120 ASSOCIATION OF OFFICIAL AGRICULTURAL CHEMISTS [Vol. II, No.

WATER IN FOODS AND F E E D I N G STUFFS.

BY W. J. M C G E E (Food and Drug Inspection Laboratory,

U. S. Custom House, Savannah, Ga.), Referee.

The principal object of this year's work was the study of the method
of drying without heat in a vacuum over sulphuric acid. The following

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outline of the method was sent out for trial:
DRYING IN VACUO WITHOUT HEAT.—OPTIONAL.

(This method was first suggested by Mr. Trowbridge at the meeting

of the Association in 1909; approved in 1913 for final action as an optional
official method in 1914; final action not yet taken.)
Mix the sample thoroughly and weigh about 2 grams by difference from a stop-
pered weighing bottle into tared crucibles provided with covers which are tared
with crucibles. Place 200 cc. of fresh C. P. sulphuric acid in a good 6 inch vacuum
desiccator. Put triplicate samples in the desiccator, smea r t he edges of the latter and
the stop-cock with lubricant (a mixture of 3 parts of hard paraffin and 5 of vaseline)
and exhaust by means of a vacuum pump. If a pump is not available, place 10 cc.
of ether contained in a small beaker in the desiccator and exhaust with a water
filter pump. It will be found convenient to interpose between the pump and the
desiccator an empty bottle next to the desiccator and a bottle of water following
this. Draw the air from the desiccator through the water and turn the desiccator
stop-cock at just the instant when the water begins to rise in the tube leading from
the empty bottle. Gently rotate the desiccator 4 or 5 times during the first 12 hours
to mix the sulphuric acid with the water which has collected as an upper layer. At
the end of 24 hours open the desiccator, forcing the incoming air to bubble through
C. P. sulphuric acid. If a good vacuum has been maintained the samples are ready
for the first weighing. After weighing place in a desiccator with fresh C. P. sulphuric
acid and exhaust as before. Rotate the desiccator once or twice during the interval
and weigh again at the end of 24 hours, repeating this process of drying in vacuo over
sulphuric acid until the weight is constant.

REPORTS OP COLLABORATORS.

W. D. Richardson: Sausage meat (vacuum method).—Constant weight in about

208 hours with a loss in weight of about 1% less than by the heating methods.
D. B. Bisbee: Cheese (vacuum method).—Weight nearly constant eighth day.
Loss of weight about 0.4% less than by heating methods.
/ . 0. Clarke: Cottonseed meal (vacuum method).—Weight practically constant in
9-15 days with loss about the same as in heating methods.
Corn meal.—In vacuum desiccator dried to approximately constant weight in 4
days and the loss was about 0.4% less than by heating methods.
Tomato ketchup.—With water content of 83.11% as indicated by heating at 100°C.
in water oven, lost 80.15% in vacuo over sulphuric acid in 5 hours, and 81.21% in
5 days. In another experiment lost 80.53% in 18 hours and 80.72% in 42 hours. Both
of these experiments were terminated by accident before constant weight was
attained.
1916] MCGEE: WATER IN FOODS AND FEEDING STUFFS 121

Hamburger steak.—In vacuo over sulphuric acid lost 70.42% of its weight in 4 days;
by heating methods, 71.09%.
Lean meat.—Ground fine lost 65.56% in 44 hours and 67.10% by heating methods.
Apple jelly.—Lost 21.66% in 48 hours and 27.45% in vacuum oven at 70°C.
Cattle Food Laboratory, U. S. Bureau of Chemistry: Comparison of this method
with drying at 100°C. at the house vacuum (average 86.4) gave the following results:
Mixed alfalfa, molasses, corn feed at 100°C.—Average pressure .86.4 mm. Mois-
ture, 3.60%.

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At 27"C.—Average pressure 7.5 mm. Moisture 1.89%.
Bran at 100°C.—Average pressure 86.4 mm. Moisture 10.79%.
At S7°C—Average pressure 7.5 mm. Moisture 10.43%.
Linseed meal at 100°C.—Average pressure 86.4 mm. Moisture 10.86%.
At 27°C—Average pressure 7.5 mm. Moisture 10.71%.

TABLE 1.
Moisture determinations under varying conditions.
(J. H. Roop, Indiana.)
D R I E D I N 6 INCH
DRIED 5 HOURS I N VACUUM DESICCA-
D R I E D 5 H O U R S TN
SUBSTANCE HYDROGEN TOR W I T H S U L -
AT 100° C . VACUO AT 7 5 ° C . P H U R I C ACID
AVERAGE

Per cent loss Per cent loss Per cent loss

Cottonseed meal 8.75 8.10 7.55

Wheat bran 11.65 11.27 11.04
Corn germ meal 4.82 4.45 4.36
Linseed meal 9.97 9.57 9.15
Corn and oats 13.01 12.42 12.68
Distillers' grains 8.90 7.95 7.64

C. 0. Swanson: This method has been in use at the Kansas Agricultural College
for several years and is considered very satisfactory. For flour the drying is con-
tinued for from 3-5 days. Very moist samples are allowed to remain in the desiccator
for 3 weeks. A shaking machine is employed to keep the acid stirred up.

COMMENTS BY T H E REFEREE.

