A O A C O f fic ia l M e t h o d s of A n a l y s is (1990)
tify. Tablets contg HgCl2, K2Cr:0 7, or other suitable preserv­
ative, >0.5 g active ingredient per tablet for each 8 fl oz (250
mL) milk, but total wt of such tablet <1 g, or 36% soln of
HCHO, 0.1 mL (2 drops) per fl oz (30 mL), may be used
unless presence of preservative is objectionable in physical or
chem. tests to be made in addn to detn of fat. If phosphatase
test is to be made, only CHC13 can be used as preservative,
and stoppers must be of phenol-free material such as red rub­
ber.
925.21 Preparation of Milk Sample
Procedure
Bring sample to ca 20°, mix until homogeneous by pouring
into clean receptacle and back repeatedly, and promptly weigh
or measure test portion. If lumps of cream do not disperse,
warm sample in H20 bath to ca 38° and keep mixing until
homogeneous, using policeman, if necessary, to reincorporate
any cream adhering to container or stopper. Where practical
and fat remains dispersed, cool warmed samples to ca 20° be­
fore transferring test portion.
When Babcock method, 924.05C, is used, adjust both fresh
and composite samples to ca 38°, mix until homogeneous as
above, and immediately pipet portions into test bottles.
925.22 Specific Gravity of Milk
Pycnometer Method
Procedure
Det sp gr at 15.6/15.6° with pycnometer or std hydrometer.
975.16 Somatic Cell Count in Milk
First Action
See 973.68. 978.25, 978,26.
947.05 Acidity of Milk
Titrimetric Method
Final Action
Measure or weigh suitable amt (ca 20 mL or 20 g) sample
into suitable dish and dil. with twice its vol. C 0 2-free H20 .
Add 2 mL phthln, and titr. with 0.1 N NaOH to first persistent
pink. If measured vol. sample was used, det. its wt from sp
gr of sample. Report acidity as % lactic acid by wt. (1 mL
0.1 N NaOH = 0.0090 g lactic acid.) If Babcock milk pipet,
924.05A(b), is used, mL 0. IN NaOH required -f 20 = % acid
as lactic acid.
Results may also be expressed as mL 0.1 N NaOH/100 g
sample.
Refs.: JAOAC 30, 130(1947); 34, 239(1951).
932.05 Citric Acid in Milk
Gravimetric Method
Final Action
A. Preparation o f Sample
To 50 g milk in 150 mL beaker, add ca 100 mg tartaric
acid and 6 mL IN H2S 0 4, and heat on steam bath 15 min.
M ilk 805
Immediately add 3 mL 2 0 % p h o s p h o t u n g s t ic a c i d s o ln , mix
well, and return to steam bath for 5 min. Transfer to 250 mL
vol. flask with alcohol, cool, dil. to vol. with alcohol, mix,
and filter thru folded paper. Pipet 200 mL clear filtrate into
centrf. bottle.
B. R e a g e n ts
(a) P o ta s s iu m p e r m a n g a n a te s o l n . — Dissolve 5 g KM n04
in H:0 and dil. to 100 mL.
(b) F e r r o u s s u lfa te s o l n . — Dissolve 200 g FeS04.7H20 in
H20 , dil. to 500 mL with H20 , and add 5 mL H2S 0 4.
(c) L e a d a c e ta te s o l n . — Dissolve 75 g Pb(0Ac)2.3H20 in
H20 , add 1 mL HOAc, and dil. to 250 mL.
C. D e te r m in a tio n
To soln in centrf. bottle add 10 mL Pb(OAc)2 soln. shake
vigorously ca 2 min, and centrf. 15 min at ca 1000 rpm. Care­
fully decant supemate from pptd Pb salts and test with little
Pb(OAc)2 soln. If ppt forms, return to centrf. bottle, add more
Pb soln, shake, and again centrf. If sediment lifts, centrf. again,
increasing speed and time, and decant. Invert bottle and drain
thoroly several min. To Pb salts in centrf. bottle add ca 150
mL H20 , shake thoroly, and sat. with H2S. Transfer to 250
mL vol. flask, dil. to vol. with H20 , mix, and filter thru folded
paper.
Evap. 200 mL filtrate to ca 20 mL, rinse into 250-300 mL
tared, g-s erlenmeyer, and adjust with H:0 to net wt of ca 40
g. Add 2 g KBr and 5 mL H2S 0 4, and. if necessary, heat to
ca 50° and let stand 5 min. Slowly (1-2 mL portions) add 20
mL KM n04 soln from pipet or buret, swirling flask few sec
after each addn. Let stand undisturbed 5 min and cool to 15°.
Slowly add FeS04 soln with const agitation until mixt. starts
to clear. Shake 1 min, continue addn of FeS04 soln until MnO:
is dissolved, and add few mL excess. Add 20 g anhyd. Na2S 0 4,
with swirling to assure soln (if Na2S 0 4 remains substantially
undissolved, repeat detn). Cool to 15° and shake vigorously 5
min.
Immediately, while still cold, collect pentabromacetone ppt
on asbestos in gooch and wash residual ppt from flask with
portion of filtrate. Wash crucible with 50 mL cold H:0 and
leave under suction few min. Dry crucible overnight in H2S 0 4
desiccator and weigh, or place crucible in drying train and aer­
ate until loss in wt does not exceed few tenths mg, making
first weighing after 20 min.
Remove pentabromacetone from crucible with alcohol fol­
lowed by ether, filling crucible 3 times with each solv. Dry
crucible 10 min at 100°, cool in desiccator, and weigh. Dif­
ference in 2 wts = wt pentabromacetone. Calc, g anhyd. citric
acid from formula: X = 0.424P. where X = g citric acid in
aliquot; P — g pentabromacetone: and 0.424 = theoretical fac­
tor for converting pentabromacetone to anhyd. citric acid. An­
hyd. citric acid in sample taken for analysis = X/0.64.
For drying pentabromacetone by aspiration, use app. shown
in Fig. 9 3 2 . 0 5 . where A is gooch, 28 mm diam., loosely packed
with cotton; B is gooch, 35 mm diam., for pentabromacetone:
and C is 500 mL suction flask. Dry air by passing thru H2S 0 4
and soda-lime, and finally filter thru cotton. Cool air entering
drying train by passing thru spiral condenser cooled with H20 .
Let crucible, B , contg pentabromacetone, remain under suc­
tion ca 1 min to remove surface moisture before placing in
app. If air does not pass thru freely, place crucible in desic­
cator short time. Maintain slow uniform flow of air by just
“cracking” suction.
Refs.: JAOAC 15, 643(1932); 16, 427(1933).
CAS-77-92-9 (citric acid)