and the capacity at 15 C. will be 50 122 = 50.16 cubic centimetres. 0.99916 Thermometers. The thermometers should be, if pos- sible, compared with some standard instrument. This applies especially to the thermometer which is to be used to determine the temperature while ascertaining the polarization of inverted sugar solutions. It will answer to verify, on Centigrade thermometers intended for ordinary use, the zero and the 100 mark; on a Fah- SUGAR ANALYSIS. 21 renlieit instrument, the 32 and the 212 mark; and to see that the degrees are of equal size. The zero-mark on the Centigrade scale (32 Fahren- heit) is ascertained by placing the bulb and part of the stem in snow or pounded ice for about a quarter of an hour. The vessel in which the snow or ice is placed should be provided with a small opening at the bottom, through which the water is drained off as it is formed. To obtain the 100 C. (212 F.) mark, the thermo- meter is suspended in the vapor of boiling water, care being taken that it does not dip into the water. The pressure of the atmosphere should be 760 mm. at the time ; if not, a correction for the variation must be made. The reading of one scale can be translated into that of the other by the following formulae : 6-5(^-32) For a comparison of the different thermometric scales see Table XVIII. Balances. For weighing out samples for polariza- tion, a balance capable of weighing up to 300 grammes and sensible to 1 milligramme will answer. For water and ash determinations an analytical balance should be used ; this should be sensible to 0.1 of a milligramme, and be capable of bearing a charge up to 200 grammes. A good balance* should give the same result in suc- cessive weighings of the same body ; the two halves of * See Deschanel-Everett : Natural Philosophy. 22 SUGAR ANALYSIS. the beam should be of equal length ; it should be sensible to a small load, and it should work quickly. It is an easy matter to determine whether a balance possesses these properties. Repeated weighings of the same load will quickly establish whether the balance is consistent with itself; this depends principally on the trueness of its knife-edges. To determine whether both halves of the beam are of the same length, the two pans should be loaded with equal weights. If the arms are of unequal length, the pan attached to the longer arm will descend. To test the sensibility, load both pans with the maxi- mum weight which they are intended to bear, and then add to one of the pans the weight to the extent of which the balance is supposed to be sensible. The addition of this slight extra weight should cause the pan on which it has been placed, to descend. Weights. The weights used, both the regular weights for analytical purposes, and the so-called sugar- weights (normal and half normal), should be verified from time to time, as they will in daily use unavoidably suffer some wear and tear. Most of the weights are so made that the plug or stopper unscrews from the body of the weight, and slight deficiencies in weight can readily be corrected by inserting tin-foil or small shot into the cavity after removing the plug. Should the weights be too heavy, a little filing will readily remedy the evil. CHAPTER II. SAMPLING DETERMINATION OF : COLOR DENSITY ALKA- LINITY ACIDITY SULPHUROUS OXIDE. Sampling- Sugars and Molasses. Too much impor- tance cannot be attached to the securing of correct sam- ples, that is to say, to the obtainment of samples which shall be representative of the substance examined. The samples of raw sugar are drawn with a long steel bar resembling the half of a pipe cut longitudinally. A hole having been made in the package, the "tryer," as it is called, is inserted, rotated completely, and then withdrawn. The sample which fills the hollow in the tryer is removed and is placed in a can. When syrups or molasses are to be sampled, a rod or a stick is inserted in the bung-hole of the barrel and rapidly withdrawn ; the adhering liquid is placed in a can, and the operation repeated until sufficient has been obtained. When sugars in hogsheads are sampled, the hogs- head is placed on its side. The manner of inserting the tryer differs. The Government takes its sample by run- ning straight through the contents from centre to centre of the heads ; at some refineries the tryer is run through diagonally from head to head. Melados are sampled through the bunghole of the hogshead. In a refinery, 100 per cent of all sugars, syrups, and molasses are sampled. 23 24 SUGAR ANALYSIS. The U. S. Government varies its requirements as to the number of packages to be sampled, with the nature of the package : Of hogsheads, tierces, boxes, and barrels, 25 per cent are required for sample and 100 per cent for a resample ; of centrifugals and of beet-sugars, in bags, 5 per cent for sample and 5 per cent for resample ; of mats, 2-| per cent for sample and 2^ per cent for resample ; of baskets, 10 per cent for sample and 10 per cent for resample ; of "Jaggeries," Pernambuco, and Brazil sugars, 5 per cent for sample and 5 per cent for resample. When the samples have been taken and are brought to the laboratory for analysis, it is necessary, either to make a separate analysis of every mark in a lot, or, as this is generally not feasible, to prepare a representative sam- ple. In order to do this, fix upon some definite quantity by weight as the unit weight. Weigh out this amount, pi'o v portionate to the number of hogsheads in each mark, and place in a well-closed jar. For example, suppose a lot of sugar contained four marks, A, B, C, and D. Mark A = 1000 hogsheads, " B= 200 " C = 350 D = Vo " Then take from : A = 100 grammes B = 20 " C = 35 D= 7 SUGAR ANALYSIS. 25 For analysis, if necessary, crush the sample, thoroughly mix the contents of the jar, and then proceed as usual. As some lots come in mixed packages, that is to say, partially in hogsheads, bags, tierces, and barrels, a certain relation between these has been assumed ; it is as fol- lows : 1 hogshead = 2 tierces. " =8 barrels. " =8 bags. To prepare average samples of refined sugars, proceed in' a similar manner, as directed above. Determination of Color of Sugar and Sugar Solu- tions. The color-tests made on sugars and on sugar solutions are generally only comparative, that is to say, the color of the sample examined is compared with that of some other sample which is taken as the standard. In the examination for color of raw sugar, the so-called "Dutch standards" are usually employed. These consist in fifteen samples of raw sugar, numbered from No. 6 to No. 20, and ranging in color from a dark-brown (No. 6) to almost a white (No. 20). They are prepared and sealed with great care by a certain firm in Holland. The samples are renewed every year, and serve as standards for the twelve months following their issue. In examining the color of sugar solutions, to learn, for instance, how effectively a certain sugar has been decolorized in passing through bone-black, two test-tubes, beakers, or cylinders made of white glass, are filled to an equal height with, respectively, the sample under exami- nation and the "standard" solution with which the sam- 26 SUGAR ANALYSIS. pie is to be compared, both solutions of course being of equal density. Various forms of apparatus have been designed for effecting color comparison. In some, the " standard " solu- tion is replaced by colored-glass disks of tints ranging from a pure white to a dark yellow or brown; by com- bination of these it is possible to produce almost any shade desired. The colorimeter probably most used is that of Stammer. As the depth of color of a solution is proportional to the length of a column of such solution, there is ascertained in this instrument the height of a column of the solution which will in color correspond to the tint of a " standard " colored-glass disk inserted in an adjoining tube. The scale is graduated in millimetres. If, for instance, a depth of one millimetre of the solution corresponds to the nor- mal tint, the color is said to be 100. If two millimetres depth of solution are required to match the tint, the color is 50 ; if four millimetres, 25 ; and so on. Determination of the Density of Solutions. j&y the Specific-gravity fflask. The most accurate way to de- termine the density (specific gravity) of a solution is by means of a specific-gravity flask (pyknometer) and a delicate balance, as already described on page 15. The weight of the flask, empty and dry, having been ascer- tained, and the weight of distilled water which it will hold at 4 C. or at the temperature at which it was graduated being known, once for all, it is only necessary to fill the clean and dry flask exactly up to the mark with the solution whose specific gravity is to be deter- mined. If the solution has not been brought to the tem- perature at which the flask was graduated, before the flask SUGAR ANALYSIS. 27 is filled with it, this must certainly be done before the weighing is made, in order that the weight of equal vol- umes of the water and the solution may be obtained. The flask filled with the solution is weighed, the weight of the flask subtracted from this figure, and the remainder divided by the weight of the correspond- ing volume of water. The result is the specific gravity of the solution. By Pipette and Beaker. An adaptation of the method just described, and which is convenient for rapid work- ing, is the following : A pipette capable of holding a certain volume, say 10 or 20 c.c., is placed in a glass beaker; both pipette and beaker of course must be perfectly clean and dry. The combined weight of the two is taken and noted. The pipette is then filled with distilled water at the temperature which is to be made the normal temperature, preferably 17.5 C. The pipette is replaced in the beaker, and the combined weight of the pipette, beaker, and water is determined. The vessels having been again cleaned and dried, the solution whose specific gravity is to be determined, is brought to the standard temperature, and the pipette filled with it up to the mark. The weight of pipette, beaker, and solution is then deter- mined. The calculation to be made is exactly as before explained, the combined weight of beaker and pipette taking the place of the weight of the pyknometer in the previous method. By Hydrometers. The hydrometer selected for mak- ing the determination may be a specific-gravity hydrome- ter or an instrument graduated according to an arbitrary scale (Brix, Baume). 28 SUGAR ANALYSIS. Whenever a solution is to be tested, care must be taken to have it as free of air-bubbles as possible. If the solu- tion whose density is to be determined is a thick syrup or a molasses, it had best be poured into a vessel provided at the bottom with a stop-cock. This vessel may advan- tageously be enclosed in a water-jacket. This can be heated and the molasses thus readily warmed, which will greatly hasten and facilitate the rising of the air-bubbles. When they have all risen to the top, the liquid is drawn off from below, without disturbing the frothy layer on the surface. The liquid is placed into a glass cylinder, which must stand perfectly level, and the hydrometer is carefully and slowly inserted. It must float free in the liquid, that is, it must not be permitted to touch the sides of the cylinder. When the hydrometer has come to rest, the point up to which it is immersed in the solution is read and recorded. The temperature of the solution is determined, and if not of the standard temperature, a correction therefor must be made. (See Table II or III). The readings of the specific-gravity, the Brix, and the Baume hydrometers can each readily be translated into the terms of the others by Table I. By Glass Spheres. For approximate density deter- mination small glass balls of different weights are some- times used. A number engraved or etched on each, desig- nates the density of a liquid in which it will float. Beginning with the heavier, the balls are succes- sively thrown into the solution whose density is to be de- termined, until a ball is found which w r ill float in the liquid tested. The number engraved on this ball indicates SUGAR ANALYSIS. 29 the density of the solution. Of course regard must here also be had to the temperature of the liquid. By Mollys Hydrostatic Balance. From one end of the beam of this balance a glass bob, preferably one pro- vided with an accurate thermometer, is suspended by a fine platinum wire. The other end of the beam is pro- vided with a counterpoise to the bob ; this counterpoise terminates in a fine metal point, and serves as the tongue of the balance. It shows the beam to be in equilibrium when, the same remains at rest in a horizontal position directly opposite to a fixed metal point. The balance, when correctly adjusted, is in perfect equi- librium when the glass bob hangs freely suspended in air. That part of the beam between the fulcrum and the end from which the bob is pendant, is provided with nine graduations, numbered from one to nine. Accompanying the balance are five weights or riders. The largest two are each equal to that weight of distilled water (at a cer- tain temperature, usually 15 C. or 17.5 C.), which the glass bob displaces when it is immersed. The other three riders weigh respectively one tenth, one hundredth, and one thousandth as much as the large rider. When the bob is immersed in water, one of the large riders must be placed at that end of the beam from which the bob is suspended. This will restore the equilibrium, and the balance then indicates the specific gravity 1.000. If the bob is immersed in a liquid heavier than water, this liquid having been brought to the temperature for which the balance was graduated, some of the other riders also must be placed on the beam in order to restore the equilibrium. The position of these riders indicates the specific gravity of the solution, each rider according 30 SUGAR ANALYSIS. to its weight, representing respectively as many tenths, hundredths, or thousandths as is expressed by the num- bered division on the beam where it is placed. Determination of Alkalinity. The alkalinity of the different products of a refinery may be caused by potas- sium, by sodium, by lime, or even partially by free am- monia. It has, however, become customary to report the alkalinity in terms of calcium oxide (caustic lime). Alkalinity is determined by the addition of an acid of known strength to a known weight or volume of the product examined, until neutrality has been established. The acid used may be either sulphuric, nitric, or hy- drochloric acid, the first of these being the one most com- monly employed. As indicator, litmus solution, phenol- phthalein, or rosolic acid (corallin) is available. Litmus turns red with free acid, while phenol-phthal- ein is colorless, and rosolic acid * is colorless or shows a pale yellow color with free acid. The indications afforded by these agents are said to be not identical, and any set of comparative determinations therefore should be carried out with the same indicator, whichever of these may be selected. The acid used is generally of " tenth-normal " strength. To prepare this there are needed of : Sulphuric oxide 4.00 grammes SO 3 in 1 litre of water. Hydrochloric acid 3.637 " HC1 " " " " Nitric acid 6.289 HNO 3 " " " " The acid should be delivered from a burette divided into tenths of a cubic centimetre.'' To effect an alkalinity determination, 10 to 20 * Use alcohol for dissolving. Of phenol-phthalein, 1 part in 500 parts of alcohol; of rosolic acid, use 1 part in 100 parts of alcohol of 90. SUGAR ANALYSIS. 31 grammes of the product to be tested are weighed out and dissolved, or, if a solution is to be examined, from 10 to 20 cubic centimetres are measured out anc 1 placed in a porcelain dish. A few drops of the indicator having been added, the acid is allowed to flow in from a burette until the change in color of the indicator shows the reaction to be finished. 1 cubic centimetre of ^ (tenth normal) sulphuric acid corresponds to 0.0040 gramme sulphuric oxide, 0.0028 gramme calcium oxide, or 0.0047 gramme potassium oxide. The number of cubic centimetres of acid used, multi- plied by 0.0028, show therefore the amount of calcium oxide present. Example. 25 cubic centimetres of a sugar solution (specific gravity 1.198) required 2.4 cubic centimetres YQ sulphuric acid to effect neutralization. This repre- sents 0.0028 X 2.4 = 0.00672 gramme calcium oxide. ' 25.0 : 0.00672 : : 100 : x. x= 0.02688 per cent calcium oxide. This is per- centage l>y volume. If percentage by weight is required, the above value must be divided by the specific gravity of the solution, or if a specific-gravity determination and this subsequent calculation are to be avoided, the solution to be tested must be in the first place weighed out, and not measured. Determination of Acidity To determine the acidity of a solution, syrup, molasses, etc., the same course is fol- lowed as above described, only of course the solution added to effect neutralization is one of sodium hy- drate (caustic soda), potassium hydrate (caustic potash), or calcium hydrate (slaked lime), and the change of 32 SUGAR ANALYSIS. color of the indicator, if litmus, must be from red to blue, or if phenol-phthalein or rosolic acid are employed, from colorless to a bright crimson. Of these solutions the cal- cium hydrate is least desirable, as the carbonic acid of the atmosphere readily precipitates in it calcium carbonate, and so changes the strength of the solution. A ^ sodium- hydrate solution contains 3.996 grammes NaOH in 1 litre of water. Test for Sulphurous Oxide in Sugar Dissolve from 10 to 20 grammes of the sugar in about 25 cubic centi- metres of distilled water. Pour into a flask, and add about 5 grammes of chemically pure zinc (free from sulphur), and 5 cubic centimetres of chemically pure hy- drochloric acid. Suspend a paper moistened with acetate of lead solution in the neck of the flask. If sulphur dioxide is present, it will be liberated from its combina- tions and changed into sulphuretted hydrogen, and this gas will turn the acetate of lead on the paper a brown or a black color, owing to the formation of sulphide of lead. CHAPTER III. SUCROSE : IN THE ABSENCE OF OTHER OPTICALLY ACTIVE SUBSTANCES. Optical Analysis METHOD I. With Balance. Weigh out 26.048 grammes of the sample.* Dissolve in 50 to 75 c.c. of water, and pour into a 100 c.c. flask. Add basic acetate of lead solution, f the amount depending on the nature of the sugar tested, and then add a few drops of a solution of sodium sulphate to insure the precipitation of any excess of the lead salt. J Filter rapidly into a covered beaker to avoid concen- tration of solution by evaporation ; rejecting the first few drops entirely, fill the 200 mm. polarization-tube, and take the reading. Several readings should be taken on the same solution, and their mean recorded. * The sample must previously have been well mixed; if the sugar, as is frequently the case, contains lumps, the whole sample must be thoroughly crushed before the mixing. In cold weather sample-cans brought in from out-of-doors, should be allowed to stand in the laboratory until their contents shall have approx- imately attained the temperature of the room. This is done in order to avoid condensation of moisture on the cold sugar, as this would slightly lower the polarization. t Basic Acetate of Lead. To 300 grammes acetate of lead and 100 grammes litharge (oxide of lead) add 1 litre of water. Allow to stand for twelve hours in a warm place, with occasional stirring; then filter, and preserve in a well-closed bottle. The basic acetate of lead must show a strongly alkaline reaction, and have a specific gravity ranging from 1.20 to 1.25 at a temperature of 17.5 C. | It is impossible to prescribe the quantity of the basic acetate of lead solution to be used; always, however, employ the least amount that will produce the desired effect, tor a voluminous precipitate causes an error in polarization. 34 SUGAR ANALYSIS. With very dark sugars and with syrups, the half- normal weight, 13.024 grammes, is often taken, dissolved up to 100 c.c., and the reading made in a 200 mm. tube; or the normal weight is used, and the reading effected in the 100 ruin. tube. It must be remembered that the temperature exerts an influence on the polarization reading. The colder the solution the higher the reading; a variation in temper- ature of two degrees Centigrade,* is stated to cause a dif- ference of one tenth of a degree on the polariscope. Decolorization of dark solutions is effected by add- ing to the solution some bone-black dust previously pre- pared^ by use of the so-called Gawalowsky'sdecolorizer, or by " blood carbon." Whichever of these is employed, the least amount possible should be used. For very dark sugars and molasses the use of sodium sulphite (a 10 per cent solution) and basic acetate of lead is recommended. J The sodium sulphite is first in- troduced, about 2 c.c., and then the basic acetate of lead solution is gradually added with constant shaking, till no further precipitation occurs. If necessary, the filtrate from this can be subjected to the action of sul- phurous acid and bone-black. Opalescence or a slight but persistent turbidity of the solution to be polarized, can be overcome by the addition of a little " alumina cream." Three to five cubic centi- * Die Deutsche Zuckerindustrie, vol. xiv. p. 503. t Warm for several hours with hydrochloric acid to dissolve the phos- phate and carbonate of lime; then wash with boiling water till all traces of chlorine are removed ; dry at about 125 C., and keep in a well-closed jar. { Allen : Commercial Organic Analysis, vol. i. p. 201. | Precipitate a solution of alum, not too concentrated, by ammonic hydrate. Wash the precipitate until all the salts have been removed, and the washings no longer tarn red litmus blue. SUGAR ANALYSIS. 