43.1.40
Total Phosphorus (2) (Final Action)
AOAC Official Method 930.35
Vinegars (1)
First Action 1930
(Unless otherwise directed, express results as g/100 mL.)
A. Organoleptic Examination (Procedure)
Note appearance, color, odor, and taste. Neutralize portion of
product with NaOH solution and note odor and taste. Extract
neutralized vinegar with ether, evaporate ether extract, and note
odor and taste of residue. (Spices and pungent materials are
indicated by characteristic odors and tastes.) Evaporate portion of
product on water bath. Odor of material as last of volatile matter
evaporates and appearance and taste of residue give information as
to source and character of vinegar.
B. Preparation of Test Sample (Procedure)
Mix thoroughly and filter through rapid paper.
C. Solids (Final Action) (Repealed First Action 1987)
Mea sure 10 mL prod uct into weighed 50 mm di am e ter,
flat-bottom Pt dish, evaporate on boiling water bath 30 min, and dry
exactly 2.5 h in oven at temperature of boiling water. Cool in
desiccator and weigh. (To obtain concordant results it is necessary to
use dish of size and shape stated and to dry exactly time specified.)
D. Ash (Final Action)
Measure 25 mL product into weighed Pt dish, evaporate to
dryness on H2O or steam bath, and heat in furnace 30 min at
500°–550°C. Break up charred mass in Pt dish, add hot water, filter
through ashless paper, and wash thoroughly with H2O. Return paper
and contents to dish, dry, and heat 30 min at ca 525°C, or until all C is
burned off. Add filtrate, evaporate to dryness, and heat 15 min at ca
525°C. Cool in desiccator and weigh (weight x). Reheat 5 min at ca
525°C, and cool £1 h in desiccator containing efficient desiccant.
Put 1 or 2 dishes (preferably only 1) in desiccator at a time. Place
weight x on balance pan before removing dish from desiccator, and
weigh rapidly to nearest mg. Calculate total ash from last weight.
E. Soluble and Insoluble Ash (Final Action)
Treat ash, D, as in 900.02D (see 44.1.05).
F. Alkalinity of Soluble Ash (Final Action)
Proceed as in 900.02E (see 44.1.05), using soluble ash obtained in
E. Express result as number mL 1M HCl required to neutralize
soluble ash from 100 mL vinegar. If relationship of ash to alkalinity
of soluble ash is abnormal, study composition of ash, especially
content of chlorides, sulfates, phosphates, and alkalies [J. Amer.
Chem. Soc. 22, 218(1900)].
G. Soluble Phosphorus (2) (Final Action 1965)
Proceed as in 964.06B (see 4.8.13), or 965.18C (see 25.1.15), or
935.45 (see 37.1.27), using solution obtained in F. If either volumetric
or colorimetric method is used, standardize with vinegar of known
phosphate content. Express results as mg P2O5/100 mL vinegar.
H. Insoluble Phosphorus (2) (Final Action 1965)
Dissolve H2O-insoluble ash, E, in ca 50 mL boiling HNO3 (1 + 8)
(use 25 mL H2SO4 [1 + 9] for colorimetric method) and proceed as in
964.06B (see 4.8.13), or 965.18C (see 25.1.15), or 935.45 (see
37.1.27). If either volumetric or colorimetric method is used,
standardize with vinegar of known phosphate content. Express
result as mg P2O5/100 mL vinegar.
I.
Dissolve ash, D, or both soluble and insoluble ash, E, in ca 50 mL
boiling HNO3 (1 + 8) (use 25 mL H2SO4 [1 + 9] for colorimetric
method) and proceed as in 964.06B (see 4.8.13), or 965.18C (see
25.1.15), or 935.45 (see 37.1.27). If ei ther vol u met ric or
colorimetric method is used, standardize with vinegar of known
phosphate content. Express result as mg P2O5/100 mL vinegar. If
desired, digest vinegar as in 935.45 (see 37.1.27), instead of using
ash from D.
J. Total Acids (Final Action)
Dilute 10 mL test portion with recently boiled and cooled water
until it appears only slightly colored and titrate with 0.5M alkali,
using phenolphthalein. 1 mL 0.5M alkali = 0.0300 g CH3COOH.
K. Nonvolatile Acids (Final Action)
Measure 10 mL test portion into 200 mL porcelain casserole,
evaporate just to dryness, add 5–10 mL H2O, and again evaporate;
repeat until ³5 evaporations have been made. Add ca 200 mL
recently boiled and cooled water, and titrate with 0.1M alkali, using
phenolphthalein. 1 mL 0.1M alkali = 0.00600 g CH3COOH.
L. Volatile Acids (Final Action)
Subtract nonvolatile acids, K, from total acids, J.
M. Total Reducing Substances Before Inversion (Final Action)
Measure 25 mL test portion into 50 mL volumetric flask and add
enough NaOH solution (1 + 1) to nearly neutralize acid. Cool, dilute
to volume with H2O, and determine reducing substances in 20 mL
solution as 906.03B (see 44.1.16). If amount of reducing substances
is very small, use 40 mL. Calculate result as invert sugar (for malt
vinegar as glucose).
