9.2.

35
AOAC Official Method 985.16
Tin in Canned Foods
Atomic Absorption Spectrophotometric Method
First Action 1985
Final Action 1988
Codex-AdoptedAOAC Method*
A. Principle
Materials are digested with HNO
3
and then HCl and are diluted.
Aqueous KCl is added to samples and standards to reduce positive
instrument interference. Sn is determined by AAS at 235.5 nm with
oxidizing N
2
OC
2
H
2
flame.
B. Reagents and Apparatus
(a) Atomic absorption spectrophotometer.With simultaneous
background correction and N
2
OC
2
H
2
burner.
(b) Tin standard solutions.(1) Stock solution.1 mg Sn/mL.
Dissolve 1.000 g Sn (reagent grade) in ca 200 mLconcentrated HCl,
add ca 200 mL H
2
O, cool to ambient temperature, and dilute to 1 L
with H
2
O. (2) Working solutions.0, 50, 100, 150, and 200 g
Sn/mL. Into each of five 100 mLvolumetric flasks, pipet 10 mLcon-
centrated HCl, 1.0 mL KCl solution, (c), and 0, 5, 10, 15, or 20 mL
Sn stock solution. Dilute to volume with H
2
O.
(c) Potassium chloride solution.10 mg K/mL. Dissolve 1.91 g
KCl and dilute to 100 mL with H
2
O.
(d) Nitric acid.Concentrated. Test purity of lot by diluting por-
tion 1:4 (v/v) with H
2
O and aspirating into AA spectrophotometer.
Absence of Sn signal indicates suitability for analysis.
C. Preparation of Materials
Accurately (0.01 g) weigh test portion into 250 mL Erlenmeyer:
3040 g juices or drinks, 20 g foods containing 5075% H
2
O, and
510 g solids or semisolids. Limit fat or oil content to 24 g and total
organics to ca 5 g. Dry in oven at 120C.
Do not add HNO
3
to test portions unless there is time to complete
this stage of digestion in the same day. Add 30 mL concentrated
HNO
3
to flask and, within 15 min, heat gently in hood to initiate di-
gestion, avoiding excessive frothing. Gently boil until 36 mL di-
gest remains or until sample just begins to dry on bottom. Do not let
material char. Remove flask from heat. Without delay, continue as
follows, including 2 empty flasks for reagent blanks: Add 25 mL
concentrated HCl, and heat gently ca 15 min until bumping from
evolution of Cl
2
stops. Increase heat, and boil until 1015 mL vol-
ume remains, using similar flask with 15 mL H
2
O to estimate vol-
ume. Add ca 40 mL H
2
O, swirl, and pour into 100 mL volumetric
flask, rinsing once with ca 10 mL H
2
O. When HCl is present in di-
gest, test portions may stand overnight or longer.
Pipet 1.0mLKCl solutionintoeachvolumetric flask. Cool toambi-
ent temperature and dilute to volume with H
2
O, adding additional
H
2
Otoapproximatelycompensate for volume of fat inflask. Mixwell
and filter ca 3050 mL through dry, medium porosity paper into dry,
polypropylene or polyethylene screw-cap bottle. Do not filter blanks.
Cap bottles until analysis. Solutions are stable several months.
D. Determination
(Caution: Due to explosive nature of gases, take care when ignit-
ing and using flame. Heating tape on N
2
O regulator may be needed
to maintain steady gas flow.)
Using 200 g/mL standard and 235.5 nm Sn line, optimize
spectrophotometer, burner, and flame according to manufacturers
instructions. Then increase N
2
O flow or decrease C
2
H
2
flow to give
oxidizing flame; red part should be ca 4 mm above burner slot. This
reduces sensitivity but improves precision to 0 0.0004 A for blank
and gives 0.201 0.001 A for 100 g/mL standard. Periodically
monitor sensitivity of a standard; if sensitivity decreases >20%, turn
off flame and carefully clean burner slot.
Zero spectrophotometer while aspirating H
2
O but do not adjust
zero until after determinations; autozero reduces precision. Aspirate
H
2
O before and after each sample, standard, and blank solution.
Take three 5 s readings for each solution, average, and reference all
A measurements to A of H
2
O.
Record A for standards, draw calibration curve, and visually check
for inaccurate standards. Two times blank-corrected A for 50g/mL
standard should not differ by more than 3% from blank-corrected A
for 100 g/mL standard.
Block standard blank solution with 50g/mL standard, and using
ratio of A, calculate concentration of standard blank:
Standard blank (g/mL) = [A
o
/(A A
o
)] 50
where A
o
and A refer to blank and mean of readings for 50 g/mL
blocking standard, respectively.
Add standard blank concentration to nominal standard concentra-
tions to obtain true standard concentrations.
Measure Aof material blanks as for standard blank and calculate:
Material blank (g/mL) =
(A
o
/A) true concentration of 50 g/mL standard
where A
o
and A refer to blank and 50g/mL standard, respectively.
Calculate mean concentration of material blanks, B.
Determine test solution concentrations by one of 2 ways: (1) Mea-
sure A of test solutions (maximum 3 solutions) and 50g/mL stan-
dard (or 100 g/mL standard, depending on test solution
concentration level), blocking test solutions with standards. Calcu-
late blank-corrected test solution concentrations:
Test solution concentration (g/mL) =
(A/A true standard concentration) B
where A and A refer to test and standard solution, respectively.
When high accuracy is not required or when calibration curvature
is extensive, use procedure (2) after confirmation that sensitivity
changes and baseline drift are absent during analytical run. (2) Cali-
brate using blank and 50, 100, and 150g/mL standards. Run mate-
rial blanks and test solutions, and calculate solution concentrations
using either instrument microprocessor or calibration curve. Calcu-
late mean of sample blank concentrations, B. Calculate
blank-corrected solution concentrations (g/mL) by subtracting B
from solution concentrations.
For both (1) and (2), calculate concentrations in test portions:
2000 AOAC INTERNATIONAL
Concentration Sn (mg / kg)
blank corrected
=
solution cocentration
test portion weight (g)
100
Reference: JAOAC 68, 209(1985).
CAS-7440-31-5 (tin)
Revised: March 1997
* Adopted as a Codex Reference Method (Type II) for atomic absorption
spectrophotometry of tin in processed meat and poutry products and
soups and broths.
Adopted as a Codex Reference Method (Type III) for atomic absorption
spectrophotometry of tin (products in other containers) in canned
corned beef.
2000 AOAC INTERNATIONAL