42.1.15 stant rate producing vigorous agitation without splashing.

Titrate
AOAC Official Method 971.27 with AgNO3 standard solution, adjusting increments with rate of
Sodium Chloride in Canned Vegetables voltage change so that accurate plot of mV against mL AgNO3 so-
Method III lution can be prepared. Add total of 50 mL AgNO3 solution to ob-
(Potentiometric Method) tain complete curve.
First Action 1971 Determine inflection point by drawing 2 straight lines with 45°
Final Action 1976 slope with respect to axes and tangent to titration curve at the
A. Principle 2 points of greatest curvature. Inflection point is at intersection of ti-
tration curve with line drawn parallel to, and midway between, other
Product is dispersed with H2O and acidified; soluble chlorides
2 lines. From volume AgNO3 solution used, calculate molarity and
are titrated potentiometrically with AgNO3. Applicable to levels
adjust to 0.0856M. Restandardize occasionally. Use inflection point
≥0.03% NaCl. For convenience in calculations, weights or vol- as end point in titrating test portions. Recheck end point potential oc-
umes and molarity are specified so that 1 mL AgNO3 = 0.1% NaCl. casionally, and redetermine when either individual electrode, com-
If balance permitting rapid weighing of specified weight is not bination electrode, or pH meter is replaced by preparing new
available, convenient weight test sample and molarity AgNO3 so- titration curve.
lution may be used. For greatest accuracy, when series of determinations on same
B. Apparatus food is performed, determine and use end point from titration curve
of that food rather than using end point obtained with NaCl standard
(a) Balance.—Capacity, ≥200 g, taring range, ≥100 g, readabil-
solution.
ity, ≤0.01 g. Mettler No. P1200 (replacement Model PM2000)
(Mettler-Toledo GmbH, PO Box VI-400, Sales International, E. Preparation of Sample
CH-B606 Greifenseel, Switzerland), or equivalent, is convenient. (a) Clear liquids with low viscosity.—(Fruit juices, clear soups,
(b) Electrodes.—Ag billet combination electrode (Beckman No. wines, etc.) Use directly.
39261, or equivalent), or separate indicating Ag (Beckman 39261, (b) Comminuted products.—(Tomato juice, tomato catsup,
Orion 94-17 [replaced by 94-17-BN], Fisher 13-639-122, or equiva- strained vegetables, etc.) Thoroughly shake unopened container to
lent), and glass reference (Beckman 39419, Orion 90-02 [replaced incorporate any sediment. Transfer entire contents to large glass or
by 90-02-00], Fisher 9-313-216, or equivalent) electrodes. Before porcelain dish and mix thoroughly, continuing stirring ≥1 min.
initial use and before each day’s use, if necessary, clean Ag billet Transfer to glass-stoppered container, and shake or stir thoroughly
electrode tip with scouring powder or other suitable material and each time before removing test portions for analysis.
rinse thoroughly with H2O. (Hot H2O may be required with some (c) General method for heterogeneous (f i sh, meat, etc.), low mois-
kinds of laboratory samples.) Clean other electrodes as recom- ture (cereal products, etc.), and hard-to-disperse, homogeneous (cheese,
mended by manufacturer. Reclean as frequently as necessary to pre- peanut butter, etc.) foods.—Weigh 50.0 g test sample into 1 L (qt) con-
vent drifting of end point reading. With some test samples, tainer of high-speed blender and add 450 g H2O. Cover, start blender at
periodically rinse electrodes with H2O and wipe with tissue to pre- low speed by use of variable transformer for initial dispersion, and blend
vent accumulation of film. It is unnecessary to coat Ag billet elec- thoroughly at high speed (1–2 min is usually adequate). Equivalent of 5 g
trodes with AgCl. test sample is conveniently dispensed through 50 mL pipet with tip cut
(c) Magnetic stirrer.—Operating through variable transformer off. Thoroughly mix test sample suspension immediately before
to permit range of speed which, once set, is constant. pipetting aliquot for analysis so that solid material is uniformly sus-
(d) pH meter.—Preferably direct reading, with scale divisions pended.
10 mV or less; range at least ±700 mV, e.g., digital type. (d) Other types of foods.—Prepare test sample by method (a),
C. Reagents (b), (c), or other suitable method.
To preserve test samples or sample suspensions for future analy-
(a) Nitric acid, dilute.—1 + 49. Dilute 20 mL HNO3 to 1 L with
sis, add 0.5 mL ca 37% HCHO solution/100 g sample or sample sus-
H2O.
pension, mix well, and store at room temperature. Correct for
(b) Silver nitrate standard solution.—0.0856M. Dissolve
dilution by HCHO solution by multiplying % NaCl by 1.005.
14.541 g AgNO3 in H2O and dilute to 1 L in volumetric flask. Stan-
dardize as in D, and adjust to exact molarity specified so that with in- F. Determination
dicated test sample weight, 1 mL = 0.1% NaCl. Store in Pyrex (a) For products containing less than 5 per cent salt.—Place 5.00 g
container out of direct sunlight. Solution is stable in room light. (or 5.00 mL if concentration is to be expressed on weight/volume basis)
(c) Sodium chloride standard solution.—0.0856M. Dissolve in prepared test sample from (a) or (b) or 50.0 g from (c) into tared 250 mL
H2O 5.000 g NaCl (if assay is <100.0% NaCl, divide 5.000 g by % beaker; add H2O to ca 50 mL if (a) or (b) is used. (Use boiling H2O with
NaCl/100 to obtain corrected weight), previously dried 2 h at 110°C, samples such as butter to melt fat.) Add 50 mL HNO3 (1 + 49). Titrate as
and dilute to 1 L in volumetric flask. in D, using 10 mL buret if salt content is ≤1%.
(d) Water.—Distilled or deionized, halogen-free by following
test: Add 1 mL ca 0.1M AgNO3 and 5 mL HNO3 (1 + 4) to 100 mL of
the H2O. No more than slight turbidity should be produced. NaCl, % = mL 0.0856M AgNO3/10