35 metres are ample, if not more than the half -normal weight has been used for making the solution. This reagent is of little value as a decolorizer, but very efficient with high- grade sugars that show the troublesome opalescence. The saccharimeters now in universal use record the amount of sucrose in per cent, provided the normal weight* of the sample has been used, and the reading has been effected in a 200 mm. tube; if a 100 mm. tube has been used, the reading must be doubled ; or if the half -normal weight has been taken, and the polarization has been effected in a 200 mm. tube, the reading must of course also be doubled. / o If for any reason the normal or the half -normal weight has not been taken, a simple calculation will serve to fig- ure the percentage of sucrose in the sample. Suppose, for instance, that 9.000 grammes had been weighed for po- larization and that these were dissolved up to 50 c.c. A polarization of this solution in a 200 mm. tube = 62.00. As a rotation of one degree represents 0.13024 gramme sucrose, there are contained in the sample 0.13024 X 62 = 8.07488 grammes pure sucrose. Hence 9.00000 : 8.07488 : : 100 : x. x= 89.72. Therefore the sample contains 89.72 per cent sucrose. A more direct way of figuring this is by means of the formula : PxW' rpr = per cent sucrose. P polarization of the solution ; W f = normal or half -normal weight of the instrument used; W = weight of substance taken for polarization. * The normal weight for the German instruments is 26.048 grammes; for the Duboscq polariseopes it is 16.192 grammes. 36 SUGAR ANALYSIS. 62.0 X 13.024 Example. -=89.72. Results so obtained can be verified by calculating the amount of sugar which would be necessary in order to indicate 100 degrees on the polariscope. This is known as Scheibler's method of " One hundred polarization." Example. In the case just discussed, a polarization of 89.7 required 13.024 grammes of the sugar: how much will be required to produce a rotation of 100 degrees on the instrument ? 89.7 : 13.024 : : 100 : x. x = 14.5195. Therefore 14.5195 grammes of this sample are polar- ized in the usual manner, and if they indicate 100 per cent, the result previously obtained, is correct. Table VII, by Scheibler, obviates the necessity of this calculation, showing at once the amount that must be used. METHOD II. Without Balance. The percentage of sucrose in a sample can also be obtained without mak- ing a weighing. A solution is made and the specific gravity of the solution is determined, either directly by a specific-gravity hydrometer, or else by some other hydrome- ter (Brix, Baurne), the readings of which are translated into the corresponding specific gravity (Table I). The polarization of the solution is then made, and the percentage of sucrose calculated by the formula : P X .2605 in which S = percentage of sucrose, P polarization of the solution, D specific gravity. If the solution needs clarifying, it is placed into a SUGAR ANALYSIS. 37 graduated flask, the amount of basic acetate of lead solu- tion that is added, is noted, and the reading increased in proportion. Example. Specific gravity of solution, 1.0909 ; Polarization of solution = 35.0. To 100 c.c. of solution added 5 c.c. basic acetate of lead solution ; this corresponds to 5 per cent of 35.0 = 1.75. Hence corrected polarization = 36.75 per cent. 36.75 X .2605 ~ '" 3er cent sucrose - This calculation can be avoided by consulting Table VI. This table is used in the following manner : Example. Corrected specific gravity = 1.0339 ; Polarization =25.0. In a line with the specific gravity 1.0339, and in the horizontal column marked 2, is found the number .504 This multiplied by 10 = 5.040. In a line with the specific gravity 1.0339, and in the column marked 5, is found the number 1.260. Adding these values, 5.040 1.260 Percentage of sucrose = 6.300 The simple polarization of a sugar, syrup, liquor, magma, or sweet-water shows the percentage of sucrose in the sample as it is. Sometimes, however, it is necessary to know what this percentage would be if the water in the sample were removed ; in other words, it may be de- sirable to ascertain the percentage of sucrose in the " dry substance." 38 SUGAR ANALYSIS. The percentage of pure sugar in the " dry substance"" is referred to as : The Quotient of Purity, or Exponent. There are several ways of determining this. The most accurate method undoubtedly, but also the one demanding most time, is the following : METHOD I. Determine polarization of the normal weight of the sample as previously described (p. 33). De- termine the percentage of water by drying to constant weight (see p. 76). Subtract the percentage of water from 100, and divide the remainder into the polarization multi- plied by 100. Example. Polarization of syrup, 33.00 ; Water in syrup, per cent, 24.16. 100.00 24.16 3300 -i- 75.84 = 43.5 75.84 Polarization on dry substance = 43.5. METHOD II. Determine polarization of the normal weight of the sample as previously described (p. 33). De- termine the degree Brix of the sample. Correct for tem- perature (Table III). Calculate polarization on the dry substance by the Pol. X 100 iormula : =pr ^ . . Degree Brix Example. Polarization, 40.00 ; Density, 50 Brix at 24 C. ; Correction for temperature, + 0.49 Degree Brix corrected for temperature, = 50.49. SUGAR ANALYSIS. 39 100.00 -4- 50.49 = 1.9806, factor ; 40.00 X 1.9806 = 79.22, polarization on the dry sub- stance, or coefficient of purity. METHOD III. Ventzke's Method. Prepare a solution of the sugar which shall have the specific gravity 1.100 at 17.5 C. Take the reading of this solution in a 200 mm. tube. This polariscope reading shows at once the percentage of pure sugar in the dry substance. This is the case, because a solution made by dissolving 26.048 grammes of chemically pure sugar in water up to 100 c.c. has the specific gravity of 1.1000 at the temperature of 17.5 C., and a column of this solution 200 mm. in length, indicates 100 per cent in the German polariscopes. The following table prepared by Gerlach* shows the specific gravity of the above solution at the temperatures given : Temper- ature. C. Specific Gravity. Temper- ature. C. Specific Gravity. Temper- ature. o C Specific Gravity. \ 10324 I6. 5 I . 10028 23 1.09834 5 . 10266 17 .10014 24 1.09802 10 .10192 17-5 .10000 25 .09770 ii .10168 18 .09986 26 .09736 12 .10144 18.5 .09972 27 .09702 13 .10119 IQ 09957 28 .09669 14 . 10095 19-5 .09943 29 09635 15 .10071 20 .09929 30 .09601 15-5 10057 21 .09897 16 . 10043 22 .09865 As the preparation of a solution which is to have * Jahresbericht iiber die Untersuchlingen und Fortschritte auf dem Gesammtgebiete der Zuckerfabrikation, 1863, p. 234. 40 SUGAR ANALYSIS. a certain specific gravity at a certain temperature is apt to prove a tedious operation, the following modification of Ventzke's method will prove serviceable : If the temperature at which the solution is prepared is not the normal temperature, a correction must be made (Table. II). This correction must be subtracted from the reading of the specific-gravity hydrometer if the temperature is lower than the normal, and added, if it is above-the nor- mal temperature. The polarization obtained in the 200 mm. tube must then be multiplied by the factor corresponding to the corrected specific gravity (Table IV). METHOD IV. Oasamajor's Method. Determine the specific gravity or the degree Brix of the solution. Cor- rect for temperature if necessary (Table III). Determine the polarization of this solution and multiply the polariza- tion by the factor corresponding to the degree Brix (Table V). Example. Polarization of solution 61.2 ; Brix, = 15.5 at 22 C.; Correction for temperature, +0.31 Corrected degree Brix = 15.81 ; Factor corresponding to 15.8 Brix is 1.548 61.2 X 1.548 = 94.74, which is the polarization on the dry substance, the coefficient of purity. The quotient of purity obtained by Method I (where the percentage of water is obtained by actual drying out), is called the "true" quotient of purity; if hydrometers are resorted to, as in Methods II, III, and IV, the resulting coefficient is called the " apparent " quotient of purity. If a syrup or a molasses has been analyzed, the re- SUGAR ANALYSIS. 41 suits of the analysis can easily be calculated into equiva- lents on the dry substance in the following manner: The reciprocal of the degree Brix (that is, the quo- tient obtained by dividing 1 00 by the degree Brix), gives a factor by which the percentage of sugar, invert sugar, and ash must be multiplied in order to reduce them to the basis of dry substance. Example. A syrup of 80. 4 Brix shows on analysis : Polarization, 31.2 ; Invert sugar, 12.5 ; Ash, 6.0. 100 -*- 80.4 = 1.2437. On Dry Substance. Hence : Polarization, 31.2 X 1.2437 = 38.80 per cent. Invert-sugar, 12.5 X 1.2437 = 15.55 " Ash, 6.0 X 1.2437 = 7.46 " Non-ascertained (by difference) = 38.19 " 100.00 per cent. If sucrose has to be determined in a molasses, a syrup, or in sweet- water, the calculation of the result to dry sub- stance can be avoided by aid of Table VIII. This table has been calculated for use with the Ger- man polariscopes (normal weight 26.048 grammes). It presupposes the addition of 10 per cent by volume of basic acetate of lead to the sucrose solution examined, and in its preparation the variable specific rotatory power of sucrose has also been taken into account. The use of the table is very simple. Example. Density of a sugar solution, 22.0 Brix. Polarization (after using 10 per cent by volume of basic acetate of lead solution for clarifying), 60.3. In column headed 22.0 Brix, and opposite to the 42 SUGAR ANALYSIS. number 60 in the column headed "Polariscope degrees," we find 15.72 per cent sucrose. Then turning on the same page to the division for tenths of a degree, in the section headed " Percent Brixfrom 11.5 to 22.5," there is given opposite to 0.3 Brix the value 0.08 per cent sucrose. Hence 60.0 = 15.72 per cent. 0.3 = 0.08 * 60. 3 = 15.80 per cent sucrose. Gravimetric Analysis. Weigh out 13.024 grammes of the sample. Dissolve with about 75 c.c. of water in a 100 c.c. flask. Add 5 c.c. hydrochloric acid containing 38 per cent HC1 (sp. gr. 1.188). Heat quickly, in two or three minutes, on a water-bath up to between 67 and 70 C. Then keep at this temperature (as close to 69 C. as pos- sible) for five minutes, with constant agitation. Cool quickly; make up to 100 c.c. Remove 50 c.c. by a pipette, place in a litre flask, and fill up to 1000 c.c. Of this so- lution take 25 c.c. (corresponding to 0.1628 gramme of sample), neutralize all free acid present by about 25 c.c. of a solution of sodium carbonate prepared by dissolving 1.7 grammes crystallized sodium carbonate in 1000 c.c. of water. Then add 50 c.c. of Fehling's solution, heat to boiling as directed in invert-sugar determination, boil for three minutes, and proceed as directed on page 69. Calculation. In Table XI seek the number of milli- grammes of copper which agree most closely with the amount of copper found. The corresponding number in the column to the left, shows at once the number of milligrammes of sucrose. Example. 25 c.c. of the inverted solution = 0.1628 gramme of sample, yielded 0.1628 gramme copper. SUGAR ANALYSIS. 43 This corresponds to 0.082 gramme sucrose ; hence there are present in the sample 50.4 per cent sucrose. As invert-,sugar, dextrose, and even raffiinose (after inversion by acid), reduce Fehling's solution, a correction of the results yielded by this method must be made, whenever appreciable quantities of the substances named are present. If the sample analyzed contains invert-sugar, the amount of this substance multiplied by 0.95 must be sub- tracted from the " Total sucrose " found, in order to ob- tain the actual amount of sucrose present. This factor 0.95 is used, because sucrose on inversion yields invert- ugar in the proportion of 100 : 95. CHAPTER IV. SUCROSE: IN THE PRESENCE OF OTHER OPTICALLY ACTIVE SUBSTANCES. THE determination of sucrose can be effected by means of the polariscope, as described in the previous chapter, provided no other optically active bodies are present. Such substances, however, occur frequently ; they may be dextro- or laevo-rotatory. If the presence of such sub- stances is suspected, it will be necessary to perform an- inversion by acid, and determine the polarization of the inverted solution. If no other optically active substances are present besides the sucrose, the polarization before and after in- version will be equal. If the polarization after inversion is higher than the polarization before inversion, laevo-rotatory bodies are present ; if the polarization after inversion is lower than the polarization before inversion, dextro-rotatory sub- stances are indicated. In the former case invert-sugar, laevulose, etc., must be considered ; in the latter, dextrose, raffinose, etc., will have to be looked for. Clerget's Inversion Method Weigh out 26.048 grammes of the sample, and determine the polarization. Of the filtrate, take 50 c.c. for inversion, or weigh out sep- arately 13.024 grammes of the sample.* Dissolve with about 75 c.c. of water in a 100 c.c. flask ; add, while agi- * Herzfeld's modification. Zeitschrift 'des Vereines fur Eiibenzucker- Industrie, 1888, p. 709. SUGAR ANALYSIS. 45 tating the solution, 5 c.c. hydrocliloric acid (sp. gr. 1.188), containing 38 per cent HC1. Heat quickly, in two or three minutes, on a water-bath up to between 67 and 70 C. Then keep the temperature of the solution for five minutes as close to 69 C. as possible. Agitate con- stantly. Then cool quickly, fill with distilled water up to the 100 c.c. mark, and polarize in a tube provided with an accurate thermometer.* The temperature at which the reading is taken should be 20 C. For dark solutions, molasses, etc., take 26.048 grammes of the sample, dissolve, add basic acetate of lead and sodium sulphate, and fill up to 100 c.c. Filter. Of the filtrate remove 50 c.c. with a pipette, place in a 100 c.c. flask, add 25 c.c. of water, and 5 c.c. of hydrochloric acid containing 38 per cent HC1, and proceed as directed above. The result is calculated by means of the formula : IQOff z 142.66- \t R = sucrose ; S sum of the two polarizations before and after inversion, the minus sign being neglected ; t = temperature in degrees Centigrade at which the polariza- tion after inversion is observed. Example. Polarization of normal weight before in- version, 87.5 ; Polarization of half-normal weight after inversion, - 14.3 at 20 C. - 14.3 x 2 87.5 28.6 100 X 116.1 -28.6 142.66 -- 10 11610- /.* o ^7 pr 116.1 '132.66 ';? * Thermometers constructed expressly for this purpose, and on which the degrees are divided into tenths, are made by C. Haack in *Tena, Germany. 46 SUGAR ANALYSIS. It is best to carry out the determination at 20 C. if possible. If, however, the determination is made at any other temperature from 10 C. to 30 C., Table X gives a series of factors by which it is necessary to multiply the difference of the indications, before and after inver- sion. Of course the factor corresponding to the temper- ature at which the reading of the inverted solution was made, must be used. Example. Direct polarization, 86.0 ; Polarization after inversion, 25.0, at a temperature of 22 C. 86.0 + 25.0 = 111.0. Referring to Table X, opposite to 22 C. there will be found the factor 0.7595. Multiplying 111 X .7595 = 84.3; this is the desired result. If any other weight than 13.024 grammes is used for the determination, the formula JS -77 -- r does not give quite correct results, because the specific rotatory power of an invert-sugar solution varies also with the de- gree of concentration of the solution. Sucrose in the Presence of Raffinose.* Prepare 26.048 grins, of the sample for polarization, as directed p. 33, and polarize. Of the polarized solution (from which all lead should first have been removed) take 50 c.c. Place in a 100 c.c. flask ; add 5 c.c. concentrated hydro- chloric acid (38.8 per cent HC1) and about 20 c.c. of dis- tilled water. Heat on a water-bath up to between 67 * Method prescribed by the German Government to regulate the duty on sugar, July 9, 1887. Several methods and numerous modifications have been proposed to effect the determination of raffinose. For the bene- fit of those desiring more information on the subject, a list of references is given on the opposite page. SUGAR ANALYSIS. 47 and 68 C. This should take about five minutes. When this temperature has been reached, it should be maintained for five minutes more. The solution is then quickly cooled to 20 C., made up to the 100 c.c. mark, and polarized at exactly 20 C. in a tube provided with a very sensitive and accurate thermometer. This tube should be enclosed in another tube or should be placed in a trough which is filled with water, so that the temperature of 20 C. may obtain throughout the observation. Author. Publication. Year. Volume. Page. Pellet and Biard. Journal des fabr. de sucre. 1885 Von Lippmann. Deutsche Zuckerindustrie. 1885 X. 310 Tollens. Zeitschrift d. V. f. Ruben- 1886 XXXVI. 236 zucker-Ind. Scheibler. Neue Zeitschrift f. Ruben- 1886 XVII. 233 zuclcer-Ind. Creydt. Zeitschrift d. V. f. Riiben- 1887 XXXVII. 153 zucker-Ind. Creydt. Zeitschrift d. V. f. Ruben- 1888 XXXVIII. 979 zucker-Ind. Directions of the Ger- Neue Zeitschrift f. Riiben- 1888 XXI. 132 man Government. zucker-Ind. Gunning. Neue Zeitschrift f. Rtlben- 1888 XXI. 335 zucker-Ind. Lotman. Chemiker Zeitung. 1888 XII. 391 Breyer. . it 1889 XIII. 559 Schulz. Zeitschrift d. V. f. Riiben- 1889 XXXIX. 673 zucker-Ind. Wortman. Zeitschrift d. V. f. Riiben- 1889 XXXIX. 767 zucker-Ind. Lindet. The Sugar Cane. 1889 XXI. 542 Herzfeld. Zeitschrift d. V. f. Riiben- 1890 XL. 165 zucker-Ind. Courtonne. Journal des fabr. de sucre. 1890 XXXI. 48 SUGAR ANALYSIS. The sucrose and raffinose are calculated by the formulae :* o (0.5188XP)-/. A QA K J 0.845 L85> S = sucrose ; H = raffinose ; P = polarization of normal weight (26.048 grins.) before inversion ; 1= polarization of normal weight (26.048 grnis.) after inversion. Example. Polarization before inversion, 93.8 Polarization after inversion, 12.7 93.8 x 0.5188 = + 48.66344 . - 12.7 x 2 - 25.40000 + 74.06344 74.06344 -f- 0.845 = 87.6. S = 87.6 per cent. 93.8 - 87.6 _6.2 -r- 1.85 = 3.35. R = 3.35 per cent. If the observation of the inverted raffinose solution has not been made at 20 C. a correction of 0.0038 for each degree Centigrade above or below 20 C. must be * Tollens and Herzfeld prefer to calculate these values by the formulee: (0.6124 xP)-/ P - S ~~ - SUGAR ANALYSIS. 49 introduced. This correction is effected by the formula :* Polarization j ( Polarization | after inversion > = K after inversion > + 0.0038 $(20 t\ at 20 C. j ( at t C. ) in which $ represents the sum of the polarizations before and after inversion. Example. Suppose a solution of sucrose and raflinose polarized : before inversion, 105.0 ; After inversion, 22.0 at a temperature of 18.2 C. Then the polarization after inversion at 20 C. will be equal to : -22.0 + 0.0038(105.0 +22.0) (20.- 18.2) - 22.0 + 0.0038(+ 127.0)(+ 1.8) -22.0 + 0.86868 - 21.13. Sucrose in Presence of Dextrose (Glucose). Qualita- tive Tests. A number of tests have been proposed for the qualitative examination of a sugar for dex- trose. Among these the following are possibly the most serviceable : f Thoroughly dry the sample to be examined. Prepare a solution of methylic alcohol satu- rated with dextrose.J Pour some of this solution on the dried sample, and stir for about two minutes. Allow the residue to settle, and pour off the clear solution. Repeat this treatment. If any dextrose is present, some chalky- * Zeitschrift des Vereines fiir Riibenzucker-Industrie, vol xl. p. 201. t Casamajor, Journal of the American Chemical Society, vol. ii. p. 428, and vol. iii. p. 87. t 100 c.c. methylic alcohol, showing 50 by Gay-Lassac ? s alcoholometer, dissolve 57 grammes of dry glucose. The specific gravity of the solution is 1.25. 