N. Total Reducing Substances After Inversion (Final Action)
Invert 25 mL test portion in 50 mL volumetric flask with 5 mL
HCl, as in 925.48(b) or (c) (see 44.1.09). Nearly neutralize with
NaOH solution (1 + 1) and determine reducing substances as in
906.03B (see 44.1.16).
O. Nonvolatile Reducing Substances (Sugar) (Final Action)
(Useful in calculating nonsugar solids.)
Evaporate 50 mL test portion on steam or water bath to syrupy
consistency, add 10 mL H2O, and evaporate again. Repeat with
10 mL H2O. Transfer residue to 100 mL volumetric flask with ca
50 mL warm H2O. Cool, invert with 10 mL HCl as in 925.48(b) or (c)
(see 44.1.09), and nearly neutralize with NaOH solution (1 + 1).
Cool, di lute to vol ume with H 2 O, and de ter mine re duc ing
substances in 20 or 40 mL, depending on amount present, as in
906.03B (see 44.1.16). Calculate result as invert sugar (for malt
vinegar as glucose). If results for total reducing substances before
and after inversion show absence of sucrose, inversion may be
omitted here.
P. Volatile Reducing Substances (3) (Procedure)
When sucrose is absent, subtract amount of nonvolatile reducing
substances, O, from mean of total reducing substances before
inversion, M, and after inversion, N. When sucrose is present,
subtract amount of nonvolatile reducing substances, O, from
amount of total reducing substances after inversion, N.
Q. Alcohol (Final Action)
Measure 100 mL test portion into round-bottom distillation flask.
Make faintly alkaline with NaOH solution (1 + 1), distil almost 50 mL,
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dilute to 50 mL at temperature of test sample, and determine specific
gravity at 20/20°C with pycnometer, 945.06C (see 26.1.06). Obtain %
by volume from 913.02 (see Appendix C). Undue foaming may be
avoided by adding small piece of paraffin, free from volatile
constituents.
R. Glycerol (4) (Final Action)
See 30.079–30.080, 12th Ed.
S. Color (Final Action)
Determine depth of color in Lovibond tintometer by good
reflected daylight, using 12.7–25.4 mm ( 12 or 1 in.) cell and brewer’s
scale. Report result in terms of 12.7 mm ( 12 in.) cell and so state.
T. Polarization (5) (Final Action)
When ever pos si ble, po lar ize in 200 mm tube with out
decolorizing. Report result on basis of 200 mm tube in °S,
925.46A(a) (see 44.1.07). When necessary, decolorize as follows:
(a) To 50 mL test portion add measured volume of saturated
neutral Pb(CH3COO)2 solution, avoiding excess of Pb; filter,
remove Pb with powdered anhydrous potassium oxalate, and filter.
Polarize and correct for dilution with Pb(CH3COO)2 solution.
(b) To 50 mL test portion add decolorizing C, avoiding excess or
too long treatment. Filter through double paper and polarize.
U. Sulfates (Final Action)
To 100 mL test portion add 2 mL ca 1M HCl, heat to bp, and add
10 mL hot BaCl2×2H2O solution (1 g/100 mL), dropwise. Continue
boiling 5 min, keeping volume ca constant by adding hot water as
required. Let mixture stand until supernate is clear (overnight is
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convenient, but this time should not be exceeded). Filter on ashless
paper or weighed Munroe crucible [Z. Anal. Chem. 2, 241(1888); J.
Amer. Chem. Soc. 31, 456, 928(1909)]. Wash Cl-free with hot water,
dry, ignite at red heat (700°–800°C), cool, and weigh. Express result
as mg SO3/100 mL vinegar.
V. Dextrin (Qualitative Test) (Procedure)
Evaporate 100 mL test portion to ca 15 mL. Slowly add 200 mL
alcohol, with constant stirring, and let stand overnight. Separate
precipitate, preferably by centrifuging, and wash with 80% alcohol.
Dissolve in minimum volume H2O and determine optical rotation.
Distinct optical rotation indicates dextrin. Treat solution with
several drops I2 solution of ca same color intensity. Formation of
reddish brown color indicates dextrin.
References: (1) JAOAC 8, 150(1924); 9, 440(1926);
10, 490(1927); 11, 499(1928); 14, 507(1931);
15, 535(1932); 16, 536(1933); 17, 360(1934);
21, 430(1938); 23, 586(1940); 25, 702(1942);
26, 233(1943); 29, 304(1946); 32, 336(1949);
45, 562(1962).
(2) JAOAC 24, 684(1941).
(3) J. Am. Chem. Soc. 39, 309(1917).
J. Ind. Eng. Chem. 5, 845(1913).
(4) USDA Bur. Chem. Bull. 137, 61.
JAOAC 3, 411(1920); 15, 535(1932); 18, 82(1935).
(5) JAOAC 5, 245(1921); 8, 151(1924);
14, 507(1931).
CAS-9004-53-9 (dextrin)