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9.1.

07
AOAC Official Method 971.20
Copper and Nickel in Tea
Atomic Absorption Spectrophotometric Method
First Action 1971
Final Action 1976
Caution: See Appendix B, safety notes on AAS, wet oxidation,
nitric acid, and perchloric acid.
A. Principle
Materials are wet ashed and after dilution Cu and Ni are deter-
mined by AA at 232.0 nm (Ni) and 324.7 nm (Cu). Matrix of stan-
dard solutions is matched to that of test solution to avoid interference
from Na and K.
B. Apparatus
Atomic absorption spectrophotometer.Capable of measuring con-
tent or changeof content of 0.05gNi or Cu/mLinaqueous solution.
C. Preparation of Standard Solutions
(a) Copper standard solution.1000 g/mL. Dissolve 1.000 g
99.99% Cu in 20 mL HNO
3
, cool, and dilute to 1 L with H
2
O.
(b) Nickel standard solution.1000 g/mL. Dissolve 1.000 g
99.99% Ni in 20 mL HNO
3
, cool, and dilute to 1 L with H
2
O.
(c) Matrix standard solutions.Prepare solutions containing 0,
0.2, 0.4, 0.8, 1.6, 2.0, 4.0, 8.0, and 10 g Ni and Cu/mL and major
metal matrix components: (1) For 3 g sample tea.To contain
180 g Ca, 100g Mg, and 40g Al/mLwith final concentration of
8% (v/v) HClO
4
. (2) For 6 g sample instant tea.To contain
7000 g K, 70 g Na, 700 g Mg, and 130 g Ca/mL with final
HNO
3
concentration of (1 + 9).
D. Preparation of Calibration Curve
Let instrument stabilize. Optimize conditions for Cu or Ni accord-
ing to manufacturers instructions.
Aspirate 10g/mL standard enough times to establish that A read-
ing is not drifting. Record 6 readings and calculate standard deviation
() = (x - y) 0.40, where x and y are maximum and minimum read-
ings, respectively, and0.40is factor toconvert range of 6values to.
Beginning with solution containing 0 Cu, aspirate each matrix
standard solution and record A. If value for 10 g/mL solution dif-
fers from average of the 6 values used to calculate by >0.01 (av-
erage of the 6 values), repeat measurements. If these determinations
indicate drift, determine cause (e.g., deposits in burner or clogged
capillary), correct it, and repeat calibration. Repeat for Ni solutions.
Plot A against g metal/mL.
E. Determination
Select test portion weight to give solution containing 0.05 but
10 g Ni/mL, usually 3 g for teas and 6 g for instant teas.
(a) Wet ashing.Accurately weigh test portion into 400 mL
beaker, add 100 mL HNO
3
, and swirl. Cover, and let react 10 min;
then place on hot plate. Evaporate to near dryness and cool. Add
50 mL HNO
3
, and for tea, add 10 mL HClO
4
. Continue evaporation
to obtain clear solution.
Transfer to 50 mL volumetric flask and dilute to volume with
H
2
O. (Insoluble KClO
4
which settles to bottom of flask does not in-
terfere.)
Prepare reagent blank containing same amounts of acids taken
from same lots, evaporated as above.
(b) Photometry.Aspirate test and blank solutions, and record
A. Measure A of matrix standard solution containing 10 g/mL. If
this value differs fromvalue of average of the 6 values used to calcu-
late by >2, repeat measurement. If these values indicate drift, de-
termine cause, correct it, and repeat calibration and test and blank
readings.
(c) Calculations.Correct readings of test solution for blank.
Convert corrected A to g/mL from calibration curve.
Concentration (mg/kg) Ni (or Cu) =
C V
W

where C =g metal/mL from curve, V = final volume test solution


(50), and W = g test portion.
References: JAOAC 53, 531(1970); 54, 658(1971).
CAS-7440-50-8 (copper)
CAS-7440-02-0 (nickel)
2000 AOAC INTERNATIONAL