It has been found at the U. S. Food and Drug Inspection Laboratory at Savannah
that the desiccator acid containing ether and water can be recovered by digesting
for about 4 hours over a free flame in a Kjeldahl flask with a drop of mercury. A
study of this method from the work of this and previous years seems to show that it
can be relied upon when heating the sample is inadmissible; and that it is valuable
also when subsequent fat extraction is contemplated and heating would tend to
harden the sample too much. For work of this kind in which time is not a factor it
may be very convenient to have an official method.
122 ASSOCIATION OF OFFICIAL AGRICULTURAL CHEMISTS [VOL. II, NO. 2

TABLE 2.
Comparison of dehydrating powers of reagents used in desiccators at room temperature
0/ 20°-3S°C. and ai atmosph eric pressure.
SULPHURIC CALCIUM SODIUM CALCIUM CALCIUM SODIUM
ACID CABBID METAL OXID CHLOHID HYDROXID

Days Per cent Per cent Per cent Per cent Per cent Per cent
loss loss loss loss loss loss

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Corn meal 1 : 1 10.18 10.06 9.54 9.22 7.76
2 11.13 10.85 10.69 9.84 8.72
3 • 11.49 11.22 11.09 10.05 9.21
4 11.60 11.29 11.03 10.02 9.06
5 11.74 11.43 11.20 10.10 9.19
6 11.82 11.54 11.22 10.14 9.28
7 11.87 11.53 11.30 10.14 9.23

Lean meat, finely 1 43.70 36.20 45.23 28.77

ground 2 : 2 65.15 63.22 62.69 56.41
3 66.04 65.50 63.53 64.08
4 66.40 65.97 63.89 64.75
5 66.56 66.10 63.98 64.90
6 66.65 66.27 64.13 65.12
7 66.78 66.38 64.23 65.25
10 66.98 66.62 64.40 65.50
Hours
Hamburger steak 3 : 3 9.00 11.93 8.73
Days
1 59.26 62.17 54.74
2 69.50 69.40 69.15
3 70.16 69.97 69.82
4 70.47 70.24 70.14

Tomato paste4: 1 77.51 40.16 77.10 77.32

2 77.67 76.40 77.35 77.54
3 77.98 77.10 77.50 77.64
Glucose and apple 1 18.91 19.59 17.84 16.43
jelly 6 : 2 19.62 18.07 16.57

Pure apple jelly 6 : 1 19.29 20.44 18.90

2 20.17 20.84 19.78
3 21.11 20.19
1
Vacuum oven 12.60%; in hydrogen 13.51%.
* Loss at 100°C., 67.10%.
a Loss at 100°C., 71.09%.
'Vacuum
s oven at 70°C, 78.4%.
Vacuum oven at 70°C, 23.83%.
•Vacuum oven at 70°C, 27.45%.

It appears from this work and from the experience of previous years, particularly
as reported at the meeting in 1913, that calcium carbid is a desiccator reagent nearly
as efficient as sulphuric acid and one that is portable. This reagent is good until a
large percentage of the lumps have loosened up into powder.
It will be best, however, to continue using sulphuric acid, lime or calcium chlorid
for precipitates of copper suboxid.
Leaving phosphorus pentoxid out of the question on account of its high cost and
its rapid decrease in efficiency, it appears that the 3 best desiccator reagents are
sulphuric acid, calcium carbid and calcium oxid, in the order named.
1916] BIDWELL: FOODS AND FEEDING STUFFS 123

RECOMMENDATIONS.
It is recommended—
(1) That further work be done in comparing the drying of various
food and feeding products over sulphuric acid, calcium carbid and cal-
cium oxid, with any other reagents thought desirable, at atmospheric
pressure and in a partial vacuum.

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(2) That the method of drying without heat over sulphuric acid as
outlined above be finally made an official optional method.
DISCUSSION.
P. F. Trowbridge: Mr. Grindley of the University of Illinois has used the method
with good results—much better than we have been able to obtain at our Missouri
Laboratory. Some materials present difficulties because they dry to a horn-like
substance. The referee has not sufficiently emphasized the need for a good vacuum.
Seven millimeters of mercury are not enough. A pump is necessary. With a pres-
sure not exceeding 1 mm. it is possible to obtain from 2-10% more moisture from
grain than by drying at 102°C.

REPORT ON FOODS AND FEEDING STUFFS.

BY G. L. BIDWELL (Bureau of Chemistry, Washington, D. C ) , Referee.
The cooperative work this year was all in charge of associate referees.
It is recommended—
(1) That the method for the detection of oats bleached with sulphur
dioxid1, be made official.
(2) That the method for determining the acidity of corn2, be made
official.
(3) That the method for determining the acidity of corn be studied
to see if it is applicable to other materials.
(4) That the effect of preliminary drying on the ether extract content
of feeds be studied.
(5) That the use of toluol or other suitable substance as a preservative
for feed samples be studied.
(6) That the method of Bryan, Given and Straughn 3 for the estima-
tion of sugar in feeds be studied and made official.

F E E D ADULTERATION.
BY C. CUTLER (Agricultural Experiment Station, La Fayette, Ind.),
Associate Referee.
The work during the past year was confined to the following recommen-
dation, approved at the 1914 meeting:
"(1) That samples be sent out for the quantitative determination of
1
2
U. S. Bur. Plant Industry Circ. 40.
3
Ibid., Bull. 199; U. S. Dept. Agr. Bull. 102.
U. S. Bur. Chem. Circ. 71.