50 SUGAR ANALYSIS. white particles and a fine deposit will remain, for dextrose is practically insoluble in the solution employed, while the sucrose will go into solution. The test is best made in a beaker with a flat bottom or on a pane of glass. If a syrup is to be examined for the presence of dex- trose, provided the dextrose has been added in suffi- ciently large quantity, and the syrup has the usual den- sity of about 40 Baume, the following test may be applied: The direct polarization of the syrup should show a percentage of sugar not higher than the number of Baume degrees which indicate the density. If, * for instance, a syrup of 40 Baume should show a direct polarization of 55.0, some dextro-rotatory substance, most probably dextrose, must have been added to this syrup, as an unadulterated product of this description would be a mixture of crystals and syrup, and could not be a clear syrup. The polariscope may also be resorted to for detecting the presence of dextrose. The manner of procedure is simple : The solution is prepared as usual for the polariscope ; then, immediately after preparing it, a reading is taken ; the solution is allowed to remain in the tube for some time, and repeated readings are taken at certain inter- vals. If dextrose is present, the successive readings will become lower and lower, for dextrose is bi-rotatory. Readings on the solution are continued until the rotatory power has become stationary ; it may take up to fifteen hours before this is attained. "When this point has been reached, treatment with hydrochloric acid (attempted inversion), will produce no SUGAR ANALYSIS. 51 effect, the dextro-rotatory power of the dextrose remain- ing unchanged. Quantitative Methods. The quantitative methods for the determination of dextrose in the presence of sucrose are based either on optical analysis, on gravimetric analy- sis, or on a combination of both. Among the methods of the first type, that of hot polarization, due to Drs. Chandler and Ricketts, is prob- ably the best.* . This method depends upon the following well-known facts : 1. Dextrose, under the conditions of analysis, exerts a constant effect upon the plane of polarized light at all temperatures under 100 C. 2. Lcevulose. The action of laevulose is not constant, the amount of rotation to the left being diminished as the temperature is increased.f 3. Invert-sugar, being a mixture of one half dextrose and one half Isevulose, does not affect the plane of polar- ized light at a certain temperature, somewhere near 90* C.J (for it can easily be seen that the constant dextro- rotatory power of dextrose must be neutralized by the varying Isevo-rotatory power of laevulose at some such temperature. The exact temperature is determined by experiment). 4. Cane-sugar, when acted on by dilute acids, is con- verted into invert-sugar, while dextrose remains practi- cally unaltered. * Abstracted from a report made by A. L. Colby to the Chairman of the Sanitary Committee in the Second Annual Report of the State Board of Health of New York, 1882. t Watts' Dictionary of Chemistry, vol. v. p. 464. t Ibid. p. 465. 52 SUGAR ANALYSIS. Hence, if a "mixed sugar" is heated with dilute acids, the cane-sugar present is converted into invert- sugar, which, with that originally present (due to the process of manufacture), is optically inactive at a certain temperature (near 90 C.) ; while the artificial dextrose, preserving its specific rotatory effect, will at this temper- ature show a deviation to the right in proportion to the amount present. It is only necessary, therefore, to secure some means of heating the observation-tube of the ordinary polari- scope, so that readings may be taken at any temperature under 100 C. The middle portion of a Soleil-Ventzke saccharimeter, ordinarily intended for the observation- tube alone, is so modified as to admit of the interposition of a metallic water- bath, provided at the ends with metal caps, which contain circular pieces of clear plate-glass. The tube for holding the sugar solution to be polarized, is made of platinum, and provided with a tubule for the insertion of a thermometer into the sugar solution. The metallic caps at the end of the tube rest on project- ing shelves inside the water-bath, thns bringing the tube into the centre of the bath, where it is completely sur- rounded by water. The cover of the w r ater-bath is arranged for the insertion of a thermometer, so that the temperatures of the water-bath and of the sugar solution may both be ascertained. The water-bath is heated from below by two to four small spirit-lamps or gas-burners. The first step in using the instrument is to determine, by experiment, the exact temperature of the sugar solution, at which invert-sugar is optically inactive on polarized light. This will vary slightly with different instruments. For the particular instrument and thermometer used in SUGAR ANALYSIS. 53 the investigations referred to, 86 C. was found, by re- peated experiment, to be the temperature of the pure in- verted sugar solution at which the reading was zero on the sugar scale. The next step taken was the determination of the value of a degree of the scale in terms of the glucose known to be the variety used to adulterate cane-sugar. It was found that the rotation to the right at 86 C. was 41 , when using a solution containing in 100 c.c. fifteen grammes of a sample containing 85.476 per cent chemically pure glucose. Hence as fifteen grammes was the amount taken, 15 x ^ffp- -T- 41 X 100 = 31.2717 grammes, which repre- sents the amount of chemically pure glucose necessary to read one hundred divisions on the sugar scale of the in- strument used; or, each division 0.312717 grammes chem- ically pure glucose. (A duplicate determination made, by using 26.048 grammes, gave as a factor 0.312488.) The success of the process depends greatly upon the -care exercised in preparing the sugar solution for the polariscope. The inversion and subsequent clarification were accomplished as follows : 26.048 grammes of the sugar to be examined w r ere com- pletely dissolved in about 75 c.c. of cold water, and were treated with 3 c.c. of dilute sulphuric acid (1 to 5 by volume) on a water-bath at a temperature of about 70 C. for thirty minutes. The solution thus inverted was then rapidly cooled, nearly neutralized with sodium car- bonate solution (saturated), transferred to a 100 c.c. flask, and the gummy matters, etc., precipitated with 5 c.c. of a solution of basic lead acetate.* The flask was then filled * Prepared by boiling for thirty minutes 440 grammes neutral lead ace- tate with 264 grammes litharge, in one and a half litres of water ; dilut- ing when cool to two litres, and siphoning off the clear liquid. 54 SUGAR ANALYSIS. to the mark, the solution transferred to a small beaker, mixed with enough bone-black to clarify completely, and then thrown on a fluted niter. The amount of bone- black necessary to effect decolorization depends on the grade of the sugar and on the color of the solution. It was not found necessary to use, even with sugars of the lowest-grade, more than five grammes.* The clarified inverted sugar solution was then placed in the platinum polarization- tube, the water-bath was filled with cold water, the thermometers were adjusted, and the temperature gradually raised to 86 C. This part of the operation should take about thirty minutes. If the sample is unadulterated, the polariscope reading would be zero at 86 C., while if starch-sugar is present the amount of deviation to the right, in degrees and fractions, multiplied by the proper factor and divided by the amount taken, would give the per cent age of chem- ically pure glucose added as an adulterant. Gravimetric Method. The following method is based on gravimetric determinations, and is independent of all optical data. This will be recognized as an advantage when the great influence is remembered that temperature- fluctuations exert on the rotatory power of invert-sugar. Unfortunately, however, the destruction of the Isevu- lose by hydrochloric acid (Sieben's process), on which this, whole scheme of analysis is based, is not always accom- plished with the same certainty, f and the results obtained by this method must therefore be received with some caution and reserve. * The bone-black used was pulverized to pass through an 80-mesh sieve,, dried at 110 C. for three hours, and kept in a well-closed bottle. t The Author : School of Mines Quarterly, 1890, yol. xi. SUGAR ANALYSIS. 55 The determinations to be made are : 1. Total sucrose. See p. 42. 2. Total reducing sugars. See p. 69. 3. Dextrose after destruction of the laevulose by Sie- ben's treatment. See p. 59. Determination No. 1 embraces : a. Invert-sugar formed from the sucrose by inversion. b. Invert-sugar existing as such. c. Bodenbender's substance (regarded as invert-sugar). d. Free dextrose (if present). Determination No. 2 embraces : a. Invert-sugar. b. Bodenbender's substance (regarded as invert-sugar). c. Free dextrose (if present). Determination No. 3 embraces : a. Dextrose from the inverted sucrose. b. Dextrose from invert-sugar. c. Dextrose from Bodenbender's substance (regarded as invert-sugar). d. Free dextrose (if present). No. 1 minus No. 2 gives the copper reduced by the (inverted) sucrose. One half of this amount represents the dextrose from this source, i.e., from the sucrose which was turned into invert-sugar. Subtracting this from No. 3 leaves the copper due to the dextrose of the invert-sugar + the dextrose of Boden- bender's substance (regarded as in vert- sugar) + free dex- trose, it" present. Call this amount x. If there is no free dextrose present, but only invert- sugar and Bodenbender's substance (regarded as invert- sugar), then 2 X x must be equal to the amount of cop- per found in No. 2. 56 SUGAR ANALYSIS. If there is no in vert- sugar, but only sucrose and dex- trose, then x will be equal to No. 2. If there is free dextrose present besides the invert- sugar, then 2 X os will be greater than No. 2, and the amount of copper representing the free dextrose will be found, as shown by example No. 3. Example 1. Present: sucrose and invert-sugar, but no free dextrose. Det. No. 1 yields 0.420 Cu Det. No. 2 " 0.040 Cu Det. No. 3 " 0.212 Cu No. 1, 0.420 minus No. 2, 0.040 0.380 -f- 2 = 0.190 Cu due to dex- trose from the inverted sucrose. Det. No. 3, 0.212 less 0.190 0.022 This corresponds to the x above. 0.022 x 2 = 0.044 Det. No. 2 = 0.040 These two values agree within 0.004, and as the limit of difference should be placed at 5 milligrammes of copper, it must be inferred that this solution contained no free dextrose. Another way of calculating is as follows : Det. No. 3, 0.212 Cu Det. No. 1 = 0.420 less Det. No. 2 = 0.040 0.380 -h 2 = 0.190 Cu 0.022 Cu SUGAR ANALYSIS. 57 This is the copper due to the dextrose from the invert- sugar, from Bodenbender's substance (regarded as invert- sugar) and from free dextrose, if any is present. This amount 0.022 must be equal to one half of No. 2, if no free dextrose is present. No. 2 = 0.040 -7-2= 0.020 ; hence there is a differ- ence of only 0.002, and therefore there is no free dextrose. Example 2. Present : sucrose and dextrose,, but no invert-sugar. Det. No. 1 yields 0.474 Cu Det. No. 2 " " 0.286 Cu Det. No. 3 " 0.382 Cu Det. No. 1 = 0.474 less No. 2 = 0.286 0.188 4- 2 = 0.094 Cu due to the dextrose of the inverted sucrose. Det. No. 3 = 0.382 less 0.094 0.288 This value is not equal to one half of No. 2, but equal to the whole of the copper found in No. 2 (in fact it shows 2 milligrammes of Cu more) ; hence this solution contained no invert-sugar, but only sucrose and dextrose. Example 3. Present : sucrose, dextrose, and invert- sugar. Det. No. 1, 0.500 Cu Det. No. 2, 0.300 Cu Det. No. 3, 0.275 Cu Det. No. 1, 0.500 less No. 2, 0.300 0.200 58 SUGAR ANALYSIS. .200 -r- 2 = .100 copper due to dextrose from the in- verted sucrose. No. 3, 0.275 less 0.100 0.175 .175 X 2 = 0.350 No. 2 is 0.300; hence, as this value 0.350 is greater than No. 2, yet not twice as great, there must be present invert-sugar and free dextrose. To calculate the amounts respectively of the invert-sugar and of the dextrose, pro- ceed as follows : No. 2, 0.300 is Cu reduced by the invert-sugar, Bodenben- der's substance and dextrose ; 0.175 is Cu reduced by one half of the invert-sugar and of Bodenbender's substance, and by the whole of the dextrose ; 0.125 X 2 = 0.250 invert-sugar and Bodenbender's substance ; and 0.300 minus 0.250 = 0.050 is the Cu reduced by the dextrose. .The 0.250 Cu reduced by the invert-sugar + Boden- beuder's substance (regarded as invert-sugar) is equal to 0.1347 invert-sugar. The 0.050 Cu reduced by the dextrose is equal to 0.0259 dextrose. (Table XV). The 0.200 Cu reduced by the invert-sugar produced from the sucrose by inversion, corresponds to 0.1015 su- crose ; hence the sample contains : SUGAR ANALYSIS. 59 Sucrose, milligrammes, 101.5 Invert-sugar (inclusive of Bodenbender's substance), milligrammes, . . . . 134.7 Dextrose, milligrammes, 25.9 Knowing the amount of dry substance on which the tests were performed, the calculation to percentage can be readily effected. Sieben's Process for Destruction of Lsevulose. Take 100 c.c. of a solution made to contain 2.5 grammes on the dry substance of invert-sugar, or of invert-sugar and laevu- lose, place in a flask, add 60 c.c. of a hydrochloric-acid solution which is six times the strength of a normal solu- o tion, and heat the flask for three hours while it is sus- pended in boiling water. After this has been done, cool immediately, neutralize with a sodium-hydrate solution which is six times the strength of a normal solution, make up to a volume of 250 c.c., and filter. Of the filtrate use 25 c.c. for the determination of the dextrose ; this is obtained as follows : Take 30 c.c. copper-sulphate solution ; * 30 cc. Rochelle-salt solution ; f 60 c.c. water. Heat to boiling. Add the 25 c.c. dextrose solution, prepared as above, and keep boiling for two minutes. Then proceed as with a gravimetric determination of invert-sugar. (See p. 69). Table XV shows the amount of dextrose corresponding to the weight of copper found. * Prepared by dissolving 69.278 grammes C. P. sulphate of copper in dis- tilled water, and making the solution up to 1 litre. f Prepared by dissolving 173 grammes Rochelle salt, cryst. and 125 grammes potassium hydrate in distilled water, and making the volume up to 500 c.c. 60 SUGAR ANALYSIS. Determination of Sucrose, Dextrose, and Lsevulose. Several methods have been suggested for the deter- mination of sucrose, dextrose, and Isevulose in the pres- ence of each other. Some of these are combinations of optical and gravi- metric methods ; as, for instance, those given by Tucker, * Apjohn,f and Dupre. J The first of these mentioned is directed to the determination of dextrose and laevulose, while the others refer also to the determination of sucrose. Winter has published an outline of the separation and determination of dextrose and Isevulose in the pres- ence of sucrose; his method is based on the action of ammoniacal acetate of lead. This reagent is prepared, immediately before use, by adding ammonic hydrate to basic acetate of lead solution, until the turbidity formed just continues to disappear. To the solution to be examined, add ammoniacal acetate of lead until no further precipitate is formed. Then filter. The precipitate must be digested with large quantities of water, and the washings must be added to the filtrate. This filtrate contains the sucrose. The precipitate consists of the lead salts of dextrose and Isevulose. It is suspended in water, carbonic-acid gas is passed in, and the solution is then filtered. The filtrate contains the dextrose. This is determined by the polariscope and by its action on alkaline copper solution. * Tucker: Manual of Sugar Analysis, 2d Ed., p. 208. f Chemical News, vol. xxi. p. 86 ; Amer. Reprint, p. 230. j Loc. cit., p. 97 ; Amer. Reprint, p. 239, Zeitschrift des Vereiues fur Riibeiizucker-Industrie, 1888, p. 782. SUGAR ANALYSIS. 61 The precipitate consists of the carbonate and the laevu- losate of lead. This is suspended in water, and sulphu- retted hydrogen gas is passed in. The sulphide of lead is removed by filtration. The filtrate is concentrated by evaporation, and the Isevulose is determined by the polari- scope and by its action on alkaline copper solution. Gravimetric Method. The gravimetric method de- scribed on page 54 can also be adapted to the deter- mination of sucrose, invert-sugar and dextrose, or laevu- lose. The determinations to be made are the same as those there directed, namely, total sucrose, total reducing sugars, and total dextrose after destruction of the laevu- lose by Sieben's treatment. The same reserve, however, as there noted, must be exercised with reference to accepting the results ob- tained. Any method by which the destruction of the laevulose could be effected completely and under all cir- cumstances, and leave the dextrose unattacked, would make this method a most valuable one. The method of calculating the results is analogous to the one before given, and consists of two steps : Step I. is always the same, and merely establishes whether the dextrose and the Isevulose are present in the proportion of 1 to 1, or whether either is in excess. Step II. determines the amount of this excess, be it of dextrose or of Igevulose. Values determined : No. 1. Copper reduced by total sucrose + total reducing sugars. No. 2. " total reducing sugars. No. 3. " " " dextrose (after Sieben's treat- ment). 62 SUGAR ANALYSIS. CALCULATION. Step I- No. 1 = Cu reduced by inverted sucrose and total reducing sugars. Less No. 2 = Cu reduced by total reducing sugars. Difference = Cu reduced by inverted sucrose. Report the corresponding value as sucrose. This difference -r- 2 = Cu reduced by the dextrose of the inverted sucrose. Call this value x. No. 3 Cu reduced by the total dextrose (after Sie- ben's treatment). Less x = Cu reduced by the dextrose of the inverted sucrose. Difference = Cu reduced by the dextrose of the total re- ducing sugars. Call this value y. Then, y X 2 = 2?/ Cu reduced by invert-sugar + free dex- trose, if any is present. Compare this value, 2y, with No. 2 : If 2y = No. 2, invert-sugar only is present. If so, report as invert-sugar. If 2y > No. 2, free dextrose is present. If 2y < T$. 2, free laevnlose is present. Step II. When 2y > JV0. 2, free dextrose is present. No. 2 = Cu reduced by the total reducing sugars. Less y Cu reduced by the dextrose from the total reducing sugars. SUGAR ANALYSIS. 63 Difference = Cu reduced by the laevulose of the total reducing sugars. Call this value p. p x 2 = 2p Cu reduced by invert-sugar. Report as invert-sugar. No. 2 = Cu reduced by the total reducing sugars, less 2p = Cu reduced by invert-sugar. Difference = Cu reduced by the free dextrose. Step II. When 2y < No. 2, free Icevulose is present. No. 2 = Cu reduced by the total reducing sugars. Less %y = Cu reduced by the invert-sugar. Report as invert-sugar. Difference = Cu reduced by the free laevulose. In these calculations no attention has been paid to the fact that the reducing-power of invert-sugar, dextrose, and laevulose for copper solutions is not identical. The reducing power of dextrose being considered as 100, that of invert-sugar is 96, and of laevulose 94. CHAPTER V. INVERT-SUGAR. Qualitative Examination for Invert-Sugar. TEST WITH METHYL-BLUE. Dissolve 1 gramme of methyl-blue in 1 litre of water, and keep for use. To execute this qualitative test for the presence of invert-sugar, dissolve 20 grammes of the sugar in water, add basic acetate of lead solution, make up to 100 cubic centimetres, and filter. Make the filtrate slightly alkaline with a 10 per cent solution of sodium carbonate, and fil- ter again. Of this filtrate take 50 cubic centimetres, representing about 10 grammes of the sugar tested, place in a porcelain casserole, and add 2 drops of the methyl-blue solution. Then place the casserole over a naked flame, and note accurately when the solution begins to boil. If the solution is decolorized by boiling, inside of one half -minute, there is sufficient invert-sugar present to permit of a quantitative determination. If it requires from one-half to three minutes boiling to effect disap- pearance of the blue color, traces of invert-sugar are to be reported; and if decolonization does not take place within three minutes, " no invert-sugar" is recorded. If the normal weight has been dissolved up to 100 c.c., 20 c.c. of the solution, clarified by basic acetate of lead, are made up to 50 c.c. The lead is removed by add- ing five drops at a time of the sodium-carbonate solution, 64 SUGAR ANALYSIS. 65 and the a^Bion of this reagent, in the same quantity, is continued^mtil no more precipitation can be detected. To 25 c.c. of the filtrate one drop of the methyl-blue solution is added; about 10 c.c. of this solution are kept actively boiling over a naked flame for one minute. If, after thus boiling for one minute, the solution is completely decolorized, it must have contained at least 0.01 per cent of invert-sugar. If it is not decolorized, it contained no invert-sugar, or certainly less than 0.015 per cent.* Quantitative Determination of Invert-Sugar. Feh- ling's solution (Soxhlet's formula) : Sulphate of copper cryst,, 34.639 grins, in 500 c.c. of water. Rochelle salts, . . . 173.0 grms. in 400 c.c. of water. Sodic hydrate, . . . 