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