9.2.

16
AOAC Official Method 979.17
Lead in Evaporated Milk and Fruit Juice
Anodic Stripping Voltammetric Method
First Action 1979
Final Action 1984
A. Apparatus
(a) Voltammetric analyzer.With staircase anodic stripping
ramp and graphite electrode coated with thin film of Hg. Capable of
measuring 5 ng Pb in presence of dissolved O
2
. (Solutions cannot be
deaerated). Peak area integration desirable. (ESAModel 3010A[re-
placed by Model 3010B] lead analyzer [ESA, Inc., 45 Wiggins Ave,
Bedford MA 01730], or equivalent.)
(b) Micropipets.50, 100, 200, and 300 L, positive displace-
ment type. (SMI or Drummond, or equivalent).
B. Reagents
(Use deionized H
2
O to prepare standard solutions. Prepare and
store solutions in same Pyrex volumetric flasks. Do not wash flasks
with strong acids between use; just rinse 3 times with deionized H
2
O.
Always prepare same solution in same flask.)
(a) Lead releasing reagent.Containing <1 ppb (ng/g) Pb. Acid
solution of cation able to displace Pb from sample. Metexchange

Reagent (ESA, Inc.), or equivalent.

(b) Lead standard solutions.(1) Stock solution.1 mg/mL.
Prepare as in 972.25D(d)(1) (see 9.2.19). (2) Intermediate solu-
tion.10g/mL. Pipet 1 mLstock solution into 100 mLvolumetric
flask containing 1.0 mLHNO
3
and ca 50 mLH
2
O. Mix, and dilute to
volume. Prepare each week. After solution is prepared 6 times in
same flask, it is stable 1 month. (3) Working solution for fruit juice
determination.3 g/mL. Pipet 30 mL solution (2) into 100 mL
volumetric flask containing 0.7 mL HNO
3
and ca 50 mL H
2
O. Mix,
and dilute to volume. (4) Working solution for evaporated milk de-
termination.1g/mL. Prepare as in (3), using 10 mL solution (2)
and 1.0 mL HNO
3
. Working solutions are stable 3 days. After being
prepared 5 times in same flask, they are stable 2 weeks. (5) Calibra-
tion solutions.Evaporated milk or fruit juice of type being deter-
mined, and containing 0.5 ppm (g/g) added Pb.
C. Determination
Calibrate instrument according to manufacturers directions. Mix
aliquot of test solution with releasing reagent, B(a), and performde-
termination according to manufacturers instructions. Data for ESA
analyzer are as shown in Table 979.17.
Run control or spiked test portion with each 1520 analyses in a
series.
Reference: JAOAC 66, 1409, 1414(1983).
CAS-7439-92-1 (lead)
2000 AOAC INTERNATIONAL
Table 979.17 Data for ESA analyzer
Calibration Juice Milk
Initial potential, V 1.025 0.005 1.090 0.005
Final potential, V 0.100 0.005 0.100 0.005
Sweep rate, mV/step 14.0 0.05 10.50 0.05
Integration set points, V 0.490 0.005 0.490 0.005
Sample size, L 300 200