50.0 grms. in 100 c.c. of water. Keep the sulphate of copper solution in one flask, and the Kochelle-salt-soda solution in another. Mix the two immediately before use. It will be found very conven- ient to have the solutions in flasks or jars provided with a siphon-arrangement, and to have the delivery-tube so graduated that the required amount may be rapidly, yet accurately measured out. The accompanying figure shows an arrangement answering this purpose. Fig. 5. Volumetric Methods. SOXHLET'S METHOD. f Take 25 c.c. of the sulphate of copper solution and add to it 25 c.c. of the Rochelle-salt-soda solution. * Wohl. Zeitschrift des Vereines fur Riibenzucker-Industrie, 1888, p. 352. f Journal fiir Practische Chemie, New Series, 1880, vol. xxi. p. 227. 66 SUGAR ANALYSIS. Place in a deep porcelain casserole, heat to boiling, and add sugar solution until the fluid, after boiling for two minutes, is no longer blue. This preliminary test indicates approximately (within about 10 per cent) the amount of invert-sugar present. Next dilute the sugar solution till it contains about 1 per cent of invert-sugar. The true concentration will be 0.9 to 1.1 per cent, which slight deviation from the con- centration desired, has no influence on the result. Take 50 cc. of Fehling's solution, heat, add the requi- site amount of sugar solution, boil for two minutes, and then pour the whole solution through a large corrugated filter-paper. Test the filtrate for copper by acetic acid and potassium ferrocyanide. If copper is found to be present, repeat the test, but take a greater volume of the sugar solution. If the fil- trate is found to be free from copper, repeat the test, but take 1 c.c. less of the sugar solution. Continue with these tests until of two sugar solu- tions, differing from one another by only 0.1 c.c., the one shows copper, and the other shows no copper in the fil- trate. The amount of sugar solution intermediate be- tween these two, must be regarded as the one that will just decompose 50 c.c. of the Fehling solution. 1.0 equivalent of invert-sugar reduces 10.12 equiva- lents of cupric oxide in solutions made as here prescribed. If the solution be diluted by four volumes of water, 1.0 equivalent of invert-sugar will reduce 9.7 equivalents of cupric oxide. METHOD.* Five, ten, or, if necessary, more * Annalen der Chemie und Pharmacie, 1849, vol. 72, p. 106. SUGAR ANALYSIS. 67 grammes of sugar are weighed out, dissolved in a flask, and the solution made up to 100 c.c. The weight of sugar used varies, of course, with the nature of the sample examined, that is to say, with the amount of invert-sugar it contains. It is advantageous to have the solution of such a strength that 20 c.c. to 50 c.c. will completely pre- cipitate the copper in 10 c.c. of the solution cited above. The Fehling solution is measured out (using 5 c.c. each of the copper sulphate and the Rochelle-salt-soda solu- tion), placed in a porcelain dish, and quickly brought to the boiling-point. The sugar solution is then run in from a burette (graduated in tenths of a cubic centime- tre) until all of the copper in the solution is precipitated as cuprous oxide. The operator is warned of the approach of the end of the reaction by the change in the color of his solution. The blue color disappears and the solution becomes colorless, or, if the sugar solution is colored, assumes a yellow tinge. The end-point, however, is determined by filtering a few drops of the solution through paper or linen cloth into a very dilute solution of potassic ferrocyanide * and acetic acid, f If a brownish-red color shows, owing to the forma- tion of cupric ferrocyanide, two tenths c.c. more of the sugar solution are added to the copper liquor, the solu- tion is again boiled, and the test repeated. This is con- tinued until the addition of a few drops of the solution to the ferrocyanide no longer produces the red color. If a polarization is to be made on the same sample, 19.21 cubic centimetres of the solution for polarization, * 20 grammes dissolved in 1 litre of water, t A 10 per cent solution. 68 SUGAR ANALYSIS. prepared by dissolving 26.048 grammes in 100 c.c., and from which the lead has been removed, represents ex- actly 5 grammes, and may be used for the determination of the invert-sugar. If the French normal weight (16.19 grammes) has been used, 30.8 c.c. are required. These amounts can be measured out from a burette, or pipettes may be procured, graduated to deliver the given volumes of solution. As 10 c.c. of the copper solution are assumed to cor- respond to 0.5 gramme of invert-sugar, the calculation is an easy one. If 5 grammes of sugar have been dissolved up to 100 c.c., the reciprocal of the number of cubic cen- timetres required of this solution to precipitate all of the copper in 10 c.c. of the copper liquor, multiplied by 100, is the direct percentage of invert-sugar sought. (See Table XII.) Example. Dissolved 5 grammes of sugar in 100 c.c. Of this solution used 22 c.c. to precipitate all of the cop* per in the Fehling solution. Referring to Table XII, 22 c.c. will be found to correspond to 4.54 per cent of invert-sugar; hence there is this amount of invert-sugar present in the sample. DEXTEOSE SOLUTION FOE STAND AEDIZING THE FEHLING SOLUTION. Dissolve 4 grammes C. P. anhydrous dextrose, in distilled water, and make up to 1000 c.c. 1 c.c. = 0.004 dextrose. To test the strength of the copper solution, place 10 c.c. of it in a porcelain dish or casserole, with from 30 to 40 c.c. of water. Boil, and run in the dextrose solution from a burette until all the copper* is precipitated. The number of cubic centimetres of the dextrose solution used, multiplied by 4, represents the number of SUGAR ANALYSIS. 69 milligrammes of dextrosg^M^uired to precipitate the cop- per in 10 c.c. oftlie Jfnlmg solution. Gravimetric Method. MEISSL-HERZFELD. Weigh out 26.048 grammes pf the sample. Place into a 100 c.c. flask, clarify with basi^i acetate of lead, make up to 100 c.c., filter, and polarise. Take an aliquot part of the filtrate, add sodium sulphate to remove any lead present, make up to a definite volume, and filter. It is best to arrange the dilution so, that the 50 c.c. of this filtrate, which are to be used for the determination of the invert-sugar, will precipitate between 200 and 300. milligrammes of copper. To 50 c.c. of the sugar solution prepared as above, add 50 c.c. Fehling's solution (25 c.c. copper sulphate and 25 c.c. of Rochelle-salt-soda solution). Over the wire-gauze above the flame lay a sheet of asbestos provided with a circular opening of about 6.5 cm. diameter; on this place the flask, and arrange the burner in such a manner, that about four minutes are consumed in heating the solution to the boiling-point. From the time that the solution starts to boil the ^jaoinent when bubbles arise not only from the centre) but also from the sides of the ves- sel continue to boil for exactly two minutes with a small flame. Then remove the flask from the flame im- mediately, and add 100 c.e. of cold distilled water, from which the air has previously been removed by boiling,* Then filter through an asbestos filter, wash, and reduce to metallic copper. f * The water is added to prevent subsequent precipitation of cuprous oxide. t This last step is sometimes omitted, the cuprous oxide being weighed after washing and drying, and the corresponding amount of copper cal- culated. 70 SUGAR ANALYSIS. This operation is carried out in the following manner: Clean thoroughly a small straight calcium-chloride tube, or other tube of similar pattern. Introduce asbestos fibres* so as to fill about half of the bulb. Draw air through while drying, cool, and weigh. Connect with an aspirator, filter the precipitated Cu 2 O, wash with hot water, and then, having changed the receiving flask, wash twice with absolute alcohol and twice with ether. Hav- ing removed the greater part of the ether by an air-cur- rent, connect the upper part of the filter tube by means of a cork and glass tubing with a hydrogen apparatus,, and, while the hydrogen gas is flowing through, cau- tiously heat the precipitate with a small flame whose tip is about 5 cm. below the bulb containing the Cu 2 O. The reduction should be completed in from two to three minutes. After the tube has been cooled in the current of hy- drogen, air is once more drawn through and the tube is. then weighed. After an analysis is completed, the asbestos is readily freed from the adhering copper by washing with dilute nitric acid. The use of the electric current has also been advo- cated for reducing the precipitate to metallic copper, f The cuprous oxide is dissolved with 20 c.c. nitric acid (sp. gr. 1.2), the solution is placed into a w r eighed platinum dish, made up to between 150 and 180 c.c. with * The asbestos must first be prepared by washing successively with a solution of caustic soda (not too concentrated), boiling water, nitric acid, and again with boiling water. When filled into the glass tube the asbestos, is made to rest on a perforated platinum cone. t Formanek Bohm. Ztschr. fur Zuckerindustrie, 1890, vol. xiv. p. 178. SUGAR ANALYSIS. 71 distilled water, and the copper precipitated by the elec- tric current. The method of calculating the amount of invert- sugar, corresponding to the weight of copper found, can best be illustrated by an example. Suppose that of the 26.048 grammes of sugar dissolved in 100 c.c., 25 c.c. had been removed, clarified with sodium sulphate, made up to 100 c.c., and filtered: 50 c.c. of this filtrate would cor- respond to 3.256 grammes of substance. Let this weight be designated by the letter p. The approximate amount of invert-sugar may be as- sumed to be _ Cu 2 ' The approximate percentage of invert-sugar will be _Cu 100 2 ~p~' Representing the former value by Z, the latter by y, we have ^ _ Cu Z = : T' and Cu 100 y = -TT x 2 p The ratio between the invert-sugar and the sucrose is determined by the following formulae, designating sucrose by the letter R, and invert-sugar by I. j2 _ 100- X Polarization Polarization + y 1= 100 - R. Example. Polarization of 26.048 grammes = 86.4. p 3.256 grammes. 72 SUGAR ANALYSIS. Suppose these 3.256 grammes have precipitated on "boiling with Fehling's solution 0.290 grammes of copper. Then, 100 X Pol. 8640 , Pol. + y = 86.4 + 4.45 " 100 - It = I, 100 -95.1 = 4.9, 4.9= I, and therefore the ratio of H : Us expressed by 95.1 : 4.9. In order to find the factor F we must hunt up the correct vertical and horizontal columns in Table XIII, The value Z 145 is most closely approximated by the column headed 150; the ratio R : I 95.1 : 4.9 is most closely approximated by the horizontal column 95 : 5. At the line of intersection of these two columns there will be found the factor 51.2, by aid of which the final calculation is effected. 4. X F ^-, X 51.2 = 4.56 p. c. invert-sugar. p 3.256 The analysis would hence show: Sucrose, ........ 86.40 Invert-sugar, ...... 4.56 If duplicate or comparative determinations of invert- sugar are to be made by this method, the same weight of substance should always be taken. Otherwise, the value of Z varying, will necessitate the employing of different factors, and in consequence discrepancies will ensue. SUGAR ANALYSIS. 73 Example : Weight used, . . . 2.500 grammes. Polarization, . . . .95.00 Cu reduced, .... 0.140 Invert-sugar 2.587 per cent. Weight used, . . . 5.000 grammes. Polarization, .... 95.00 Cu reduced, . . . . 0.278 Invert-sugar = 2.768 per cent. Of the methods here described, Soxhlet's is possibly the most exact, but its execution calls for more time than can generally be given in a technical laboratory. Of the other two methods given either may be used in practice, as each gives reliable results. Comparative determinations have shown that the results yielded by these two methods agree closely.* If an invert-sugar determination has been made in a syrup, the result can be recorded either as percentage on the syrup, or as percentage on the dry substance. The calculation necessary to obtain the latter, corresponds of course, to that explained on page 41. These methods of determining invert-sugar are based on the assumption that there are no other substances present besides invert-sugar which will precipitate the copper from its solution. Sometimes, however, such bodies are present. In beet-sugars their existence has been amply demonstrated, and their presence in cane- products is probable. * The Author, ' ' Determination of Invert-Sugar by Alkaline Copper Solutions," School of Mines Quarterly, November, 1888. 74 SUGAR ANALYSIS. To determine the invert-sugar in sucli cases, a dupli- cate copper determination, the one before, the other after the destruction of the invert-sugar, is necessary.* Of the caustic potash necessary for the preparation of Fehling's solution, dissolve 40 grammes, together with 175 grammes Rochelle salt, and make the solution up to 400 c.c. with water; 20 grammes of the caustic potash dissolve up separately with water to 100 c.c. I. Heat 10 grammes (50 c.c.) of the sugar, clarified with basic acetate of lead, to boiling. Into this put 50 c.c. of Fehliug's solution heated to the boiling-point. This solution is composed of 25 c.c. copper-sulphate solution, 20 c.c. of the alkaline Rochelle-salts solution, and 5 c.c. of the caustic-potash solution. Boil exactly two minutes. II. 10 grammes (50 c.c.) of the sugar, clarified with basic acetate of lead, are boiled for 10 minutes with 5 c.c. of -the caustic-potash solution, care being taken to re- plenish the water which evaporates. Then 25 c.c. copper- sulphate solution + 20 c.c. of the alkaline Rochelle-salts solution are added, and the mixture boiled for two min- utes more. The rest of the determination is then carried out exactly as before described. The amount of copper obtained under II. is sub- tracted from the amount found under I., and the remain- der calculated to invert-sugar. Soldaini's Solution. Within the past few years great claims have been made for the Soldaini copper solution for the determination of invert-sugar, as being superior to the numerous so-called " Fehling" solutions, f * Bodenbender and Scheller. t Stammer's Jahresbericht, 1885, p. 283, enumerates no less than twenty different formulae for the preparation of the same. SUGAR ANALYSIS: 75 Soldaini's solution is prepared* by dissolving 15.8 grammes of sulphate of copper in a hot solution of 594 grammes of potassium bicarbonate. After the copper pre- cipitate has completely dissolved, the solution is made up to 2 litres. The specific gravity of the solution is about 1.1789. The manner of working with this solution is analo- gous to that described on page 69 et seq. The time of boiling is 10 minutes. Table XIV shows the relation between the amount of copper reduced and the invert-sugar. This solution has as yet not been generally adopted, but many opinions in its favor have been expressed. Among the objections cited against itf are, that it contains only one fifth the amount of copper that Feh- ling's solution contains, and that hence it must be in many cases less sensitive than the former. On being greatly diluted it deposits cupric oxide, and on boiling for a long time it deposits cuprous oxide. * Schellers formula. t Herzfeld, Zeitschrift des Vereines fur Riibenzucker-Industrie, 1890, vol. xl. p. 52. CHAPTER VI. WATER ASH- SUSPENDED IMPURITIES. Water. Weigh out 5 to 10 grammes of the sample. If the determination is to be made on a rather moist sugar or on a syrup, a corresponding amount of perfectly dry powdered glass or of sand must be intimately mixed with the sample. Place in an air-bath, the heating of which should be commenced only after the introduction of the assay. The heat should be gradually carried up to between 95 and 100 C., and continued until the sample has attained to constant weight. The loss in weight sustained, represents the water. Example. Weight of dish, sand, and sample, . 23.0000 " and sand, . . . 18.0000 Sample taken, 5.0000 Original weight of dish, sand, and sample, . . 23.0000 Final weight (after drying to constant weight), 21.1546 Water = 1.8454 5.000 : 1.8454 : : 100 : x. x = 36.91 per cent water. Instead of drying in an air-bath, the drying can be done in a current of any inert gas, or it can be still more rapidly accomplished by drying in a vacuum. A tube provided with a number of small branch-tubes, each of 76 SUGAR ANALYSIS. 77 which can be closed independently by means of a stop- cock, is put into connection with a vacuum-pump. The samples of sugar in which the moisture is to be deter- mined, are weighed into metal dishes provided with a cover and of known weight, and these dishes, after being placed on a steaming water-bath, are connected with the branch-tubes and the air exhausted. Entire dessication is accomplished in from half an hour to one hour's time. A method for determining approximately the amount of water in a sample of syrup, liquor, or sweet- water, is to take the Brix hydrometer reading of the solution, and to subtract this from 100. The difference is accepted as representing the water. Example. Density of syrup in degrees Brix, 75.0. 100 Less 75 25 per cent of water. Ash. SCHEIBLEK'S METHOD. Weigh out 2.5 to 5 grammes of sample into a platinum ash-dish. Moisten with eight to ten drops of chemically pure cone, sulphuric acid, or better, with sixteen to twenty drops of dilute sulphuric acid (1 : 1). Pour a little ether over the con- tents of the dish and ignite. This treatment yields a porous carbonized mass, and avoids in a great measure the danger of loss by the assay mounting and creeping over the sides of the dish. When all gases have burned off, place in a platinum muffle, or in a Russia sheet-iron muffle (the metal should be about -^ inch in thickness), and keep the muffle at a dull-red heat until the sample has been turned completely to ash ; cool and weigh. 78 SUGAR ANALYSIS. As the addition of sulphuric acid has converted a num- ber of the salts present in the sugar into sulphates, 10 per cent is deducted from the weight of the ash found in order to make the results obtained by this method harmonize with those obtained by the method of carbonization. Example. Used 2.5 grammes of sugar. Weight of dish + ash, . . 13.9030 " 13.8490 Ash, 0.0540 Subtract 10 per cent, . . 0.0054 Total ash, 0.0486 Total ash, 1.944 per cent. This subtraction of one tenth of the weight of the ash is generally assumed to answer for beet-sugars, but is entirely misleading where cane-products are analyzed, be- cause the ash of the latter possess a composition entirely different from the ash of the former.* At present, however, the subtraction of one tenth is still the general practice. That unreliable results are obtained by this method of incineration with sulphuric acid and the subsequent subtraction of one tenth from the weight of the sulphated ash, even when beet-sugars are analyzed, has been re- cently admitted by European chemists of note.f Von Lippmann J advocates taking the dried-out sample, on which the water determination has been made, saturating it with vaselin-oil (having a boiling-point of about 400), * The Author, "Ash Determinations in Raw Sugars," School of Mines Quarterly, vol. xi. No. 1. t Die Deutsche Zucker-Industrie, 1890, March 14, No. 11. Beilage 1, p. 337. \ Loc. cit. SUGAR ANALYSIS. 79 and igniting the mixture. The carbonized mass is then to be burned to ash in a mixed current of air and oxygen. METHOD or CARBONIZATION. Weigh out 2.5 to 5.0 grammes of the sample. Carbonize at a low heat. Ex- tract the soluble salts from the carbonaceous mass with boiling water ; ignite the residue. Add the ash obtained to the aqueous extract and evaporate to dryness. Moisten with ammonium carbonate, drive off all ammonia, cool, weigh, and report as carbonate ash. Quantitative Analysis of Sugar- Ash. Dissolve 10 grammes of the sugar in hot water and filter ; * wash the residue thoroughly with boiling water and evaporate the filtrate and the washings to dryness. Carefully carbonize the mass, and then extract the same with boiling water until nitrate of silver no longer gives the reaction for chlorine. Evaporate the solution to small bulk. The residue must be dried, ignited, and weighed. This weight is noted as, insoluble ash. The solution and the ash ob- tained are then combined, hydrochloric acid is added, and the solution evaporated to diyness. All the chlorine is then driven off, the residue is taken up with water and a little hydrochloric acid, and filtered. The insoluble residue in the filter is thoroughly washed, and the wash- ings are added to the filtrate. This residue is silica. To the filtrate ammonic hydrate is added, and the solution is boiled and filtered ; the residue, iron and alumina, must be thoroughly washed, and the washings added to the filtrate. * This should be done in every case so as to have all the analyses made under the same conditions; in most instances it will be imperative, for the inorganic suspended impurities (sand, clay, etc.) in a sample of cane-sugar often weigh more than the total sugar-ash. 80 SUGAR ANALYSIS. To tills ammonium oxalate is added, and the whole is evaporated to diyness. The ammonia is burned off, and the oxalates are changed to carbonates by adding a little ammonium carbonate, and again driving off the ammonia. The mass is then taken up with water, filtered, washed, and the washings added to the filtrate. The residue con- sists of the carbonates of calcium, and magnesium. The o filtrate is evaporated to small bulk, ammonium carbonate is added, and the evaporation is then continued to diyness, the ammonia is cautiously driven off, and the residue weighed. This gives the alkalies in the form of carbonates, and this weight added to the weight of the insoluble ash previously determined, represents the total carbonate ash. Suspended Impurities. It is often necessary to de- termine the share of work done in filtration respectively by the bag-filters and the bone-black. The former, of course, remove only the mechanically suspended impurities, 'or at least the greater part of them, and leave to the bone-black the rest of the work to be accomplished. The suspended impurities are both mineral and or- ganic; their determination is effected in the following manner : Dissolve from 2.5 to 10 grammes of the sample in hot water. Pour on a filter-paper which has previously been dried and weighed between watch-glasses, and wash with boiling water until all of the sugar has been removed. This is most conveniently done by the aid of a vacuum- pump. Then dry filter and contents to constant weight, and weigh as before between watch-glasses. The increase in weight over the previous weight, represents the total suspended impurities. Ignite the filter and contents in a SUGAR ANALYSIS. 