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9.2.

15
AOAC Official Method 974.13
Lead in Evaporated Milk
Anodic Stripping Voltammetric Method
First Action 1974
Final Action 1976
A. Principle
Evaporated milk is dry-ashed and residue is dissolved in dilute
HNO
3
. Pb is electroanalytically concentrated on hanging Hg drop or
Hg filmelectrode, and determined by reversing potential sweep and
measuring anodic current peak.
B. Apparatus
See 982.23B(a)(d) (see 9.1.02).
C. Ashing
Proceed as in 973.35D (see 9.2.14).
D. Preparation of Standard Curve
Prepare standards as in 973.35C(d) (see 9.2.14) and 1M HNO
3
re-
agent blank. Transfer 1020 mL standard solution to cell, depending
on cell capacity. Adjust to 25 1C, and bubble N
2
through solution
5 min. Adjust gas inlet tube to let N
2
flowgently above and across so-
lutionsurface. If hangingdropHgelectrode is used, addfresh drop Hg
to capillary tip with micrometer (Hg drop must be reproducible for
each measurement), turn on stirrer motor, and electrolyze solution
110 min at 0.6 Vagainst saturated calomel electrode (time depends
on manufacturers instructions). Stop stirring and let solution stand
30 s. Linearly increase applied voltage (positive voltage scan). Use
manufacturers instructions for rate of scan, e.g., 26 mV/s. Measure
wave height at half-wave potential (0.45 0.05 V against saturated
calomel electrode). Plot g Pb/mL standard solution against wave
height sensitivity factor (SF). Repeat for each standard solution and
reagent blanksolution. Prepare newcurve witheachbatchof samples.
E. Determination
Transfer to cell same volume test solution as used in standardization.
Bubble N
2
, add Hg drop, and apply voltage as in standardization. Mea-
sure wave height at appropriate potential and determine Pb concentra-
tion by comparing wave height of test solution with that of standard
curve or analyze standard solution immediately before or after sample
solution (preferable when instrument scale factor must be changed).
Prepare reagent blank solution as in 973.35D (see 9.2.14), last
paragraph, and analyze as above.
F. Calculations
Calculate g Pb/mL as follows:
C = C
( ) ( )
( ) ( )
WH SF WH SF
WH SF WH SF
B B
B B


where C and C =g Pb/mL test portion and standard, respectively;
SF, SF, SF
B
, and SF
B
= sensitivity factor settings of test portion,
standard, and reagent blank and [may be different for test (SF
B
) and
standard (SF
B
)] solutions, respectively; and WH, WH
B
, WH
B
, and
WH = wave heights.
ppm (g/g) Pb =
C 50
g sample

Reference: JAOAC 56, 1246(1973).


CAS-7439-92-1 (lead)
2000 AOAC INTERNATIONAL

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