D. Standardization (b) For products containing 5 or more per cent salt.—Place

Pipet 25 mL NaCl standard solution into 250 mL beaker, dilute 5.00 g (or 5.00 mL if concentration is to be expressed on w/v basis)
to ca 50 mL with H2O, and add 50 mL HNO3 (1 + 49). Insert elec- prepared test sample from (a) or (b) into 100 mL volumetric flask
trodes, start magnetic stirrer, and stir throughout titration at con- and dilute to volume with H2O. Mix, and transfer aliquot containing

© 2000 AOAC INTERNATIONAL

50–250 mg NaCl to 250 mL beaker. If test sample is prepared by (c),
transfer weighed aliquot containing 50–250 mg NaCl to tared
250 mL beaker. Proceed as in D, beginning “…dilute to ca 50 mL
with H2O,…”.

NaCl, % = F × mL 0.0856M AgNO3/10

where F = dilution factor = 100/mL aliquot titrated if test sample is

prepared by (a) or (b) or 50/g aliquot titrated if prepared by (c).
(c) General case.—Accurately weigh approximately test sample
weight stated. (If % NaCl ≥5%, weigh <5 g sample rather than dilut-
ing to 100 mL, if more convenient.) Use ca 0.1M AgNO3 solution,
accurately standardized as in D, without adjusting to specific
molarity, and titrate as in D.

NaCl, % =
mL AgNO3 × M AgNO3 × 0.05844 × 100/g test sample

If test sample is overtitrated, add NaCl standard solution, and com-

plete titration. Correct for volume of standard solution added.
References: JAOAC 54, 471(1971); 57, 1209(1974).
CAS-7647-14-5 (sodium chloride)

© 2000 AOAC INTERNATIONAL