81 platinum crucible, and record the weight of the ash as mineral or inorganic suspended impurities ; the difference between the total suspended impurities and this figure gives the organic suspended impurities. An ash determination made as previously described represents the mineral matter contained in the sugar, in the form of salts, etc., as well as the mineral matter mechanically suspended, and which latter, the bag-filters are supposed to remove. The inorganic suspended impurities when subtracted from the total ash show the "soluble" ash, the more or less complete removal of which is expected of the bone- black. Example. Use<^ 2.5 grammes of raw sugar. Weight of watch-glasses + filter -|- total sus- pended impurities, . . 22.5071 Weight of watch-glasses + filter, .* . . ! 22.5000 Total suspended impurities, . 0.0071 Weight of crucible + ash of filter + inor- ganic suspended impurities, .... 13.20020 Weight of crucible, 13.20000 Ash of filter + inorganic susp. impurities, . 0.00020 Ash of filter, .... 0.00008 Inorganic susp. impurities, . 0.00012 Total suspended impurities, 0.00710 = 0.2840 per cent. Inorganic " " 0.00012 = 0.0048 it U Organic " " 0.00698 = 0.2792 a a 82 SUGAR ANALYSIS. Total ash (previously determined), . 0.5040 per cent. Inorganic suspended impurities, . . 0.0048 " " Soluble ash, . 0.4992 Determination of Woody Fibre. About 20 to 25 grammes of the sample, in as finely divided a state as possible, are placed in a flask or beaker, into which cold water is poured. The water, after having been in con- tact with the chips or shavings from 20 to 30 minutes, is decanted carefully, in order to avoid any loss of the weighed sample. This treatment with cold water is re- peated two or three times, and is then followed by a similar treatment with hot water; finally, the sample is boiled several times, fresh water being taken for each treatment, and the treatment continued until all the sol- uble material has been washed out. Sometimes this is followed by washings with alcohol and ether. . The sample is then transferred to a weighed filter, preferably made of asbestos, and gradually dried to con- stant weight. If dried in the air-bath, a temperature of 110 C. should not be exceeded. If the sample can be dried in vacuo, and subsequently weighed in a covered dish" or capsule, all danger of oxidation and absorption of moisture are avoided. The increase in weight which is noted in the filter, of course represents the woody fibre. Detection of the Sugar-Mite. To detect the sugar- mite (Acarus sacchari) iu raw sugars, dissolve the sample in warm water ; the mite will cling to the sides or to the bottom of the vessel. Drain off the solution and identify by means of a microscope.* * For drawings, see Hassall, " Food and its Adulterations." CHAPTER VII. ORGANIC NON-SUGAR. IN regular technical analyses the organic matter not sugar, raffinose, or invert-sugar is not determined. It is assumed to be represented by the difference between 100 and the constituents determined, viz., sucrose, raffi- nose, invert-sugar, water, and ash. This difference is fre- quently recorded as "non-ascertained," or " undeter- mined matter." There are several methods for the direct determina- tion of this organic matter, but the results which they yield are of. value chiefly for comparative purposes. The following method is perhaps the most satisfactory: Dissolve 10 to 20 grammes of raw sugar in warm water. Add basic acetate of lead solution in excess. Warm for a short time and filter. Wash the precipitate thoroughly ; then suspend it in water and pass in sulphu- retted hydrogen until all the lead is precipitated as sul- phide. Filter out the sulphide of lead, wash thoroughly, and evaporate the filtrate and washings to dryness (con- stant weight), in a dish previously -weighed. The tem- perature at which the drying is done, must not exceed 100 C. Example. Used 10 grammes of raw sugar. Weight of dish and organic matter, .... 17.0973 < dish, . . . . 17.0482 Organic matter, . 0.0491 Organic matter = 0.491 per cent. o a 84 SUGAR ANALYSIS. The organic bodies accompanying sucrose can be divided into three classes : 1. Organic acids, or bodies that can act as acids. 2. Nitrogenous substances. 3. Non-nitrogenous substances. These classes embrace respectively the following bodies : ORGANIC ACIDS.* Adetic, , C H Melassic, . . . C H (?) Aconitic, . . oXo. 1 Metapectic, . . cXV Apoglucic, A spar tic, . . C 18 H 10 0, . C 4 H,N0 4 Oxalic, .... Oxycitric, . . . C 2 6 HX Butyric, . . C 4 H 8 0, Parapectic, . . . C 24 H 30 21 Citric, . . . C.H.O, Pectic, .... C,,H,,0 13 Formic, . CH,0 2 Propionic, . . . C H Succinic, c'nX Glutamic, . . . OH.NO. Tartaric, . . . CHO Lactic, . . . Malic, . . . C 3 H,0 3 . C H Tricarballylic, . - Ulmic, .... 0H,0 6 o.X.6. Malonic, . . 4 65 C S H 4 0. 24 18 9 NITROGENOUS SUBSTANCES. Albumin, . . Ammonia, . . : c ^^^ i:t!i*jyfji5^ RI -? ota v^-"i3-^ _ , .JT ^-5So2^ o -w -S Sx cc- *j liKtriltf32 5 18 SCHEME II. BABE NON-VOLATILE ACIDS. UFIVBESIT7 90 SUGAR ANALYSIS. SCHEME II. Rare Non- Volatile Acids. Dissolve 20 grammes of the sample ; precipitate by neutral acetate of lead, place on a filter, and wash with boiled distilled water until the washings no longer contain lead. Precipitate. It contains the lead salts Filtrate 1. Add an excess of acetate of lead in solution, filter, and wash the pre- of the organic acids, as well Precipitate. Filtrate 3. as the sulphate and phosphate of lead ; small quantities o f parapectin may also be found in the lead precipi- Suspend in water, pass sul- phuretted hydrogen in excess, and filter out the sulphide of lead. From the filtrate re- move the sulphuretted hydro- gen by boiling, add alcohol and a few cubic centimetres of acetic acid. Filter. This contains aspartic and metapeetic acids. Add several cubic centimetres of an ammoniacal solution of acetate of lead leave at rest for 12 hours, filter, wash, de- compose by sulphuretted hydrogen, and filter out the sulphide of lead. Evaporate the filtrate to small bulk; add an equal volume of nitric acid (sp. gr. 1.42), and heat tate (Pectin for a quarter of an hour Aspartic acid is precipitated only by basic acetate of Precipi- tate. Filtrate. remains unchanged ; metapeetic acid is decomposed into oxalic acid, which goes into solution, and into mucic acid which lead.) For the separation of Pectin and para- This may contain small quantities of crystallizes on cooling. Filter. these sub- stances see col- pectin. These sub- glucic, malic, and succinic acids Crystals. Mother Liquor. umn 2. s tanc e s which were not The washed This contains aspar- may be completely pre- crystals of mucic tic and oxalic acids s e p arated cipitated by neu- acid are boiled produced by the fore- in the same tral acetate of 5ead. with nitric acid; going decomposition. manner as Besides these there the mucic acid is Pass a current of N 2 O 3 . legumin. may be present decomposed Nitrogen is set free, To effect traces of aspartic completely into and at the same time this, acidify and of metapeetic oxalic and tar- malic acid is formed strongly acids, which may taric acids, the (at the expense of the with acetic be identified after identification of aspartic acid). This acid, boil, the precipitation of which .proves the is searched for as and filter the former acids. presence origi- directed in Scheme I. out the co- by nitrate of cal- nally of mucic The identification of agulum. cium and alcohol. acid. malic acid proves the (See the following existence of aspartic column.) acid in the original solution. SCHEME III. VOLATILE ACIDS. SUGAR ANALYSIS. SCHEME! III. Volatile Acids. 20 to 100 grammes of the sample (syrups, etc., are brought to 20 Baum6) are rendered strongly acid by dilute sulphuric acid. All the chlorine of the metallic chlorides is pre- cipitated with a standardized sulphate of silver solution, and the precipitate of argentic chloride is filtered out. The liquid is distilled as long as acid vapors pass over, the dis- tillate is exactly saturated with a solution of barium hydrate, and any excess of this reagent which might have been added, is removed by a stream of carbonic-acid gas. The liquid is concentrated, the barium carbonate filtered out, and the filtrate evaporated to dryness at 110 C. in a platinum capsule. Residue of Distilla- Distillate. tion. Contains nearly the whole of lactic acid, only traces having passed over into the distillate. Add three volumes of alcohol and distil the mixture with milk of lime. Filter the boiling solution to separate the hydrate and sulphate of calcium. In this filtrate the lime is precipitated by a stream of carbonic-acid gas. Evaporate to dry- ness, take up the residue with strong alcohol, filter again, and let the filtrate stand. If lactic acid is present, crystals of calcium lactate are formed, which are re- cognized by their charac- teristic structure. The dried barium salts obtained from the distillate are ex- tracted with boiling alcohol of 88 per cent, the operation being repeated several times, and the residue remaining undis- solved, is filtered out. Residue. Formate and nitrate of barium. Traces of acetate of barium. Dis- solve in a little water, and precipitate the barium with sulphate of sodium. Filter, and mix a portion of the filtrate with argentic nitrate. Citrate of sil- ver, which is precipi- tated, is reduced by heating to a mirror of metallic silver. In an- other portion of the solution test for formic acid by the reduction of mercuric to mercur- ous chloride. Solution. Acetate, propionate, and butyrate of barium. Evaporate to small bulk, take up with a little water, precipitate the barium with sulphuric acid, filter out the precipitate, and divide the fil- trate into two equal parts. Neutral- ize one portion with sodium hydrate, and then add this to the other portion. Subject the whole to distillation. Distillate. Butyric and propionic acids. They are identi- fied by their odor, and the oily drops which are formed in decomposing their salts by sul- phuric acid. Residue. Acetic acid. Iden- tified by its odor, and by the forma- tion of acetic ether, produced on warm- ing one of its salts with sulphuric acid and alcohol. SCHEME IV. APPROXIMATE DETERMINATION OF ORGANIC ACIDS: NON-VOLATILE AND VOLATILE. SUGAR ANALYSIS. SCHEME IV. Approximate Determination of Organic Acids, Non- Volatile and Volatile. Non-volatile Acids. Volatile Acids. A. Precipitation by neutral acetate of lead. B. Precipita- tion by basic C. Precipita- tion by ammo- D. Not precipitated by acetate of lead: formic, Oxalic, citric, tartaric, and acetate of lead. niacal acetate acetic, lactic, propiouic, malic acids. Incompletely: Pectic, para- of lead. As- and butyric acids. pectic, parapectic, glucic, pectic, glucic, partic and met- melassinic, ulmic, and suc- cinic acids. mic, and succi- apec ic aci s. nic acids. Par- 50 grammes of the sam- 50 grammes of the sample are dissolved in distilled apectin. In- completely: as- The filtrate ple to be examined (in case of juices a larger water and made slightly acid partic and met- obtained from amount must be taken; with acetic acid. The solu- apectic acids, the precipita- thick syrup must be di- tion is boiled to expel the car- bonic acid, and neutralized and pectin. tion with basic acetate of lead luted), are strongly acidi- fied with dilute sulphuric with sodium hydrate (free is mixed with acid. All the chlorine from carbonic acid). A ' several cubic which has been previously slight excess of neutral ace- To the filtrate centimetres of determined volumetrically tate of lead is added, and ; from the lead an ammoniacal in a separate sample, is digested for one hour. The salts precipita- acetate of lead precipitated by a stand- residue is placed on a dry i ted by neutral solution. Al- ardized sulphate of silver and weighed filter, and is j acetate of lead, low to stand for solution. The filtrate from washed with boiled distilled there is added twelve hours. the argentic chloride is water until tlie washings give a slight excess Filter, allow to distilled until acid fumes no longer the reaction for of basic acetate drain off, and no longer pass over. This lead. (For treatment of the of lead, and the wash once with distillate is then mixed filtrate, see B.) \ precipitate fil- distilled water with a solution of barium The precipitate contains tered out. (For to which a lit- hydrate, any excess of the lead salts of the above- filtrate, see C.) tle ammoniacal this reagent is precipitated named acids, and besides The precipi- acetate of lead by carbonic acid, and the sulphate and phosphate of ; tate is placed has been add- solution filtered. The fil- lead, if the sample examined on a dried and ed. The pre- trate is evaporated to dry- contained sulphates and weighed filter, cipitate, dried ness at 110 C. in a weighed phosphates. The filter .with then washed, and weighed, is platinum capsule: the its contents is dried at 110 dried at 110 C., treated as de- residue represents the C., and weighed. The pre- and weighed. scribed under weight of the organic cipitate is removed, the filter A part is incin- A and B. acid salts of barium, which is burned in a weighed plati- erated as in A, Xote. The are determined as sul- num crucible, the precipi- and the weight am m o n i a c a 1 phates or carbonates. tate is again added, and of the organic acetate of lead If nitrates were present heated to dull redness. acids determin- must be added in the sample analyzed, To facilitate the combus- ! ed by differ- only gradually the residue contains also tion of the tfarbon, small ence. as there and in small barium nitrate. In that doses of ammonium nitrate described. amounts, for case the nitric acid must are repeatedly added, great without this be determined, the weight care being taken to prevent precaution it is of the barium nitrate cal- loss bv spitting. After cool- apt to precipi- culated from the result, ing, the crucible is weighed. tate sugar, and and this value subtracted The wt ight of the contents then even an from the weight of the of the crucible subtracted approxima te organic acid salts of ba- from that of the precipitate determinat i o n rium previously found. dried at 110 C. represents of the acids the weight of the organic sought for, be- acids, because the sulphate comes very dif- and phosphate of lead are ficult. not altered by the ignition. SUGAR ANALYSIS. 95 Determination of Total Nitrogen.* An amount of the substance, varying from 0.7 to 2.8 grammes, according to its proportion of nitrogen, is placed in a digestion-flask with approximately 0.7 gramme of mercuric oxide and 20 cubic centimetres of sulphuric acid, t The flask is placed in an inclined position, and heated below the boiling-point of the acid, from five to fifteen minutes, or until frothing has ceased. The heat is then raised until the acid boils briskly, and this boiling is con- tinued until the contents of the flask have become a clear liquid, colorless, or of a very pale straw color. While still hot, finely pulverized potassium perman- ganate is introduced carefully and in small quantity at a time, till, after shaking, the liquid remains of a green or purple color. After cooling, the contents of the flask are transferred to the distilling-flask, with about 200 cubic centimetres of water ; to this a few pieces of granulated zinc and 25 cubic centimetres of potassium-sulphide solution t are added, shaking the flask to mix its contents. Sufficient of a sodium hydrate solution is then added to make the reaction strongly alkaline. This reagent should be poured down the sides of the flask, so that it does not mix at once with the acid solution. The flask is then connected with the condenser, and its contents are distilled until all ammonia has passed * The Kjeldahl method. Abstracted from Bulletin No. 19, U. S. Depart- ment of Agriculture. t C. P. acid, specific gravity 1.83, free from nitrates and ammonium sulphate. I Prepared by dissolving 40 grammes of commercial potassium sulphide in 1 litre of water. A saturated solution of sodium hydrate, free from nitrates. 96 SUGAR ANALYSIS. over into standard hydrochloric acid. * The distillate is then titrated with standard ammonia. Previous to use, the reagents should be tested by a blank experiment with sugar, which will partially reduce any nitrates that are present, and which might otherwise escape notice. If the nitrogen present in organic combination is to be ascertained, the nitrogen present in the form of nitric acid and in the form of ammonia must be separately determined, and their sum subtracted from the total nitrogen found ; the remainder is the nitrogen in or- ganic combination. Non-Nitrogenous Organic Substances. The determi- nation of non-nitrogenous organic substances is effected by aid of basic and neutral acetate of lead and alcohol (pectin and parapectin), by the successive use of water, alkalies, acids, alcohol, and ether (cellulose), by treat- ment with ether (fats, essential oils), by the aid of yeast fermentation, and alcohol (isolation of mannite).t Determination of Pure Cellulose.! To make this de- termination, place 10 grammes of the sample, 30 to 40 grammes of pure potassium hydrate, and about 30 to 40 c.c. of water into a glass retort. Close the retort by a glass stopper, place in an oil-bath, provided with a thermo- meter, and heat up gradually. At about 140 C. the solution will commence to boil and foam 'considerably. Increase the temperature to about 180, and continue heating for about one hour. When the contents of the * Half-normal acid, 18.25 grammes HC1 to the litre. t For details of these determinations see Zeitschrift des Vereines fur Elibenzucker-Indnstrie, 1879, vol. xxix. p. 906. \ Method of G. Lange. Chemisches Repertorium, 1890, vol. xiv., No. 3, p. 30. SUGAR ANALYSIS. 97 retort cease foaming, become quiet, and begin to turn dry, the end of the reaction has been reached. Remove the retort from the oil-bath, and after cool- ing to about 80, add hot water and rinse the contents of the retort carefully first with hot and then with cold water, into a beaker. After cooling, acidify with dilute sulphuric acid ; this acid will precipitate the particles of cellulose which have been kept in suspension in the strong alkaline solution. Then, with very dilute sodium, hydrate, produce anew a faintly alkaline reaction, so that all of the precipitated substances, excepting the cellulose, may be again brought into solution. The residue is then transferred to a weighed filtering tube provided with a finely perforated platinum cone and washed out thoroughly, first with hot water, and then with cold. Drying is effected on a water-bath, and the filter with its contents weighed. The residue is then removed from the filter, ignited, and the weight of the ash found subtracted from the value previously obtained. The difference in weight represents pure cellulose. CHAPTER VIII. NOTES ON THE REPORTING OF SUGAR-ANALYSES, DETERMI- NATION AND CALCULATION OF THE RENDEMENT, ETC. IN commercial analyses it is customary to report only- Polarization, Invert-sugar, "Water, Ash, Non-ascertained, the " non-ascertained " being the balance required to make the analysis figure up to 100. When beet-sugars are examined, and a raffinose deter- mination has been made, this substance, of course, makes another item in the report, which would then embrace : Polarization, Sucrose, Raffinose, Invert-sugar, Water, Ash, Non-ascertained. The polarization in the first form of analysis given above, may either correspond to, be greater, or smaller than the amount of sucrose really present, for the presence of other optically-active bodies influences the polariscope- reading to a marked degree. SUGAR ANALYSIS. 