9.2.

19
AOAC Official Method 972.25
Lead in Food
Atomic Absorption Spectrophotometric Method
First Action 1972
Final Action 1976
A. Principle
Organic matter is digested and Pb released coprecipitates with
SrSO
4
. Soluble sulfate salts are decanted, and precipitate is con-
verted to carbonate salt, dissolved in acid, and determined by AA at
217.0 or 283.3 nm.
B. Apparatus
(a) Atomic absorption spectrophotometer.Operated at 217 or
283.3 nm.
(b) Stirring motor.With eccentric coupling for stirring centri-
fuge tubes.
C. Reagents
(Age all new glassware and all glassware which has contained
high Pb concentration in boiling HNO
3
before washing. Never let
used glassware dry before washing, and always include final HNO
3
rinse followed by deionized H
2
O rinse.)
(a) Strontium solution.2%. Dissolve 6 g SrCl
2
6H
2
O in
100 mL H
2
O.
(b) Ternary acid mixture.Add 20 mL H
2
SO
4
to 100 mL H
2
O,
mix, add 100 mL HNO
3
and 40 mL 70% HClO
4
, and mix.
(c) Nitric acid 1M.Add 128 mL redistilled HNO
3
to
500800 mL distilled or deionized H
2
O and dilute to 2 L. Redistilled
HNO
3
(GFS Chemical, Inc., No. 63) may be diluted and used without
redistillation.
(d) Lead standard solutions.(1) Stock solution.1000g/mL.
Dissolve 1.5985 g Pb(NO
3
)
2
, recrystallized as in 935.50B (see
9.2.12), in ca 500 mL1MHNO
3
in 1 Lvolumetric flask and dilute to
volume with 1M HNO
3
. (2) Working solutions.Prepare 100 g
Pb/mL by diluting 10 mL stock solution to 100 mL with 1M HNO
3
.
Dilute 1, 3, 5, 10, 15, and 25 mL aliquots of this solution to 100 mL
with 1M HNO
3
(1, 3, 5, 10, 15, and 25 g Pb/mL, respectively).
D. Separation of Lead
Accurately weigh test portion containing 10 g dry matter and 3
g Pb. Place in 500 mLboiling or Kjeldahl flask and add 1 mL2%Sr
solution, C(a), and several glass beads. Prepare reagent blank and
carry through same operations as sample. Add 15 mL ternary acid
mixture, C(b), for each g dry matter and let stand 2 h. Heat under
hood or H
2
O vacuum manifold system until flask contains only
H
2
SO
4
and inorganic salts. (Note: Take care to avoid material loss
from foaming when heat is first applied, and when foaming occurs
soon after material chars. Remove heat and swirl flask before contin-
uing digestion. Add HNO
3
, if necessary.)
Cool digest few min. (Digest should be cool enough to add ca
15 mL H
2
Osafely, but hot enough to boil when H
2
Ois added.) Wash
while still hot into 4050 mL tapered-bottom centrifuge tube and
swirl. Let cool, centrifuge 10 min at 350 g, and decant liquid into
waste beaker. (Film-like precipitate on surface may be discarded.)
Dislodge precipitate by vigorously stirring with eccentric-coupled
stirring motor. To complete transfer, add 20 mL H
2
O and 1 mL
0.5M H
2
SO
4
to original flask and heat. Do not omit this step even
though it appears transfer was complete in first wash. Wash hot con-
tents of original digestion flask into centrifuge tube containing precip-
itate. Swirl to mix, cool, centrifuge, and decant liquid into waste
beaker.
Dislodge precipitate by stirring vigorously, add 25 mL saturated
(NH
4
)
2
CO
3
solution (ca 20%), and stir until all precipitate is dis-
persed. Let stand 1 h, centrifuge, and decant liquid into waste beaker.
Repeat (NH
4
)
2
CO
3
treatment.
After decanting, invert centrifuge tube on paper towel and drain
all liquid. Add 5 mL1MHNO
3
(use larger volume 1MHNO
3
in both
sample and blank if >25 g Pb is expected), stir vigorously to expel
CO
2
or use ultrasonic bath 23 min, let stand 30 min, and centrifuge
if precipitate remains. (Use same technique for all test portions.)
E. Determination
Set instrument to previously established optimum conditions, us-
ing airC
2
H
2
oxidizing flame and 217 or 283.3 nm resonant wave-
length. Determine A of test and blank solutions and 5 standards
within optimumworking range (1080%T) before and after sample
readings. Flush burner with 1M HNO
3
and check 0 point between
readings. Determine Pb fromstandard curve of Aagainst g Pb/mL:
Concentration Pb (mg / kg)
( g Pb / mL) (mL 1M HNO
=

3
)
g test portion
Reference: JAOAC 55, 737(1972).
CAS-7439-92-1 (lead)
2000 AOAC INTERNATIONAL