9.2.17 - 972 - 23 PDF

9.2.
17
AOAC Official Method 972.23
Lead in Fish
Atomic Absorption Spectrophotometric Method
First Action 1972
Final Action 1976
A. Apparatus
(a) Atomic absorption spectrophotometer.See 973.35B(a)
(see 9.2.14); range 010 g/mL.
(b) Lead lamp.Hollow cathode Pb lamp.
(c) Crucible.Porcelain, ca 50 mL capacity and 5 cm deep; or
tall-form Vycor or quartz beaker, 100 mL.
B. Reagents
(a) Hydrochloric acid.1M. Dilute 82mLHCl to1Lwith H
2
O.
(b) Lead standard solutions.(1) Stock solution.1 mg
Pb/mL 1M HNO
3
. See 972.25C(d) (see 9.2.19). (2) Working solu-
tion.10g Pb/mL. Pipet 10 mLstock solution into 1 Lvolumetric
flask, add 82 mL HCl, and dilute to volume with H
2
O.
(c) Buffer solution.Disperse 163 g EDTA in 200 mL H
2
O in
2 L volumetric flask and add enough NH
4
OH to dissolve. Dilute
60 mL 70.5% HClO
4
by pouring carefully into ca 500 mL H
2
O and
cool. Dissolve 50 g La
2
O
3
in HClO
4
solution. Add 8 drops methyl or-
ange indicator to ammoniacal EDTA solution and add La
2
O
3
solu-
tion to EDTA solution while stirring vigorously. If necessary, add
NH
4
OH to maintain alkalinity of above solution to methyl orange.
Dilute to 2 L.
C. Reagent Blank
Before proceeding with analysis, test purity of reagents as fol-
lows: Evaporate 4 mL HNO
3
in crucible to dryness on hot plate or
steambath, dissolve residue in 1MHCl, and transfer to 25 mL volu-
metric flask. Heat residue again successively with two 5 mLportions
1M HCl and add to flask. Cool, dilute to volume with 1M HCl, and
mix. Proceed with determination. Total reagent blank should be 10 g
Pb (equivalent to 0.4 mg/kg in material) for determinations at levels
1 mg/kg. For determinations at <1 mg/kg, purify reagents as in
973.50B(see11.1.13) toattainblank<50%of limitinglevel of concern.
D. Preparation of Material
Weigh ca 25 g (to nearest 0.1 g) test portion into crucible, A(c),
and dry 2 h at 135150C. Transfer to cold, temperature-controlled
furnace and slowly raise temperature to 500C. Set control and
check for maintenance of 500C. (Temperature as lowas 550Cmay
cause loss of Pb.) Ash overnight (16 h). Remove test portion, let cool
to roomtemperature, cautiously add 2 mL HNO
3
, and swirl. Evapo-
rate carefully just to dryness on warmhot plate or steambath. Trans-
fer to cooled furnace, slowly raise temperature to 500C, and hold at
this temperature 1 h. Remove dish and cool. Repeat HNO
3
ashing, if
necessary, to obtain clean, practically C-free ash. Add 10 mL 1M
HCl and dissolve ash by heating cautiously on hot plate. Transfer to
25 mL volumetric flask. Heat ash residue again successively with
two 5 mL portions 1M HCl and add to flask. Cool, dilute to volume
with 1M HCl, and mix.
E. Preparation of Standard Curve
Transfer 0, 1, 3, 5, 15, 25, and 50 mL Pb working solution,
B(b)(2), to separate 50 mL volumetric flasks and dilute to volume
with 1M HCl (0, 0.2, 0.6, 1.0, 3.0, 5.0, and 10.0 g Pb/mL, respec-
tively). Set spectrophotometer to previously established optimum
conditions for maximumsignal at 283.3 nm. Use airC
2
H
2
flowrates
recommended by manufacturer for standard conditions for Pb. For
digital concentration readout, calibrate in concentration mode with
solutions containing 0.2 and 10.0 g Pb/mL. Record concentration
directly after calibration of instrument. For strip chart readout, set
amplification to give 1% absorption reading for 0.2g/ mL work-
ing solution and prepare standard curve of A against g Pb/mL.
F. Determination
Use aliquot of test solution, D, and proceed as in (a) or (b). Treat
reagent blank, C, as test portion and subtract reading fromA of sam-
ples.
(a) Clear solutions.Determine A of test and standard solutions
as in E, using following sequence 3 times: Read standard solution
first, then test solution, alternating until all test and standard solu-
tions have been read. When many test solutions are to be analyzed,
standard solutions may be read after series of 3 test solutions instead
of after each.
ppm (g/g) Pb =
g Pb / mL test solution 25
g test portion
(b) Cloudy solutions.Proceed as in (a), but add 1 mLbuffer solu-

tion, B(c), to aliquots of test and standard solutions before reading.
If additional dilutions are necessary or if buffer is added:
ppm (g/g) Pb = g Pb/mL test solution
(mL diluted test solution/mL original aliquot)
(25/g test portion)
References: JAOAC 55, 727, 733(1972); 56, 406(1973).
CAS-7439-92-1 (lead)
2000 AOAC INTERNATIONAL

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(b) Cloudy solutions.Proceed as in (a), but add 1 mLbuffer solu-

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