99 Invert-sugar turns the plane of polarized light to the left. At 17.5 C. one part of invert-sugar neutralizes the optical effect of 0.34 parts of sucrose. In order, therefore, to obtain the sucrose corrected for this disturbing influ- ence, the amount of invert-sugar found is multiplied by 0.34, and the result is added to the direct polarization. This sum is then regarded as representing the sucrose. Frequently a polarization after inversion is made, and compared with the direct polarization. If there are no other optically active bodies present in the sample besides the sucrose, the result of the polari- zations before and after inversion will be identical, or at least agree very closely. If the polarization after inver- sion is higher than the direct polarization, the presence of laevo-rotary bodies is indicated ; if it is lower, dextro- rotatory substances are present. Recent investigations have, however, shown that this method of inversion and subsequent polarization (Cler- get's test) is not applicable to sugars rich in reducing sugars (so-called invert-sugar), because the inverting acid (hydrochloric acid) increases the Isevo-rotation of the invert-sugar,* and because the reducing sugar sometimes consists of a mixture of laevo- and of dextro-rotatory sub- stances in varying proportions. In dealing with samples of such description, as, for instance, low sugars and molasses, sugar-cane products, an exhaustive analysis is desirable, in order to gain all information possible with regard to the nature of the sample. * Jungfleisch and Grimbert, Report to the French Academy of Sci- ences, December, 1889. 100 SUGAR ANALYSIS. Such an analysis should record- Reaction (acid, alkaline, or neutral), Total sucrose, Polarization after inversion, Direct polarization, Total reducing sugars, Water, Ash. The interpretation of an analysis of this description is not always an easy matter. If the polarization after inversion agrees with the direct polarization plus 0.34 times the total reducing sugar, this value may be regarded as the amount of sucrose (crystallizable sugar) present. As, however, all results obtained by the Clerget method on sugars rich in invert-sugar are open to doubt, it will be better, even in case the direct polarization plus 0.34 times the total re- ducing sugar is equal to the polarization after inversion, to resort to gravimetric determinations for verification of the result. In case of non-agreement of the direct polarization plus 0.34 times the total reducing sugar, and the Clerget test, of course gravimetric analysis must be employed. Determine the total sucrose, after inversion, by its reducing action on copper solution, and in a similar man- ner determine also the total reducing sugar. Calculate the latter over to its equivalent of sucrose by subtracting one twentieth of the amount found; deduct this result from the total sucrose, and report the remainder as sucrose. SUGAR ANALYSIS. 101 Example. Polarization before inversion, . . . 52.70 Polarization after inversion, . . . 63.12 Total reducing sugar, . . . . . . 22.89 Total sucrose (gravimetric det.), . . 79.20 22.89 Total sucrose, 79.20 L . 1.14 Less . . 21.75 21.75 Sucrose = 57.45 Concerning the nature of the reducing sugar, this may be present as a. Optically Inactive Sugar. The existence of a sugar that will reduce copper solution, but which is inactive to polarized light, is, at best, doubtful. But it might happen that'the Isevo-rotatory power of the invert- sugar is just neutralized by the dextro-rotatory influence of some other substance raffinose or dextrose, for in- stance.* In either case the direct polarization and the polarization after inversion would agree. b. Invert-Sugar. In this case, barring the danger of an increased Isevo-rotation by the inverting acid, the polarization after inversion will be equal to the sum of the direct polarization plus 0.34 times the reducing sugar. c. Dextrose (Glucose). In this case the polarization after inversion is equal to the direct polarization minus the reducing sugar multiplied by a factor. This factor has been given as 0.8. This seems, however, to be cor- rect only when the dextrose, which is a bi-rotatory sub- stance, has reached its lowest rotatory value, for experi- ments made by the author on mixtures of anhydrous crystallized dextrose and raw sugars of various grades, * Borntrager, Deutsche Zuckermdustrie 1890, p. 277, claims, that owing to bi-rotation of the dextrose of the anhydrous invert-sugar, the laevo-ro- tation, of the laevulose is temporarily neutralized. 102 m SUGAR ANALYSIS. gave values that fluctuated considerably from the factor quoted. d. Mixture of Invert-Sugar and Dextrose, or Invert- Sugar and Lcevulose, in varying proportions : In this case only an analysis of the reducing sugar (see page 61) will permit a conclusion as to its* compo- sition. In all cases a gravimetric determination of the invert-sugar, the dextrose, or laevulose will afford a valu- able check on any inferences that may be drawn from the data obtained by optical analysis. If a cane-juice has been analyzed, the report should embrace the following determinations : * 1. Density expressed as specific gravity, or in degrees, of Bauine or Brix. 2. Total solids. 3. Sucrose. 4. Reducing sugar (glucose). 5. Solids not sugar. 6. Coefficient of purity. 7. Glucose ratio. No. 5 is equal to No. 2, less No. 3 + No. 4. No. 6 is found by multiplying No. 3 by 100, and dividing by No. 2. No. 7 is obtained by multiplying No. 4 by 100, and dividing by No. 3. The percentage of extraction is obtained by dividing the weight of juice obtained by weight of cane used, and multiplying by 100. Rendement. The yield in crystallizable sugar can be analytically determined by the Payen-Scheibler method. This process is based on the treatment of the raw * Scheme adopted by the Louisiana Sugar Association. SUGAR ANALYSIS. 103 sugar, whose rendement is to be ascertained, by solutions that will wash out the molasses-forming impurities, and leave behind the pure crystallizable sugar. Five solutions are required : No. 1 is a mixture in equal parts, by volume, of abso- lute alcohol and ether. No. 2 is absolute alcohol. No. 3 is alcohol of 96 per cent Tralles.* No. 4 is alcohol of 92 per cent Tralles. No. 5 is alcohol of 85 per cent to 86 per cent Tralles, to which 50 c.c. of acetic acid per litre have been added. Solutions Nos. 3, 4, and 5 are all saturated with pure sugar; and, in order that they should remain saturated with sugar at all temperatures, they are kept in flasks which are half filled with best granulated sugar, pre- viously washed with absolute alcohol. These fiasks are provided with a siphon arrangement ; the air enters through chloride-of-calcium tubes, so as to be thoroughly dried; the solution is discharged through tubes filled with pure and dry sugar. Plugs of felt placed at the ends of these tubes prevent the carrying over of any sugar particles. The w r ashing operation is carried out as follows : The accurately weighed sample, usually 13.024 grammes, is placed into a 50 c.c. flask which has previously been dried. A cork or a rubber stopper, through which two glass tubes are made to pass, serves to close the flask. One of these tubes reaches down almost to the bottom of the flask ; it is provided with a felt-plug at its mouth ; this * The alcoholometer of Tralles gives the percentage volume for the temperature of 60 F. = 15| C. Watt's Dictionary of Chemistry, vol. i. p. 84. 104 SUGAR ANALYSIS. serves as strainer. The shorter tube only reaches to just below the cork or stopper. The longer tube is connected, by means of a rubber tube, with a large receiving bottle, from which the air is to a great extent exhausted by an aspirator or a vacuum pump. The rubber tube is pro- vided with a pinch-cock, so that connection can be made or broken at will, between the receiving bottle and the small flask which holds the sample. The apparatus being thus arranged, about 30 c.c. of solution No. 1 is allowed to flow into the flask containing the sugar. This solution is permitted to remain quietly in contact w^ith the sample for from fifteen to twenty minutes, and is then drawn over into the receiving bottle. When it has all been drained over, 30 c.c. of solution No. 2 are introduced. After a contact of two minutes this solution is drawn off, and followed successively by about the same amounts of the other three solutions, in the order of their numbering. The last of these, solution No. 5, is really the active reagent, the others principally serving to displace the moisture contained in the sugar. This solution is allowed to remain on the sample for half an hour, being frequently and well shaken in the mean time to insure intimate contact. It is then drawn off, and replaced by a fresh supply of the same solution. This in turn is drawn off, and the treatment is repeated with fresh amounts of solution No. 5, until the solution standing above the sugar, remains per- fectly colorless. The time of contact is thirty minutes for each treatment. The last traces of the solution No. 5 are then removed by successive addition of solutions Nos. 4, 3, and 2, in the SUGAR ANALYSIS. 105 order named. These are added and drawn off at inter- vals of two minutes each. The last traces of alcohol are re- moved by drying on a water-bath, a current of dry air being continuously drawn through the flask in the mean time. When the sample is perfectly dry, the cork with its inserted tubes is carefully withdrawn, and any sugar clinging to the long tube or its felt plug, is carefully washed into the flask. The solution is then made up to 50 c.c. and polarized. The reading on the polariscope represents in percentage the yield in crystallizable sugar. Calculation of Rendement UNITED STATES OF AMERICA. From the polarization (the crystallizable) subtract five times the ash, for sugars of all grades. If the sugars are products of the beet, then, in addi- tion to the above, subtract for 1st Products: Three times the invert-sugar (non- cry stallizable), if it does not exceed one quarter per cent ; five times the invert sugar (non-cry stallizable), if it ex- ceeds one quarter per cent. 2d Products: Three times the invert-sugar (non-crys- tallizable), if it does not exceed one half per cent ; five times the invert-sugar (non-crystallizable), if it exceeds one half per cent. 'ENGLAND.* Beet-Sugars. 1st. Products. Basis, 88 p. c. From the crystallizable sugar deduct five times the ash and three times the non-crystallizable, provided the latter does not exceed one quarter per cent. If it ex- ceeds this amount, then subtract five times the non- crystallizable. Lower Products. JBasis, 75 p. c. From the crystal- * Liste Generate des Fabriques de Sucre. Paris, 1889. 106 SUGAR ANALYSIS. lizable, deduct five times the ash and three times the non- crystallizable, provided it does not exceed one half per cent. If it exceeds this limit, deduct five times the non-crystallizable. FRANCE. * Beet-Sugars. From the crystallizable sugar subtract four times the ash and twice the non-crys- tallizable, which must not exceed one quarter per cent. From this rendement, figured without fractions of a de- gree, subtract one and one half per cent. GERMANY. From the crystallizable sugar r (as deter- mined by the polariscope), subtract five times the salts, i.e., the ash less the suspended impurities, and twice the invert-sugar. Duty The duty levied by the United States Gov- ernment is based on the polariscope test and on color. For the color-test the "Dutch standards" (see page 25) have been adopted as the guide. In testing by the polariscope every fraction over a full degree is figured as if the next whole degree had been indicated. Thus, a sugar testing 94.0 degrees on the polariscope pays the duty prescribed for this grade, but a sugar testing 94.1 is classed as a 95.0 sugar. The following is quoted from the existing law (March, 1890): "All sugars not above No. 13 Dutch standard in color, . . . testing by the polariscope not above 75, shall pay a duty of 1^- cent per pound, and for every addi- tional degree, or fraction of a degree, shown by the polari- scope test, they shall pay y^ of a cent per pound addi- tional. * Liste GenSrale des Fabriques de Sucre. Paris, 1889. SUGAR ANALYSIS. 107 "All sugars above No. 13 Dutch standard shall be classified by the Dutch standard of color, and shall pay duty as follows, namely: All sugar above No. 13 and not above No. 16, 2 f cents per pound ; all above No. 16 and not above No. 20, 3 cents; all above No. 20, 3| cents." Calculation of the Weight of Solids and Liquids from their Specific Gravity. One cubic foot of distilled water weighs 62.50 Ibs. = 1000 ounces. The specific gravity of water is 1.000. If the decimal point of a specific- gravity value be moved three places to the right, the weight of a cubic foot in ounces will be obtained. This value divided by 16 gives the weight of a cubic foot in pounds. From this the following rule is deduced : To find the weight in pounds per cubic foot : Determine the specific gravity. Remove the decimal point three places to the right, and divide by 16. Example. Specific gravity of a bone-black is 0.87904. 879.04 -4-16 = 54,94. Hence the bone-black weighs 54.94 Ibs. per cubic foot. As above stated, if the decimal point of a specific- gravity value is removed three places to the right, the weight of a cubic foot in ounces will be obtained, and this figure divided by 16 will give the weight of a cubic foot in pounds. But if the cubic foot be assumed equal to 7.5 gallons, 7.5 X 16 = 120. Therefore, To find the weight of a gallon in pounds : Determine the specific gravity. Remove the decimal point three places to the right, and divide by 120. Example. A syrup has a specific gravity of 1.413. 1413^-120 = 11.78. Hence the syrup weighs 11.78 Ibs. per gallon. CHAPTER IX. SYNONYMS LITERATURE ON SUGAR ANALYSIS TABLES. SYNONYMS. English. German. French. Cane-sugar Eohrzucker Sucre de Canne Saccharose Saccharose Saccharose Sucrose Sucrose Sucrose Common sugar Crystallizable sugar Saccharobiose Sucre-normal Sucre Diglucosic alcohol Saccharon Cannose Dextrose Dextrose Glucose Glucose Glycose Glycose Glycose Fruit sugar Honey sugar Honigzucker Diabetic sugar Uric sugar Harnzucker Eag sugar Potato-sugar Eight-handed sugar Grape sugar Traubenzucker Sucre de Eaisin Starch sugar Starkezucker Dextro-glucose Krumelzucker Sucro -glucose Levulose (laevulose) Lavulose Levulose Fruit sugar Fruchtzucker Left-handed glucose Linksfruchtzucker Laevo-glucose Sucro-glucose Syrupzucker Schleimzucker Honigzucker Chylariose Chyliarose 108 SUGAR ANALYSIS. SYNONYMS. Continued. 109 English. Invert-sugar German. Invertzucker French. Sucre invert! Sucre interverti Raffinose Melitose Plus-sugar Raffinose Melitose Melitriose Pluszucker Gossypose Baumwollzucker Raffinotriose Raffinoliexose Raffinose Melitose REFERENCES TO LITERATURE ON SUQAR ANALYSIS. BOOKS AND PERIODICALS. 1839 PELIGOT, E. Analyse et Composition de la Betterave a Sucre. 1840 PELIGOT, E. Composition chimique de la Canne a Sucre. 1848 *BACHE, A. D v AND MCCULLOUGH, E. S. Keport on Sugar and Hydrometers. 1863 FRESE, 0. Beitriige zur Zuckerfabrikation. 1865 ICERY, E. Recherches sur les Jus de la Canne a Sucre. 1867 *MANDELBLUH> C. Leitfaden zur Untersuchung der ver- schiedenen Zuckerarten, sowie der in der Zuckerfabrikation vorkommenden Produkte. 1867 MOXIER, E. Guide pour PEssai et 1' Analyse des Sucres. 1868 *VIOLETTE, C. Dosage du Sucre an Moyen des Liqueurs titrees. 1869 MOIGXO, L'ABBE. Saccharometrie optique, chimique et melassimetrique. 187-i Possoz, L. Notice sur la Saccharometrie chimique. 1875 GUNNING, J. W. La Saccharometrie et Tlmpot sur le Sucre. 1875 TERREIL, M. A. Notions pratiques sur TAnalyse chimique des Substances sacchariferes. 1875 WACKEXRODER, B. Anleitung zur cliemischen Unter- suchung technischer Produkte welche auf dem Gebiete der Zuckerfabrikation und Landwirthschaft vorkommen. 1876 MAUMEXE, E. J. Traite theorique et pratique de la Fabri- cation du Sucre. 1878 *URE'S Dictionary of Arts, Manufactures, and Mines, vol. iii.,' and Supplement (1879). Asterisks mark the publications consulted. F. G. W. 110 SUGAR ANALYSIS. Ill 1879 BARBET, E. Analyse des Liquides Sucres. 1879 *LANDOLT, H. Das optische Drehungsvermogen Organischer Substanzen und die prakfcischen Anwendungen desselben. 1880 COLLIER, P. Report of Analytical and Other Work done on Sorghum and Cornstalks. Department of Agriculture, Report No, 33. 1881 FRANKEL, J., AND HUTTER, R. A. Practical Treatise on the Manufacture of Starch, Glucose, Starch-sugar, and Dextrine. 1882 *LANDOLT, H. Handbook of the Polariscope and its Practi- cal Applications. (From the German.) 1882 *VoN LIPPMANN, E. Die Zuckerarten und ihre Derivate. 1882 *SPONS' Encyclopaedia of the Industrial Arts, Manufactures, and Raw Commercial Products, vol. ii., article: "Sugar Analysis." 1883 LE DOCTE, A. Traite complet du Controle chimique de la Fabrication du Sucre. 1883 LEPLAY, H. Chimie theorique et pratique des Industries du Sucre. 1883 *TUCKER, J. H. A Manual of Sugar Analysis, (Second Edi- tion.) 1884 *COMMERSON, E., ET LAUGIER, E. Guide pour Analyse des Matieres sucrees. (Third Edition.) 1884 *VoN WACHTEL, A. Hilfsbuch fiir chemisch-techuische Un- tersuchungen auf dem Gesammtgebiete der Zuckerfabri- kation. 1885 * ALLEN, A. H. Commercial Organic Analysis, vol. i., arti- cle: "Sugars." 1885 *FRUHLING, R., UND SCHULZ, J. Anleitung zur Unter- suchung der fiir die Zuckerindustrie in Betracht kom- menden Rohmaterialien, Producte, Nebenproducte und Hiilfssubstanzen. (Third Edition.) 1887 *Ausfuhrungs-Bestimrnungen zum Zucker-steuergesetz vom 9ten Juli, 1887. (German Government.) 1887 *SCHMIDT, F., UND HAEXSCH. Gebrauchs- Anweisung zu den Polarisations- Apparaten von Schmidt und Haensch. 1887 *STAMMER, K. Lehrbuch der Zuckerfabrikation. (Second Edition.) 1888 LOCK AND NEWLAND. Sugar: A Handbook for Planters and Refiners. SUGAR ANALYSIS. 1888 PELLET. Nouveau Precede simple, rapide et pen couteux de Dosage direct du Sucre contenue dans la Betterave, la Canne, la Bagasse, le Sorgho, etc. 1888 *SACHS, F. Revue Universelle des Progres de la Fabrication du Sucre. 1888 *ToLLEsrs, B. Kurzes Handbuch der Kohlen-hydrate. 1888 *WEIN, E. Tabellen zur quantitativen Bestimmung der Zuckerarten. 1889 *BASSET, N. Guide du Planteur de Cannes. 1889 *LEPLAY, H. Etudes chimiques sur la Formation du Sucre. 1889 *SPENCER, G. L. A Handbook for Sugar Manufacturers and their Chemists. PERIODICALS. *The American Chemist (1870-1877). *The Louisiana Planter and Sugar Manufacturer. America. Weekly. Sugar Bowl and Farm Journal. America. Weekly. The Sugar Beet. America. Monthly. *Sugar Cane. England. Monthly. Sugar. England. Monthly. The Journal of the Society of Chemical Industry. England. Monthly. *Chemiker Zeitung. Semi-weekly. *Die Deutsche Zuckerindustrie. Weekly. *Jahresbericht iiber die Untersnchungen und Fortschritte auf dem Gesammtgebiete der Zuckerfabrikation. *Neue Zeitschrift fiir Riibenzucker-Industrie. Semi-monthly. *Oesterreichisch-Ungarische Zeitschrift fiir Zucker-Industrie und Laudwirthschaft. Six numbers per annum. Taschenkalender fiir Zuckerfabrikanten. K. Stammer. Annual. Wocheuschrift des Centralvereines fiir Riibenzucker-Industjie in der Oester: Ungar: Monarchie. *Zeitschrift des Vereines fiir die Riibenzucker-Industrie des Deutschen Reichs. Monthly. Zeitschrift fiir Zuckerindustrie in Bohmen. Ten numbers per annum. Bulletin de TAssociation Beige des Ohimistes. Monthly. * Journal des Fabricants de Sucre. France. Weekly. *La Sucrerie Indigene et Coloniale. France. Weekly. TABLES. RELATION BETWEEN SPECIFIC GRAVITY, DEGREES BRIX AND DEGREES BAUMfi, FOR PURE SUGAR SOLUTIONS FROM TO 100 PER CENT. (Temperature 17.5 C. = 63.5 F.) MATEG-CZEK AND SCHEIBLEB. o p 100 100 - (0.6813 X Degree Baume)' Degree Baume = 1.46778 X F.* 259 3 Degree Brix = 259,3 g - -v^ ^ r-. Specific Gravity * The values of F. are given in Zeitschrift des Vereines ftir Rubenzucker- Industrie, 1865, page 580; 1870, page 263; 1874, pages 843 and 950. 115 SUGAR ANALYSIS. 117 Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees "^.gaum^. 0.0 .OOOOO 0.00 4.0 .01570 2.27 O. I .00038 O.O6 4.1 .01610 2-33 0.2 .00077 O. II 4.2 .01650 2. 3 8 0-3 .00116 0.17 4.3 .01690 2.44 0.4 00155 0.23 4-4 .01730 2.50 0-5 .00193 0.28 4-5 .01770 2.55 0.6 .00232 0-34 4.6 .OlSlO 2.61 0.7 .00271 0.40 4-7 .01850 2.67 0.8 .00310 0-45 4-8 .01890 2.72 0.9 .00349 0.51 4-9 01930 2.78 .0 .00388 0-57 5-0 .01970 2.84 .1 .00427 0.63 5-i .02010 2.89 .2 . 00466 0.68 5-2 .02051 2.95 3 - 00505 0.74 5-3 .O2O9I 3.01 4 .00544 0.80 5.4 .02131 3.06 5 .00583 0.85 5-5 .02171 3.12 .6 .00622 0.91 5-6 .O22II 3.18 7 . 00662 0.97 5-7 .02252 3.23 .8 .00701 1.02 5-8 .02292 3.29 9 .00740 1. 08 5-9 02333 3-35 2.0 .00779 I. 14 6.0 02373 3-40 2.1 .00818 I.I9 6.1 .02413 3-46 2.2 .00858 1.25 6.2 02454 3-52 2-3 .00897 1.31 6-3 .02494 3-57 2.4 .00936 1.36 6.4 02535 3.63 2-5 .00976 1.42 6-5 -02575 3-69 2.6 .01015 1.48 6.6 .026l6 3-74 2.7 .01055 i-53 6.7 .02657 3.80 2.8 .01094 1-59 6.8 .02697 3-86 2.9 .01134 1.65 6.9 .02738 3-91 3-o .01173 1.70 7.0 .02779 3-97 3-i .OI2I3 1.76 7.1 .02819 4-03 3-2 .01252 1.82 7.2 .O286O 4.08 3-3 .01292 1.87 7-3 .02901 4.14 3-4 .01332 . 1-93 7-4 .02942 4.20 3-5 .01371 1.99 7-5 .02983 4-25 3-6 .01411 2.04 7-6 .03024 4-31 3-7 .01451 2.IO 7-7 . 03064 4-37 3-8 .01491 2.16 7-8 .03105 4.42 3-9 01531 2.21 7-9 .03146 4.48 118 SUGAR ANALYSIS. Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baume. S.o 1.03187 4-53 . 13.0 I .05276 7-36 8.1 I .03228 4.59 I3-I 1.05318 7 4i 8.2 1.03270 4.65 13-2 1.05361 7-47 8-3 I.033II 4.70 13-3 1-05404 7-53 8.4 1.03352 4.76 13-4 1.05446 7.58 8.5 1-03393 4-82 13-5 1.05489 7.64 8.6 I 03434 4-87 13.6 1.05532 7.69 8-7 1.03475 4-93 13-7 1-05574 7-75 8.8 1-03517 4.99 13-8 1.05617 7.81 8.9 1.03553 5-04 13-9 1.05660 7.86 9.0 1-03599 5.io 14-0 1.05703 7.92 9.1 1.03640 5.i6 14.1 1.05746 7.98 9.2 1.03682 5-21 14.2 1.05789 8.03 9-3 1.03723 5-27 1-4-3 1.05831 8.09 9-4 I.03765 5-33 14.4 1.05874 8.14 9-5 1.03806 5.38 14.5 1.05917 8.20 9.6 1.03848 5-44 14.6 1.05960 8.26 9-7 1.03889 5-50 14.7 1.06003 8.31 9.8 1.03931 5-55 14.8 I . 06047 8.37 9-9 1.03972 5-61 14.9 1 . 06090 8 . 43 10. 1.04014 5.67 15.0 1.06133 8.48 10. I 1.04055 5-72 I5-I 1.06176 8.54 10.2 1.04097 5.78 15-2 1.06219 8.59 10.3 1.04139 5-83 15-3 1.06262 8.65 10.4 1.04180 5.89 15 4 1.06306 8.71 10.5 1.04222 5-95 15-5 1.06349 8.76 10.6 1.04264 6.00 15.6 i .06392 8.82 10.7 1.04306 6.06 15.7 1.06436 8.88 10.8 1.04348 6.12 15-8 1.06479 8-93 10.9 1.04390 6.17 15.9 1.06522 8.99 II. 1.04431 6.23 16.0 1.06566 9.04 ii. i 1.04473 6.29 16.1 1.06609 9.10 II. 2 I.045I5 6-34 16.2 1.06653 9-i6 ii. 3 1.04557 6.40 16.3 1.06696 9.21 11.4 1.04599 6.46 16.4" 1.06740' 9.27 ii. 5 1.04641 6.51 16.5 1.06783 9.33 ii. 6 1.04683 6.57 16.6 1.06827 9.38 ii. 7 1.04726 6.62 16.7 1.06871 9.44 ii. 8 1.04768 6.68 16.8 1.06914 9-49 11.9 I .04810 6.74 16.9 1.06958 9.55 12.0 1.04852 6.79 17.0 1.07002 9.61 12. 1 1.04894 6.85 17.1 i .07046 9.66 12.2 1.04937 6.91 17.2 1.07090 9.72 12.3 1.04979 6.96 17-3 1.07133 9.77 12.4 I.0502I 7.02 17.4 107177 9.83 12.5 1.05064 7.08 17-5 1.07221 9.89 12.6 1.05106 7-13 17.6 1.07265 9.94 12.7 1.05149 7.19 17.7 1.07309 10.00 12.8 1.05191 7.24 17-8 1.07358 10.06 12.9 1.05233 7.30 17.9 1.07397 ! 10. i i SUGAR ANALYSIS. 119 Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baume". 18.0 1.07441 10. 17 23.0 .09686 12.96 I8.I 07485 IO.22 23.1 .09732 13.02 lS.2 07530 10.28 23-2 .09777 13.07 18.3 07574 10-33 23-3 .09823 I3.I3 18.4 .07618 10.39 23-4 .09869 13.19 18.5 .07662 10 45 23-5 .09915 13.24 18.6 .07706 10.50 23.6 .09961 I3.30 18.7 07751 10.56 23-7 . 10007 13-35 18.8 -07795 IO.62 23-8 .10053 I3.4I 18.9 .07839 10.67 23-9 .10099 13.46 19. o .07884 10-73 24.0 .10145 13-52 19.1 .07928 10.78 24.1 . lOlgl 13.58 19.2 07973 10.84 24.2 .10237 I3.63 iQ-3 .08017 10.90 24-3 . 10283 13.69 19.4 .08062 10.95 24.4 .10329 13-74 iQ-5 .08106 II. OI 24-5 10375 13.80 19.6 .08151 1 1. 06 24.6 . 10421 13.85 19.7 .08196 II. 12 24.7 . 10468 I3-9 1 19.8 .08240 II.I8 2 4 .8 .10514 13.96 19.9 .08285 11.23 24-9 . 10560 14.02 20.0 .08329 . 11.29 25.O . 10607 14.08 20.1 .08374 11-34 25-1 .10653 14.13 20.2 .08419 11.40 25.2 . 10700 14. 19 20.3 .08464 11-45 25.3 . 10746 14.24 2O.4 .08509 11.51 25-4 .10793 14.30 20.5 08553 H.57 25-5 . 10839 14-35 20.6 08599 11.62 2 5 .6 .10886 14.41 20.7 .08643 11.68 25-7 . 10932 14.47 20.8 .08688 11-73- 25-8 .10979 14.52 20.9 . -08733 11.79 25-9 .11026 14-58 21. .08778 11.85 26.0 . 11072 14.63 21. I .08824 11.90 26.1 .11119 14-69 21.2 .08869 11.96 26.2 .11166 14.74 21-3 .08914 12. OI 26.3 . 11213 14.80 21.4 .08959 12.07 26.4 .11259 14.85 21-5 . 09004 12.13 26.5 .11306 14.91 21.6 .09049 . 12.18 26.6 II353 14.97 21.7 .09095 12.24 26.7 . 11400 15.02 21.8 .09140 12.29 26.8 .11447 15.08 21.9 .09185 12.35 26.9 .11494 15.13 22. O .09231 12.40 27.0 .11541 15-19 22. I .09276 12.46 27.1 .11588 15.24 22.2 .09321 12.52 27.2 11635 15-30 22.3 09367 12.57 27-3 .11682 15-35 22.4 .09412 12.63 27-4 .11729 I5-4I 22.5 .09458- 12.68 27-5 .11776 15.46 22.6 09503 12.74 27-6 .11824 15-52 22.7 .09549 12.80 27-7 .11871 15-58 22.8 09595 12.85 27-8 . 11918 ^15-63 22.9 .09640 12.91 27-9 .119^5 15.69 120 SUGAR ANALYSIS. Degrees Brix. Specific Gravity. Degrees Baume". Degrees Brix. Specific Gravity. Degrees Baume. 28.0 I.I2OI3 15-74 33-0 .14423 18.50 28.1 I. I 2060 15.80 33-1 14472 18.56 28.2 I. I2I07 15.85 33-2 .14521 18.61 28.3 I.I2I55 I5.9 1 33-3 14570 18.67 28.4 I.I22O2 15.96 33-4 . 14620 18.72 28.5 I. I225O 16.02 33-5 . 14669 18.78 28.6 I.I2297 16.07 33-6 .14718 18.83 28.7 I-I2345 16.13 33-7 .14767 18.89 28.8 I.I2393 16.18 33.8 .14817 18.94 28.9 I.I2440 16.24 33-9 . 14866 19.00 29.0 I.I2488 16.30 34-o .14915 19.05 29.1 I.I2536 16.35 34-1 . 14965 19.11 29.2 1.12583 16.41 34.2 .15014 19.16 29-3 I .12631 16.46 34-3 .15064 19.22 29.4 I.I2679 16.52 34-4 .15113 19.27 29-5 I.I2727 16-57 34-5 .15163 19-33 29.6 I.I2775 16.63 34-6 I52I3 19.38 29.7 I . 12823 16.68 34.7 .15262 19.44 29.8 I.I287I 16.74 34-8 .15312 19.49 29.9 I.I29I9 16.79 34-9 .15362 19-55 30.0 1.12967 16.85 35-0 .15411 19.60 30.1 I.I30I5 16.90 35-1 .15461 19.66 30.2 I.I3063 16.96 35-2 -I55II 19.71 30.3 I.I3III 17.01 35.3 .15561 19.76 30-4 I.I3I59 17.07 35-4 .15611 19.82 30.5 I.I3207 17.12 35-5 .15661 19.87 30.6 I.I3255 17.18 35-6 .15710 19-93 30.7 I.I3304 17.23 35-7 .15760 19.98 30.8 I.I3352 17.29 35-8 .15810 20.04 30-9 I . 13400 17-35 35-9 .1586*1 20.09 31.0 I.I3449 17.40 36.0 .15911 20. 15 3I-I I.I3497 17.46 36. i .15961 20.20 31.2 I.I3545 I7.5I 36.2 . l6oil 20.26 31-3 I.I3594 17-57 36.3 .16061 20.31 3L4 1.13642 17.62 36-4 . 16111 20.37 3 r -5 1.13691 17.68 36.5 . 16162 20.42 31-6 I.I3740 17-73 36.6 .16212 20.48 3i.7 I.I3788 17-79 36.7 .16262 20.53 31-8 I.I3837 17.84 36.8 .16313 20.59 3i-9 I.I3885 17.90 36-9 .16363 20.64 32.0 LI3934 17-95 37-0 .16413 20.70 32.1 I.I3983 18.01 37-1 .16464 20.75 32.2 I.I4032 18.06 37-2 .16514 20.80 32.3 I.I4O8I 18.12 37.3 .16565 20.86 32.4 I.I4I29 18.17 37.4 .16616 20.91 32.5 I.I4I78 18.23 37-5 . 16666 20.97 32.6 I.I4227 18.28 37-6 .16717 21. 02 32-7 1.14276 18.34 37-7 .16768 21.08 32-8 I.I4325 18.39 37-8 .16818 21.13 32-9 I H374 18.45 37-9 . 16869 21. 19 SUGAR ANALYSIS. 121 Degrees Brix. Specific Gravity. Degrees Baiiine*. Degrees Brix. Specific Gravity. Degrees Baume". 38.0 . 16920 21.24 43-0 1950S 23-96 38.1 .16971 21.30 43-1 .19558 24.01 38.2 .17022 21-35 43-2 .19611 24.07 38.3 .17072 21.40 43-3 .19663 24. 12 38.4 .17132 21.46 43.4 .19716 24.17 38-5 .17174 21-51 43-5 .19769 24.23 38.6 .17225 21-57 43-6 .19822 24.28 38.7 .17276 21.62 43-7 19875 24-34 38.8 .17327 21.68 43-8 19927 24-39 38.9 17379 21.73 43-9 . 19980 24.44 39-o .17430 21.79 44.0 20033 24.50 39-i .17481 21.84 44.1 . 20086 24-55 39-2 17532 21.90 44-2 .20139 24.61 39-3 .17583 21.95 44-3 .20192 24.66 39-4 .17635 22.00 44.4 -20245 24.71 39-5 .17686 22.06 44-5 . 20299 24-77 39-6 .17737 22.11 44-6 .20352 24.82 39-7 .17789 22.17 44-7 . 20405 24.88 39-8 .17840 22.22 44-8 .20458 24-93 39-9 .17892 22.28 44-9 .20512 24.98 40.0 17943 22.33 45-0 .20565 25.04 40.1 .17995 22.38 45.1 .20618 25.09 40.2 .18046 22-44 45-2 .20672 25-I4 40-3 .18098 22.49 45-3 .20725 25.2O 40.4 .18150 22-55 45-4 20779 25.25 40.5 . 18201 22.6O 45 5 .20832 25.31 40.6 .18253 22.66 45-6 .20886 25-36 40.7 18305 22.71 45-7 .20939 25-4I 40.8 18357 22.77 45-8 - 20993 25-47 40.9 .18408 22.82 45-9 .21046 25.52 41.0 .18460 22.87 46.0 .21100 25-57 41.1 .18512 22.93 46.1 2II54 25.63 41.2 .18564 22.98 46.2 .21208 25.68 41-3 .18616 23-04 46.3 .21261 25-74 41.4 .18668 23.09 46.4 .21315 25-79 41-5 . 18720 23-15 46.5 .21369 25.84 41.6 .18772 23.20 46.6 .21423 25.90 4*. 7 .18824 23.25 46-7 21477 25.95 41.8 .18877 23-31 46.8 .21531 26.OO 41.9 .18929 23.36 46.9 .21585 26.06 42.0 .18981 23.42 47-o - .21639 26.11 42.1 .I9 33 23.47 47.1 21693 26.17 42.2 . 19086 23.52 47-2 21747 26.22 42.3 .19138 23.58 47-3 .21802 26.27 42-4 .19190 23.63 47-4 .21856 26.33 42.5 .19243 23.69 47-5 .2iqiO 26.38 42.6 .I9 2 95 23.74 47.6 .21964 26.43 42.7 . 19348 23.79 47.7 I .22019 26.49 42.8 .19400 23.85 47.8 1.22073 26.54 42.9 19453 23.90 47-9 1.22127 26.59 122 SUGAR ANALYSIS. Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baume. 48.0 .22182 26.65 53-0 .24951 29.31 48.1 .22236 26.70 53-1 .25008 29-36 4 8.2 .22291 . 26.75 53-2 .25064 29.42 48.3 .22345 26.81 53-3 .25120 29.47 48.4 . 22400 26.86 53-4 -25177 29.52 43-5 22455 26.92 53-5 25233 29-57 48.6 .22509 26.97 53-6 .25290 29.63 48-7 .22564 27.02 53-7 25347 29.68 48.8 .22619 27.08 53-8 .25403 29.73 48.9 .22673 27.I3 53-9 .25460 29.79 49.0 .22728 27.18 54 -o .25517 29.84 49.1 .22783 27-24 54.i 25573 29.89 49.2 .22838 27.29 54.2 .25630 29.94 49-3 .22893 27-34 54-3 .25687 30.00 49.4 .22948 27.40 54-4 .25744 30.05 49-5 .23003 27-45 54-5 .25801 30.10 49.6 .23058 27.50 54-6 .25857 30. 16 49-7 .23113 27.56 54-7 259H 30.21 49.8 .23168 27.61 54-8 .25971 30.26 49.9 .23223 27.66 54-9 .26028 30.31 50.0 .23278 27.72 55-o .26086 30-37 50.1 23334 27.77 55-1 .26143 30.42 50.2 23389 27.82 55-2 . 26200 30-47 50-3 23444 27.88 55-3 .26257 30-53 50.4 23499 27-93 55-4 .26314 30.58 50.5 23555 27.98 55-5 .26372 30.63 50.6 .23610 28.04 55-6 .26429 30.68 50.7 . 23666 28.09 55-7 .26486 30.74 50.8 .23721 28.14 55-8 .26544 30-79 50.9 23777 28.20 55-9 .26601 30.84 51-0 .23832 28.25 56.0 .26658 30.89 5i-i .23888 28.30 56-1 .26716 30.95 51-2 23943 28.36 56-2 .26773 31.00 5i-3 .23999 28.41 56.3 .26831 31-05 51-4 24055 28.46 56-4 .26889 31.10 51-5 .24111 28.51 . 56.5 .26946 31. 16 51.6 .24166 28.57 56.6 .27004 31.21 51-7 .24222 28.62 56.7 .27062 31 .26 51.8 .24278 28.67 56.8 .27120 3i-3i 51-9 24334 28.73 56.9 .27177 31-37 52.0 . 24390 28.78 57-o 27235 31.42 52.1 .24446 28.83 57-1 .27293 31-47 52.2 .24502 28.89 57-2 .27351 3I-52 52.3 .24558 28.94 57-3 .27409 31-58 52.4 .24614 28.99 57-4 .27467 31-63 52. '5 .24670 29.05 57-5 27525 31.68 52.6 .24726 29.10 57-6 .27583 31-73 52.7 .24782 29.15 57-7 .27641 31-79 52.8 1.24839 29.20 57-8 .27699 31.84 52.9 1.24895 29.26 57-9 .27758 31.89 SUGAR ANALYSIS. 123 Degrees Brix. Specific Gravity. Degrees Baiiine*. Degrees Brix. Specific Gravity. Degrees Baume. 58.0 .27816 31-94 63.0 .30777 34-54 58.1 .27874 32.00 6 3 .I 30837 34-59 58.2 .27932 32.05 63.2 .30897 34-65 5S.3 .27991 32. 10 63.3 .30958 34-70 58.4 .28049 32.15 63-4 .31018 34-75 58.5 .28107 32.20 63-5 .31078 34.80 58.6 .28166 32.26 63.6 .31139 34-85 58.7 .28224 32.31 63-7 .31199 34-9 58.8 .2^8283 32.36 63-8 .31260 34-96 58.9 .28342 32.41 63.9 .31320 35-01 59- . 28400 32.47 64.0 .31381 35-o6 59-i .28459 32.52 64.1 .3M42 35-n 59-2 .28518 . 32.57 64.2 3*502 35-i6 59-3 .28576 32.62 64-3 .31563 35-21 59-4 .28635 32.67 64.4 .31624 35-27 59-5 .28694 32-73 64-5 .31684 35-32 59-6 .28753 32.78 64.6 3 J 745 35-37 59-7 .28812 32.83 64.7 . 3 i 806 35-42 59-8 .28871 32.88 64.8 .31867 35-47 59-9 .28930 32.93 64.9 .31928 35-52 60.0 .28989 32.99 65.0 .31989 35-57 60. i .29048 33-04 65.1 .32050 35-63 60.2 .29107 33-09 65.2 .32111 35-63 60.3 .29166 33.14 65.3 .321/2 35-73 60.4 .29225 33-20 65.4 .32233 35-78 60.5 .29284 33-25 65.5 .32294 35-S3 60.6 29343 33-30 65.6 .32355 35-88 60. 7 .29-103 33-35 65.7 32417 35-93 60.8 .29462 33-40 65.8 .32478 35-98 60.9 .29521 33-46 65-9 .32539 36.04 61.0 .29581 33.51 66.0 .32601 36.09 61.1 . 29640 33.56 66.1 .32662 36.14 61 .2 .29700 33-61 66.2 32724 36.19 61.3 29759 33-66 66.3 32785 36.24 61 .4 .29819 33-71 66.4 32847 36.29 61.5 .29878 33-77 66.5 .32908 36.34 61.6 .29938 33-82 66.6 .32970 36.39 61.7 . 29998 33-87 66.7 33031 36.45 61.8 30057 33-92 66.8 33093 36-50 61.9 .30117 33-97 66.9 .33155 36.55 62.0 30177 34-03 67.0 .33217 36.60 62.1 .30237 34-o8 67.1 .33278 36.65 62.2 .30297 34-13 67.2 33340 36.70 62.3 30356 34.18 67-3 .33402 36.75 62.4 .30416 34-23 67.4 33464 36.80 62.5 30476 34.28 67-5 .33526 36.85 62.6 30536 34-34 67.6 33588 36.90 62.7 .30596 34-39 67-7 33650 36.96 62.8 1-30657 34-44 67.8 33712 37.01 62.9 1.30717 34-49 67-9 33774 37.o6 124 SUGAR ANALYSIS. Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baiiine". 68.0 1.33836 37-11 73-0 1.36995 39-64 68.1 1.33899 . 37-16 73-1 37059 39-69 68.2 1.33961 37-21 73-2 1.37124 39-74 68.3 1.34023 37-26 73.3 .37188 39-79 68.4 1.34085 37-31 73.4 .37252 39-84 68.5 1.34148 37.36 73.5 .37317 39-89 63.6 1.34210 37-41 73-6 .37381 39-94 68.7 1.34273 37-47 73-7 .37446 39-99 68.8 1-34335 37-52 73-8 37510 40.04 68.9 1.34398 37-57 73-9 37575 40.09 69.0 i . 34460 37-62 74-o 37639 40.14 69.1 1.34523 37-67 74.1 37704 40.19 69.2 I.34585 37-72 74-2 .37768 40.24 69-3 i 34648 37-77 74-3 .37833 40.29 69.4 I-347II 37.82 74-4 .37898 40.34 69-5 1-34774 37.87 74-5 -37962 40.39 69.6 1.34836 37-92 74.6 .38027 40.44 69.7 1.34899 37-97 74-7 .38092 40.49 69.8 i 34962 38.02 74-8 38157 40.54 69.9 1-35025 38.07 74-9 ..38222 40.59 70.0 1.35088 38.12 75-0 .38287 40.64 70.1 I.35I5I 38.18 75-1 .38352 40.69 70.2 I.352I4 38-23 75-2 38417 40.74 70.3 I-35277 38.28 75-3 .38482 40.79 70.4 1-35340 38.33 75-4 .38547 40.84 70.5 1-35403 38.38 75-5 .38612 40.89 70.6 1.35466 . 38.43 , 75-6 08677 40.94 70.7 1-35530 38.48 75-7 .38743 40.99 70.8 1-35593 38.53 75.8 .38808 41.04 70.9 1.35656 38.58 75-9 38873 41.09 71.0 1.35720 38-63 76.0 .38939 41.14 71. 1 I.35783 38.68 76.1 . 394 41.19 71.2 1.35847 38-73 76.2 .39070 41.24 71.3 I-359IO 38-78 76.3 .39135 41.29 71.4 1-35974 38.83 76.4 .39201 41-33 71-5 1.36037 38.88 76.5 .39266 41.38 71.6 1.36101 38.93 76.6 39332 41-43 71.7 1.36164 38.98 76.7 39397 41.48 71.8 1.36228 39-03 76.8 39463 41.53 71.9 1.36292 39-o8 76.9 39529 41.58 72.0 1-36355 39-13 77-0 39595 41.63 72.1 1.36419 39-19 77-i . 39660 41.68 72.2 1-36483 39-24 77-2 .39726 41-73 72.3 1.36547 39-29 77-3 39792 41.78 72.4 1.36611 39-34 77-4 -39858 41.83 72-5 1.36675 39 39 77-5 .39924 41.88 72.6 1.36739 39-44 77-6 3999 41-93 72-7 1.36803 39 49 77-7 i .40056 41.98 72.8 1.36867 39-54 77-8 i .40122 42.03 72-9 1.36931 39-59 77-9 1.40188 42.08 SUGAR ANALYSIS. 125 Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baume. 78.0 .40254 42.13 83.0 43614 44.58 7 8.1 .40321 42.18 83.1 .43682 44.62 7 8.2 40387 42.23 8 3 .2 43750 44-67 78.3 40453 42.28 83-3 .43819 44-72 78.4 .40520 42.32 83.4 .43887 44-77 73.5 .40586 42.37 83-5 43955 44.82 78.6 .40652 42.42 83.6 44024 44.87 78.7 .40719 42.47 83.7 44092 44.91 78.8 .40785 42.52 83.8 .44161 44.96 78.9 .40852 42-57 83-9 .44229 45-01 7Q.O .40918 42.62 84.0 .44298 45-o6 79.1 .40985 42.67 84.1 .44367 45-11 79-2 .41052 42.72 8 4 .2 44435 45.16 79-3 .41118 42.77 84-3 44504 45-21 79-4 .41185 42.82 84.4 4-4573 45-25 79-5 .41252 42.87 84-5 .44641 45-30 79 - 6 .41318 42.92 84.6 .44710 45-35 79-7 41385 42 . 96 84-7 44779 45-40 79-8 .41452 43-or 84.8 .44848 45-45 79-9 -41519 43.06 84.9 .44917 45-49 80.0 .41586 43-H 85.0 .44986 45-54 80. i .41653 43.16 85-1 45055 45-59 80.2 .41720 43-21 85-2 -45124 45-64 80.3 .41787 43-26 85-3 45193 45 '-69 80.4 .41854 43-31 85.4 .45262 45-74 80.5 .41921 43.36 85-5 45331 45.78 80.6 .41989 43-41 85.6 .45401 45-83 80.7 .42056 43-45 85.7 -45470 45-88 80.8 .42123 43-50 85.8 45539 45-93 80.9 .42190 43-55 85.9 .45609 45.9 8 81.0 .42258 43.60 86.0 45678 46.02 81.1 42325 43-65 86.1 45748 46.07 81.2 .42393 43-70 86.2 .45817 46.12 81.3 .42460 43.75 86.3 .45887 46.17 81.4 .42528 43.80 86.4 45956 46.22 81.5 .42595 43-85 86.5 .46026 46.26 Si. 6 42663 43-89 86.6 .46095 46.31 81.7 42731 43-94 86.7 .46165 46.36 81.8 .42798 43-99 86.8 46235 46.41 81.9 .42866 44.04 86.9 46304 46.46 82.0 42934 44.09 87.0 .46374 46.50 82.1 .43002 44.14 87.1 46444 46.55 82.2 43070 44.19 87.2 -46514 46.60 82.3 43137 44-24 87.3 .46584 46-65 82.4 43205 44.28 87-4 .46654 46.69 82.5 .43273 44-33 87-5 .46724 46.74 82.6 43341 44.38 87.6 .46794 46.79 82.7 . .43409 44-43 87.7 .46864 46.84 82.8 .43478 44.48 87.8 .46934 46.88 82.9 43546 44-53 87.9 .47004 46.93 126 SUGAR ANALYSIS. Degrees Brix. Specific Gravity. Degrees Baume. Degrees Brix. Specific Gravity. Degrees Baume. 8S.o .47074 46.98 93-0 00635 49-34 88.1 47145 47-03 93-1 50707 49-39 88.2 .47215 47.08 93-2 50779 49-43 88.3 4/285 47.12 93-3 50852 49-48 88.4 .47356 47-17 93-4 50924 49-53 88.5 .47426 47-22 93-5 . 50996 49-57 88.6 .47496 47.27 93-6 .51069 49.62 88.7 .47567 47-31 93-7 .51141 49.67 88.8 47637 47-36 93-8 .51214 49.71 88.9 .47708 47.41 93-9 .51286 49-76 89.0 47778 47.46 94.0 51359 49.81 89.1 .47849 47.50 94.1 5I43I 49-85 89.2 .47920 47.55 94-2 51504 49.90 89-3 .47991 47.60 94-3 51577 49-94 89.4 .48061 47-65 94-4 .51649 49-99 89-5 .48132 47.69 94-5 .51722 50.04 89.6 .48203 47-74 94-6 51795 50.08 89.7 .48274 47-79 94-7 .51868 50.13 89.8 48345 47-83 94.8 5I94I 50.18 89.9 .48416 47-88 94.9 .52014 50.22 90.0 .48486 47-93 95-0 52087 50.27 90.1 .48558 47.98 95-1 52159 50.32 90.2 .48629 48.02 95-2 .52232 50.36 90.3 .48700 48.07 95-3 52304 50.41 90.4 .48771 48.12 95 4 52376 50-45 90.5 . .48842 48.17 95-5 52449 50.50 90.6 .48913 48.21 95-6 52521 50 55 90.7 48985 48.26 95-7 52593 50.59 90.8 .49056 48.31 95-8 52665 50.64 90.9 .49127 48.35 95-9 .52738 50.69 91.0 .49199 48.40 96.0 .52810 50.73 91.1 .49270 48.45 96. i .52884 50-78 Ql.flf 49342 48-50 96.2 .52958 50.82 QI-3 49413 48.54 96.3 .53032 50.87 91.4 49485 48.59 96.4 53IO6 50.92 91-5 .49556 48.64 96.5 .53l8o 50.96 91.6 .49628 48.68 96.6 53254 51.01 91.7 .49700 48.73 96.7 .53328 51-05 91.8 49771 48.78 96.8 .53402 51.10 91.9 .49843 48.82 96.9 534"6 5LI5 92.O 49915 48.87 97.0 53550 5I-I9 92.1 .49987 48.92 97.1 53624 51-24 92.2 .50058 48.96 97.2 53698 51.28 92.3 .50130 49.01 97-3 53772 51-33 92.4 .50202 49.06 97.4 53846 5I-38 92.5 50274 49.11 97-5 53920 5L42 92.6 50346 49-^5 97-6 53994 51-47 92.7 .50419 49.20 97-7 .54068 Si-Si 92.8 .50491 49-25 97-8 .54142 5I-56 92.9 50563 49.29 97-9 .54216 51.60 SUGAR ANALYSIS. 127 Degrees Brix. Specific Gravity. Degrees Baume". Degrees Brix. Specific Gravity. Degrees Baume". 98.0 .54290 51.65 99.0 .55040 52.11 98.1 .54365 51.70 99.1 55II5 52.15 98.2 . 54440 51-74 99.2 .55189 52.20 98.3 54515 5L79 99-3 55264 52.24 98.4 54590 51.83 99.4 -55338 52.29 93.5 .54665 51-88 99-5 55413 52.33 98.6 54740 5L9 2 99 6 .55487 52.38 98.7 .54815 5L97 99-7 .55562 52.42 98.8 .54890 52.01 99.8 .55636 52.47 98.9 .54965 52.06 99.9 557II 52.51 100. 1.55785 52.56 II. CORRECTIONS FOR TEMPERATURE IN DE- TERMINATIONS BY THE SPECIFIC GRAV- ITY HYDROMETER. (CASAMAJOR.) 129 130 SUGAR ANALYSIS. II. Normal Temperature : 15.0 C. Normal Temperature : 17.5 C. Temperature in Degrees Centigrade. Add to the Reading of the Hydrometer. Temperature in Degrees Centigrade. Add to the Reading of the Hydrometer. 9. go 0.0005 7-5 O.OOIO 15.00 . 0000 13.0 0.0005 18.20 -f 0.0005 17-5 . 0000 20.75 O.OOIO 20.2 -j-o . 0005 23.20 O.OOI5 23-0 O.OOIO 25.30 O.OO2O 25.0 0.0015 27.30 0.0025 27.0 0.0020 29.40 0.0030 29.0 0.0025 31.20 0.0035 31.0 o . 0030 32.80 o . 0040 32-5 O.OO35 34.50 0.0045 34-7 0.0040 36. 10 0.0050 36.2 0.0045 37.60 0.0055 37-4 O.OO5O 38.80 o . 0060 39-o 0.0055 40.40 0.0065 40.5 0.0060 41.60 o . 0070 42.0 0.0065 42.90 0.0075 43-4 O.OO7O 44.20 0.0080 44.2 0.0075 45.00 0.0083 45-0 0.0080 III. CORRECTIONS FOR TEMPERATURE IN DE- TERMINATIONS BY THE BRIX HYDRO- METER. , Normal Temperature = 17.5 0. (STAMMER) 131 132 SUGAR ANALYSIS. III. DEGREE BRIX OF THE SOLUTION. Degree Centi- 5 10 15 20 25 30 85 40 50 60 70 75 grade. The degree read is to be decreased by O 0.17 0.30 0.41 0.52 0.62 0.72 0.82 0.92 0.98 1. 1 1 1.22 1-25 1.29, 5 0.230.30 0.37 0.44 0.52 0-59 0.65 0.72 0.75 0.80 0.88 0.91 0.94 10 O.2OO.26 0.29 0-33 0.36 0-39 0.42 0-45 0.48 0.50 o.54 0.58 0.61 II 0.180.23 0.26 0.28 0.31 0.34 0.36 0-39 0.41 0-43 0.47 0.50 0-53 12 O. l6 O.2O O.22 0.24 0.26 0.29 0.31 0-33 0-34 0.36 0.40 0.42 0.46 13 0.14 o. 18 o. 19 0.21 0.22 0.24 0.26 0.27 0.28 0.29 0-33 0.35 0-39 14 0.12,0. 15 0.16 0.17 0.18 o. 19 0.21 0.22 0.22 0.23 0.26 0.28 0.32 15 0.09 o. ii 0.12 0.14 0.14 0.15 0.16 0.17 0.16 0.17 o. 19 O.2I 0.25 16 0.06 0.07)0.08 0.09 0.10 O. IO O. II 0.12 O.I2 0.12 o. 14 o. 16 0.18 '?, 0.02 o. 02 0.03 0.03 0.03 0.04 0.04 0.04 O.O4 O.O4 0.05 0.05 0.06 The degree read is to be increased by 18 0.02 0.03J0.03 0.03 0.03 0.03 0.03 0.03 0.03 0.03 0.03 0.03 O.O2 !Q 0.06 0.080.08 0.09 0.09 O. IO O. IO O. IO O. IO 0.10 O. IO 0.08 O.O6- 20 O. II 0.140.15 0.17 0.17 0.18 0.18 o.iS o. 19 o. 19 0.18 0.15 O.II 21 O. 16 O.2OJO.22 O.24 0.24 0.25 0.25 0.25 0.26 O.26 0.25 0.22 0.18 22 0.21 0.260.29 0.31 0.31 0.32 0.32 0.32 0.33 0-34 0.32 0.29 0.25 23 0.270.320.35 0.37 0.38 0-39 0-39 0.39 0.40 0.42 0-39 0.36 0.33 24 0.32 0.380.41 0-43 0.44 0.46 0.46 0.47 0.47 O.5O 0.46 0-43 0.40 25 0-37 0.44 0.47 0.49 0.51 0-53 0-54 0.55 0.55 0.58 0-54 0.51 0.48 26 0.430.500.540.56 0.58 0.60 0.61 0.62 0.62 0.66 0.62 0.58 0-55 27 0.49 0.57 0.61 0.63 0.65 0.68 0.68 0.69 0.70 0.74 0.70 0.65 0.62 28 0.56 0.640.68 0.70 0.72 o. 76 0.76 0.78 0.78 0.82 0.78 0.72 o. 70 29 0.63 0.71 0.75 0.78 0.79 0.84 0.84 0.86 0.86 0.90 0.86 0.80 0.78 30 0.70 0.780.82,0.87 0.87 0.92 0.92 0.94 0.94 0.98 0.94 o.8S 0.86 35 I. 10 1.17 1.22 1.24 1.30 1.32 1-33 i-35 1.36 1-39 1-34 1.27 1-25 40 1.50 1.61 1.67 I.7I 1-73 1.79 1.79 i. 80 1.82 1.83 1.78 1.69 1.65 50 2.65 2.712.74 2.78 2.80 2.80 2.80 2.80 2.79 2.70 2.56 2.51 60 ... 3-87 3.88,3.88 3.88 3-88 3.88 3.88 3-9 3.82 3-70 3-43 3-41 7O c . 1 8 c .-?n c . 14 ^ 13 5 10 5.08 5.06 4.90 4.72 4.47 4-35 /^ 80 3 . J. U 6.62 6-59 j **t 6.54 D ' x O 6.46 6.38 j vw '6.30 6.26 6.06 5.82 5-50 5-33 IV. FACTO ES. Arranged for Specific Gravity Determinations. Calculated for Wiechmann : Sugar Analysis, from the data given in Table I. 26.048 Factor = Degree Brix X Specific Gravity 134 SUGAR ANALYSIS. IV. Specific Gravity. Factor. Specific Gravity. Factor. Specific Gravity. Factor. Specific Gravity. Factor. .0950 1.053 .0980 1.023 .1010 0.990 I . 1040 0-959 0955 1.047 .0985 1.013 .1015 0.985 I . 1045 0-955 .0960 1.042 .0990 1.008 .1020 0.981 1.1050 0.950 .0965 1-037 0995 1.004 .1025 0.976 I.I055 0.946 .0970 1.033 .IOOO I.OOO .1030 0.972 I . 1060 0.942 0975 1.028 .1005 0.944 1035 0.968 V. FACTORS. Arranged for Brix determinations. Calculated for Wiechmann: Sugar Analysis, from the data given in Table I. 26.048 Factor = Degree Brix x Specific Gravity" 185 136 SUGAR ANALYSIS. y. Degree Brix. 1 2 3 4 5 6 7 8 9 o 260.381 I 30. 140 86.726 6^ .OIQ 51 . 006 43. 313 37> m 32.459 28.842 I 25-947 23-579 J. J^f . Ai-|.W 2I.6O6 19.936 w * VA y 18.505 o * - v v 17-265 T- J * J * O 16.179 15.222 14.370 13-609 2 12.923 12.303 n-739 11.225 10-753 10.318 9.918 9-547 9.202 8.881 3 8.582 8.302 8.039 7-793 7.560 7-342 7.135 6.939 6-754 6.578 4 6.41! 6.253 6. 101 5-957 5.819 5.688 5.562 5.441 5-326 5-215 5 5.109 5.007 4.909 4.814 4-723 4-635 4.551 4.469 4-390 4.314 6 4.241 4.170 4.101 4-034 3.969 3.907 3-846 3.7&7 3-730 3.674 7 3.621 3-568 3.517 3-468 3.419 3-372 3.327 3.282 3-239 3.197 8 3-155 3.H5 3.076 3-038 3.OOO 2.964 2.928 2.893 2.859 2.826 9 2-794 2.762 2.731 2.700 2.671 2.641 2.613 2.585 2-557 2-531 10 2.504 2.479 2-453 2.428 2.404 2.380 2-357 2-334 2.311 2.289 ii 2.268 2.246 2.225 2.205 2.185 2.165 2.145 2.126 2.107 2.088 12 2.070 2.052 2.035 2.017 2.OOO 1.983 967 951 935 .919 13 903 1.888 873 .858 .843 1.829 .815 .801 .787 774 14 .760 1.747 734 .721 .709 1.696 .684 .672 .660 .648 15 .636 .625 .613 .602 59 1 1.580 .569 559 548 .538 16 .528 .518 .508 .498 .488 1.478 .469 459 450 .441 17 432 423 .414 -405 397 1.388 .380 371 .363 355 18 347 339 -331 323 315 1.308 .300 293 .285 .278 19 .271 .264 .256 .249 243 1.236 .229 .222 .215 .209 20 .202 .196 .189 -183 .177 I.I7I . 164 .158 .152 .146 21 .140 134 .129 .123 .117 i. in .106 .100 095 .089 22 .084 .079 1.073 .068 .063 1.058 . -053 047 .042 037 23 033 .028 1.023 .018 .013 1.008 .004 0.999 0.994 0.990 24 0.985 0.981 0.976 0.972 0.968 0.963 0.959 0-955 0.950 0.946 25 0.942 0.938 0-934 0.930 0.926 0.922 0.918 0.914 0.910 0.906 26 0.902 0.898 0.894 0.891 0.887 0.883 0.879 0.876 0.872 0.869 27 0.865 0.861 0.858 0.854 0.851 0.847 0.844 0.841 0.837 0.834 28 0.831 VI ESTIMATION OF PERCENTAGE OF SUGAR BY WEIGHT, IN WEAK SUGAR SOLUTIONS. Tucker : Manual of Sugar Analysis. Abridged from a table calculated by: (OSWALD.) 137 138 SUGAR ANALYSIS. VI. Degree Brix. Specific Gravity. READING OF THE SACCHARIMETER. 1 2 3 4 5 6 7 8 9 10 0.0 I.OOOO .260 .521 .781 1.042 1.302 1.563 1.823 2.084 2-344 2.605 0-5 I.OOlg .260 .520 .780 1.040 1.300 1.560 1.820 2.o8c 2.34C 2.600 1.0 1.0039 259 .519 778 1.038 .297 1-557 1.816 2.076 2-335 2.595 1-5 1.0058 259 .518 777 1 .036 295 1-554 1.813 2.072 2-331 2.590 2.0 1.0078 258 .517 775 1.034 .292 i.55i 1.809 2.068 2.326 2.585 2-5 1.0097 .258 .516 774 1.032 .290 1.548 i. 806 2.064 2.322 2.580 3-o I.OII7 257 .515 772 1.029 .287 1-545 1.802 2.060 2.317 2-575 3-5 I.OI37 257 514 .771 1.028 .285 1-542 1.799 2.056 2.313] 2.570 4.0 I.OI57 256 .513 .769 1.026 .282 1-539 1.795 2.052 2.308 2.565 4-5 I.OI77 .256 .512 .768 1.024 .280 1.536 1.792 2.048 2.304 2-559 5-0 1.0197 255 .511 .766 1.022 277 1-533 1.788 2.044 2.299 2-554 5-5 I.02I3 .255 .510 .765 1.020 275 i-53 1.785 2.040 2.295 2.549 6.0 1.0237 254 .509 .763 I .Ol8 .272 1-527 1.781 2.036 2.290 2-544 6.5 1.0257 254 .508 .762 1.016 .270 J -524 1-778 2.032 2.285 2-539 7.0 1.0278 253 507 .760 i .014 .267 1.521 1-774 2.027 2.281 2.534 7-5 1.0298 .253 .506 .758 1. 012 .265 1.518 1.771 2.023 2.276 2.529 8.0 1.0319 .252 SOS -757 I.OIO .262 I-5I5 1.767 2.019 2.272 2.524 8-5 1-0339 .252 .504 756 1.008 .260 1.512 1.763 2.015 2.267 2.519 9.0 1.0360 .251 503 -754 1.006 .257 1.509 1.760 2. Oil 2.263 2.514 9-5 1.0380 251 .502 753 1.004 .255 1.506 1-757 2.OO7 2.258 2.509 10. I.O4IO 250 .501 75i 1.002 .252 1-503 1-753 2.OO3 2.254 2.504 10.5 1.0422 250 .500 75 I. 000 .250 1.500 1.750 -999 2.249 2.499 II. 1.0443 249 499 .748 .998 247 1.497 1.746 995 2.245J 2.494 "5 1.0464 249 .498 .747 .996 .245 1.494 1-743 .991 2.240 2.489 12.0 1.0485 248 .497 745 994 .242 1.491 1-739 -987 2.236 2.484 12-5 1.0506 2 4 8 .496 744 .992 .240 1.488 1-735 -983 2.231 2-479 13-0 1.0528 247 495 742 .990 .237 1.484 1-732 979 2.227 2.474 13-5 1.0549 247 494 .741 .988 235 1.482 1.728 975 2.222 2.469 14.0 1.0570 2 4 6 493 739 .986 .232 1.479 1.725 .971 2.218 2.464 14-5 1.0591 2 4 6 .49 2 .738 .984 230 1.476 1.722 .967 2.213 2.459 15.0 1.0613 245 .491 736 .982 .227 1-473 1.718 963 2.209 2-454 15-5 1.0635 245 .490 735 .980 225 1.470 1.714 959 2.2O4 2-449 16.0 1.0657 244 .489 733 .978 .222 1.467 1.711 -955 2.2OO 2.444 ^16.5 1.0678 244 .488 732 .976 .220 1.464 1.708 -951 2.195 2-439 17.0 I . 0700 243 .487 .730 974 .217 1.461 1.704 .948 2.I9I 2-434 17-5 I .'0722 243 .486 .729 .972 .215 1.458 1.701 944 2.186 2.429 18.0 1.0744 242 485 .727 .970 .212' 1.455 1.697 .940 2.182 2.424 18.5 1.0765 242 .484 .726 .968 2IO 1.452 1.694 .936 2.178 2.420 19.0 1.0787 241 483 .724 .966 207 1.449 1.690 932 2.173 2.415 19-5 I.oSlO 241 .482 723 .964 205 1.446 1.687 .928 2.169 2.410 20. o 1.0833 240 .481 .721 .962 202 1 1.443 1.683 .924 2.164 2.405 20.5 1.0855 240 .480 .720 .960 2OO 1 . 440 i. 680 .920 2.160 2.400 21. 1.0878 239 -479 .718 958 197 1-437 1.676 .916 2.155 2.395 21-5 I . 0900 239 .478 .717 .956 195 1-434 1-673 .912 2.I5I 2.39 22.0 1.0923 238 477 .715 954 192 1.431 i . 669 . 908 2. 146 2.385 22.5 I . 0946 238 .476 .714 952 190' 1.428 1.666 .904 2.142 2.380 23.0 I . 0969 237 -475 .712 .950 187 1.425 1.662 .900 2-137 2-375 VII. "HUNDRED POLARIZATION." (SCHEIBLEB.) 139 140 SUGAR ANALYSIS. YII. SoS O 64 147.2 51-2 17 62.6 13-6 -30 22 -24 63 145-4 50.4 16 60.8 12.8 -31 -2 3 .8 24.8 62 143.6 49-6 15 59 12 -32 -25.6 -2 5 .6 61 141.8 48.8 14 57-2 II. 2 -33 -27.4 26.4 60 140 48 13 55-4 10.4 -34 -29.2 -27.2 59 138.2 47-2 12 53-6 9 .6 -35 -31 -28 58 136.4 46.4 II 51-8 8.8 -36 -32.8 -28.8 57 134.6 45-6 10 50 8 -37 -34-6 29.6 56 132.8 44.8 9 48.2 7-2 -38 36.4 -30-4 55 131 44 8 46.4 6.4 -39 -38.2 -31.2 54 129.2 43-2 7 44.6 5-6 -40 -40 -32 SUGAR ANALYSIS. 177 XVIII. FAHRENHEIT, CENTIGRADE, REAUMUR. Fah- ren- heit. Centi- grade. Reaumur. Fah- ren- heit. Centi- grade. Reaumur. Fah - Cend- he*. ^ de - Reaumur. o j 212 100 80 165 73.89 59-n 118 47.78 38.22 211 99-44 79-56 164 73-33 58.67 117 47-22 37-78 2IO 98.89 79.11 163 72.78 58.22- 116 46.67 37-33 209 98.33 78.67 162 72.22 57-78 H5 46.11 36.89 208 97.78 78.22 161 71.67 57-33 114 45.55 36.44 2O7 97.22 77-78 160 71.11 56.89 H3 45 36 206 96.67 77-33 159 70.55 56.44 112 44-44 35.56 205 96. ii 76.89 158 70 56 III 43-89 35-11 2O4 95-55 76.44 157 69.44 55'56 110 43-33 34.67 203 95 76 156 68.89 55-n 109 1 42.78 34-22 2O2 94-44 75.56 i55 68.33 54.67 108 42.22 33.78 2OI 93-89 75-n 154 67-78 54.22 107 41.67 33.33 200 93-33 74.67 i53 67.22 53-78 106 41.11 32.89 199 92.78 74.22 152 66.67 53-33 105 40-55 32.44 198 92.22 73.78 151 66.11 52-89 104 40 32 iQ7 91.67 73-33 150 65.55 52.44 103 39-44 31.56 196 91.11 72.89 149 65 52 IO2 38.89 31.11 J 95 90-55 72.44 148 64.44 51-56 IOI 38.33 30.67 194 90 72 i47 63.89 51.11 100 37.78 30.22 193 89.44 71.56 146 63.33 50.67 99 37-22 29.78 192 88.89 71.11 i45 62.78 50.22 98 36.67 29-33 191 88.33 70.67 144 62.22 49.78 97 36.11 28.89 100 87.78 70.22 M3 61.67 49-33 96 35.55 28.44 189 87.22 69.78 142 6i.n 48.89 95 35 28 188 86.67 69-33 141 60.55 48.44 94 34-44 27.56 187 86.11 68.89 140 60 48 93 33.89 27. II 1 86 85.55 68.44 139 59-44 47-56 92 33-33 26.67 185 85 68 138 58.89 47.11 91 32-78 26.22 184 84.44 67.56 i37 58-33 46.67 90 32.22 25.78 183 83-89 67. ii 136 57-78 46.22 89 31.67 25.33 182 83-33 66.67 i35 57-22 j 45.78 88 31.11 24.89 181 82.78 66.22 i34 56.67 45-33 87 30-55 24-44 180 82.22 65.78 i33 56.11 1 44.89 86 30 24 179 81.67 65-33 132 55-55 44-44 85 29.44 23.56 178 8i.ii 64.89 131 55 44 84 28.89 23.11 177 80.55 64.44 180 54-44 43-56 83 28.33 22.67 176 j 80 64 129 53-89 43-H 82 27.78 22.22 175 79-44 63.56 128 53-33 42.67 81 27.22 21.78 174 78.89 63. II 127 52.78 42.22 80 26.67 21-33 i73 78.33 62.67 126 52.22 41.78 79 26. ii 20.89 172 77.78 62.22 125 51-67 41-33 78 25-55 20.44 171 77.22 61.78 124 51-11 40.89 77 25 20 170 76.67 61.33 123 50.55 40.44 76 24.44 19.56 169 76.11* 60.89 122 50 40 75 23.89 ig.II 168 75-55 60.44 121 49-44 39-56 74 23-33 18.67 167 75 60 120 48.89 39-n 73 22.78 18.22 166 74-44 59.56 119 48.33 38.67 72 22.22 17.78 178 SUGAR ANALYSIS. Fah- ren- heit. Centi- grade. Reaumur. Fah- ren- ' heit. Centi grade. Reaumur. Fah- ren heit. Centi- grade. Reaumur. o o o 71 70 21.67 21 . II 17.33 16.89 M 0.55 0.44 4 -5 -20 -20.55 -16 -16.44 69 20-55 16.44 31 0.55 -0.44 -6 21 . II 16.89 68 20 16 30 I. II -0.89 -7 21.67 -17-33 67 19.44 15-56 29 -1.67 -1.33 -8 22.22 -17.78 66 18.89 15.11 1 28 2.22 -1.78 -9 -22.78 18.22 ^5 18.33 14.67 27 -2. 7 8 2.22 -10 23-33 -18.67 64 17.78 14.22 26 -3-33 2.67 II -23-89 19. ii 63 17.22 13.78 25 3-89 -3-II 12 24.44 -19.56 62 16.67 13-33 24 -4-44 -3.56 -13 -25 20 61 16.11 12.89 23 -5 4 14 25-55 20.44 60 15.55 12-44 22 -5-55 4-44 26.11 20.89 59 15 12 21 -6. ii -4.89 16 26.67 -21-33 58 14.44 11.56 20 -6.67 -5-33 -17 27.22 21.78 57 13-89 II. II 19 -7.22 -5.78 -18 27. 78 22.22 56 13.33 10.67 18 -7-78 -6.22 -19 -28.33 22.67 55 12.78 10.22 17 -8-33 6.67 -20 28.89 -23.11 54 12.22 9.78 16 -8.89 7.II 21 -29.44 -23.56 53 11.67 9-33 15 9-44 -7.56 22 -30 -24 52 II. II 8.89 14 10 -8 23 30.55 24.44 5* 10-55 8.44 13 10.55 -8-44 -24 -31.11 -24.89 50 IO 8 12 ii. ii -8.89 25 -31.67 -25-33 49 9.44 7.56 II 11.67 -9-33 26 32.22 -25.78 48 8.89 7. ii 10 12.22 --9.78 -27 -32.78 26.22 47 8.33 6.67 9 12.78 10.22 -28 -33-33 -26.67 46 7-78 6.22 8 -13-33 IO.67 -29 -33.89 27.11 45 7.22 5-78 7 -13.89 II. II -30 -34-44 27.56 44 6.67 5-33 6 14-44 11.56 31 -35 -28 43 6. ii 4.89 5 -15 12 -32 -35-55 -28.44 42 5-55 4-44 4 -15-55 12.44 ! -33 36.11 28.89 5 4 3 16. ii 12.89 | -34 -36.67 -29.33 40 4-44 3.56 2 -16.67 -13-33 35 37-22 39 3-89 3.H I -17.22 -I3.78 -36 -37.78 3O.22 38 3-33 2.67 -17-78 14.22 -37 -38.33 -30.67 37 2.78 2.22 i -18-33 -I4.67 -38 -38.89 31. II 36 2.22 1.78 2 -18.89 -15.11 -39 39-44 -3L56 35 1.67 1-33 -3 -19.44 -40 -40 -32 34 I. II 0.89 XIX. TABLES FOR CONVERTING CUSTOMARY AND METRIC WEIGHTS AND MEASURES. UNITED STATES COAST AND GEODETIC SURVEY. OFFICE OF STANDARD WEIGHTS AND MEASURES. T. C. MENDENHALL, Superintendent. WASHINGTON, D.C., 1890. [Authorized Reprint.'} 180 SUGAR ANALYSIS. CUSTOMARY TO METRIC. Inches LINEAR. Feet Yards Miles CAPACITY. Fluid drams T?, - , to milli- _ iq _ uld _ Quarts to milli- to to to kilo- litres or ounces *.._ . Ill: to Gallons metres. metres. metres. metres. cubic centi- to mull- litres. litres. to litres. metres. I _ 25.4000 0.304801 0.914402 1.60935 i = 3-70 29-57 0.94636 3-78544 2 = 50.8001 o . 609601 1.828804 3.21869 a = 7-39 sg^s 1.89272 7-57088 3 76.2001 0.914402 2 . 743205 4.82804 3 = 11.09 88.72 2.83908 11.35632 4 = 101 .6002 1.219202 3.657607 6-43739 4 - 14.79 118.30 3-78544 15.14176 127.0002 I . 524003 4.572009 8.04674 5 = 18.48 147.87 4.73180 18.92720 6 = 152.4003 I . 828804 5.486411 9.65608 6 = 22.18 177-44 5.67816 22.71264 7 = 177.8003 2.133604 6.400813 11.26543 7 = 25.88 207.02 6.62452 26.49808 8 =' 203 . 2004 2.438405 7.315215 12.87478 8 = 29.57 236.59 7-57088 30.28352 9 = 228.6004 2 743205 8.229616 14.48412 9 33-28 266.16 8.51724 34.06896 SQUARE. WEIGHT. Square inches to square centi- Square feet to square deci- metres. Square yards to square metres. Acres to hec- tares. Grains to milli gramme Avoirdu- pois Avoirdu- pois Troy pounds to ounces to kilo- grammes. metres. . grammes. x - 6.452 9 290 0.836 0.4047 i = 64.7989 28.3495 0-45359 31.10348 2 12.903 18.581 i .672 0.8094 2 = I2 9-5978 56.6991 0.90719 62 . 20696 3 = !9-355 27.871 2.508 1.2141 3 194.3968 85.0486 i . 36078 93.31044 4 25.807 37.161 3-344 1.6187 '4 = 259.1957 113.3981 1.81437 124.41392 S 32.258 46.452 4.181 2.0234 5 = 323.9946 141.7476 2.26796 1 55-5 I 74Q 6 38.710 55-742 5- OI 7 2.4281 6 = 388.7935 170.0972 2.72156 186.62089 7 45.161 65.032 5-853 2.8328 7 = 453-5924 198.4467 3-I75I5 217.72437 8 74-323 6.689 3-2375 S = 518.3914 226.7962 3-62874 248.82785 9 = 58^065 83.613 7-525 3.6422 g 2 55- I 457 4.08233 279.93I33 CUBIC. Cubic inches Cubic Cubic Bushels to feet to yards to to cubic cubic cubic hecto- centi- metres. metres. litres. metres. j = 16.387 0.02832 0.765 0.35242 | i chain r= 20.1169 metres. a = 32-774 0.05663 1.529 0.70485 i square mile = 259 hectares. 3 =r 49.161 0.08495 2.294 1.05727 i fathom = 1.829 metres. 4 = 65-549 o. 11327 3-058 1.40969 i nautical mile = 1853.27 metres. 5 = 81.936 0.14158 3 823 i .76211 i foot = o - 04801 metre, 9.4840 58 log. 6 _ 98.323 114.710 0.16990 o. 19822 4-587 5-352 2.11454 2.46696 i avoir, pound = 15432-35639 g rains = 453.5924277 gram, i kilogramme. 8 131 097 0.22654 6.116 2.81938 9 147.484 0.25485 6.881 3-17181 SUGAR ANALYSIS: 181 METRIC TO CUSTOMARY. LINEAR. Metres Metres Metres inches. tofeet ' yards. Kilo- metres to miles. CAPACITY. Millili- fluid to gal- to drams. i = 39-3700 3.28083 i .093611 0.62137 i = 0.27 0.338 1.0567 2.6417 2.8375 2 = 78.7400 6.56167 2.187222 1.24274 a = 0.54 0.676 2.1134 5.2834 5.6750 3 = 118.1100 9-84250 3.280833 1.86411 3 = 0.81 1.014 3.1700 7.9251 8.5125 4 = 157.4800 I3-I2333 4.374444 2 48548 4 = 1.08 1 35 2 4.2267 10.5668 11.3500 i = 196.8500 := 236.2200 16.40417 19.68500 5.468056 6.561667 3 . T 068 5 3.72822 5 6 = 5.6* 1.691 5 2834 13.2085 14.1875 2.029 6.3401 15.8502 17.0250 7 =. 275.5900 22.96583 7.655278 4-34959 7 *= 1.89 2.368 7.3968 18.4919 19.8625 S = 314.9600 26.24667 8.748889 4.97096 8 2.16 2.706 8.4534 21.1336 22.7000 9 = 354-3300 29-52750 9.842500 5-59233 9 = 2.43 3-43 9-5 J oi 23.7753 25.5375 SQUARE. WEIGHT. Square centi- metres to Square metres to Square metres to Hec- tares to Milli- grammes Hecto- v"ir> K"o- S ToT S * grammes , to pounds square inches. square feet. square yards. acres. to grains, to grains, f^o^es avoirdu - av. ' pois< x = 0.1550 10.764 1.196 2.471 i = 0.01543 15432.36 3-5274 2.20462 2 = 0.3100 21.528 2.392 4.942 2 = 0.03986 30864.71 7.0548 4.40924 3 = 0.4650 32.292 3-588 7-413 3 = 0.04630 46297.07 10.5822 6.61386 4 = o . 6200 43-055 c? R in 4.784 9.884 4 = 0.06173 61729.43 14.1096 8.81849 5 6 jo ' y 64.583 7.176 * 2 * 355 14.826 5 6 = 0.09259 92594.14 21.1644 13.22773 7 = 1.0850 75-347 8.372 17.297 7 = 0.10803 108026.49 24.6918 i5-43 2 35 S = I . 2400 86 . i i i 9-568 19.768 8 = 0.12346 123458.85 28.2192 17.63697 9 = 1-3950 96.874 10.764 22.239 9 = 0.13889 138891.21 31.7466 19.84159 CUBIC. WEIGHT. -(Continued.) Cubic centi- metres to cubic inches. Cubic deci- metres to cubic inches. Cubic metres to cubic feet. Cubic metres to cubic yards. Quintals to pounds av. Milliersor Grammes to pounds av. ounces, Troy. i = 0.0610 61 .023 35-3*4 1.308 i = 220.46 2204.6 0.03215 2 = 0.1220 122.047 70.629 2.616 ' 2 = 440.92 4409.2 0.06430 3 = 0.1831 183 070 105.943 3-924 3 661.38 6613.8 0.09645 4 = 0.2441 244.093 141.258 5.232 4 881.84 8818.4 0.12860 S 0.3051 305-117 176.572 6.540 = 1102.30 11023.0 0.16075 6 = 0.3661 366.140 211.887 7.848 6 = 1322.76 13227.6 0.19290 7 = 0.4272 427.163 247.201 9- I s6 7 = 1543.22 15432.2 0.22505 8 = 0.4882 488.187 282. 516 10.464 g = 1763.68 17636.8 0.25721 <) 0-5492 549-2io 317.830 11.771 9 = 1984.14 19841.4 0.28936 INDEX. A PAGE Acidity, determination of 31 Alkalinity, determination of 80 Analyses, reports on sugar 98 Analysis-schemes for organic acids 85 Angle of rotation 6 Ash, determination of: method of carbonization 79 " " Scheibler's method 77 " " Von Lipprnann's method 78 Ash, quantitative analysis of sugar 79 Average samples, preparation of 24 B Balances, examination of 21 " qualities of good. 21 Baume hydrometer 13 " " scale of 14 testing 15 Brix (Balling) hydrometer. ... . . 13 " " scale of 14 " testing , 15 C Calculation of the weight of solids and liquids from their specific gravity 107 Cane-juice analysis, report on 102 Casamajor's method of determining the exponent 40 Cellulose, pure, determination of 96 Chandler, and Ricketts, method of 51 Circular polarization 2 Clerget's inversion method 44 Color, determination of 25 Colorimeters 26 Control tube 11 Covers of polariscope tubes, examination of 13 183 184 INDEX. D PAGE Decoloriz&tion of dark sugar solutions 34 Densimetric degrees 14 Density of solutions, determination of * 26 Dextrose in sugar, gravimetric method of determination 54 " " qualitative tests for 49 " " quantitative methods of determination 51 Dextrose solution for standardizing Fehling's solution 68 Dutch standards , 25 Duty on sugar, United States of America 106 E Exponent * 38 F Fehling's solution, formula of 65 Flasks, graduation of 18 G Glass spheres, for density determinations , 28 Graduated glass vessels, verification of 19 Graduation of flasks , 18 H Hot polarization, method of 51 Hydrometers, varieties of 13 ' ' range of scales of 14 1 ' methods of testing 15 Hydrostatic balance, Mohr's 29 I Inversion, Clerget's method of 44 Invert-sugar, Bodenbeuder and Scheller's method of determination 74 " " Fehling's method of determination 66 " ' ' Meissl-Herzf eld's method of determination 69 " " Soxhlet's method of determination 65 5' " qualitative examination for 64 " " quantitative determination of 65 L Lsevulose, Sieben's process for destruction of 59 Light, polarization of 1 Literature on sugar-analysis, references to 110 INDEX. 185 M PAGE Methyl-blue test for invert-sugar. . . 64 Molasses, sampling of. 24 N Nitrogenous substances, list of , 84 Nitrogen, total, determination of 95 Non-nitrogenous organic substances, determination of 96 " list of 84 Normal weights. , 5 Opalescence in sugar solutions 1 34 Optically inactive sugar .' , 101 Organic acids, list of 84 " " schemes of analysis , 85 Organic non-sugar, determination of ' 83 P Polarimeters, see polariscopes 3 Polariscopes 3 ' ' adjustment of 6 " examination of , 9 " principle of construction 3 Polariscope-covers, examination of 13 Polariscope-tubes, examination of 13 Polarization, circular 2 Polarization of light 1 Preparation of solutions for polariscope 34 Quartz-plates 11 " measurement of 11 Quartz, right-rotating and left-rotating. . . 2 Quotient of purity 38 " " true and apparent 40 R Raffinose, determination of 46 " literature on determination of 47 Reducing-sugar, nature of 101 Rendement, calculation of, in various countries 105 " Payen-Scheibler method of determination 102 Reporting sugar-analyses , 98 Rotation, angle of 6 186 INDEX. S PAGE Saccharimeter, adjustment of 6 Saccharimeter-degrees, equivalence of 6 Saccharimeters, examination of 9 " optical parts of 4 " scales of 5 Sampling sugars and molasses 23 Sample, preparation of average. 24 Schmitz's table for use in testing saccharimeters 10 Sieben's process for destruction of laevulose 59 Soldaini's solution 74 Specific-gravity flask 26 Specific-gravity hydrometer, scale of 14 testing of 15 Spberometer, construction and use of 11 Stammer's colorimeter 26 Sucrose, gravimetric determination of 42 " optical determination of, with balance 33 " optical determination of, without balance, 36 " dextrose, and laevulose, determination of 60 " in presence of dextrose 49 ' ' in presence of raffinose 46 Sugar-analysis, literature on '. 110 Sugar-mite, detection of 82 Sulphurous oxide, test for 32 Suspended impurities, determination of 80 Synonyms in nomenclature 108 T Table I. Relation between specific gravity, degrees Brix and degrees Baume, for pure sugar solutions from to 100 per cent 115 II. Corrections for temperature in determinations by the specific- gravity hydrometer .... 129 III. Corrections for temperature in determinations by the Brix hy- drometer 131 IV. Factors: arranged for specific-gravity determinations 133 V. Factors: arranged fer Brix determinations 135 VI. Estimation of percentage of sugar by weight, in weak sugar solutions , 137 VII. " Hundred Polarization" 139 VIII. For use with solutions prepared by addition of one-tenth volume of basic acetate of lead 143 IX. Pounds solids per cubic foot in sugar solutions 153 X. Factors for the calculation of Clerget inversions 155 INDEX. 187 PAGE Table XI. Determination of total sugar 157 XII. Determination of invert-sugar : volumetric method. (Using Fehling's solution.) , 159 XIII. Determination of invert-sugar: gravimetric method. (Using Fehling's solution.) 161 XIV. Determination of invert-sugar: gravimetric method. (Using Soldaini s solution.) 163 XY. Determination of dextrose 165 XVI. Determination of Isevulose 169 XVII. Density of water at the temperatures from to 50 Centigrade, relative to its density at 4 Centigrade 173 XVIII. Comparison of thermometric scales 175 XIX. Tables for converting customary and metric weights and meas- ures 179 Thermometers, conversion formulae 21 " . verification of 20 V Ventzke's method of determining exponent 39 Verification of graduated glass vessels ,...." 19 Verification of thermometers 20 W Water, determination of . . : 76 Weights, verification of 22 Woody fibre, determination of 82