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Aoac971 20

The document describes a method for determining copper and nickel content in tea through atomic absorption spectrophotometry. Tea samples are wet ashed to dissolve the metals and diluted. Standard solutions are prepared and a calibration curve is plotted. Test solutions and blanks are analyzed to determine copper and nickel concentrations in mg/kg.

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Jhon Alexander Rincon Reina
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64 views1 page

Aoac971 20

The document describes a method for determining copper and nickel content in tea through atomic absorption spectrophotometry. Tea samples are wet ashed to dissolve the metals and diluted. Standard solutions are prepared and a calibration curve is plotted. Test solutions and blanks are analyzed to determine copper and nickel concentrations in mg/kg.

Uploaded by

Jhon Alexander Rincon Reina
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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9.1.

07 Beginning with solution containing 0 Cu, aspirate each matrix


AOAC Official Method 971.20 standard solution and record A. If value for 10 µg/mL solution dif-
Copper and Nickel in Tea fers from average of the 6 values used to calculate σby >0.01 × (av-
Atomic Absorption Spectrophotometric Method erage of the 6 values), repeat measurements. If these determinations
First Action 1971 indicate drift, determine cause (e.g., deposits in burner or clogged
Final Action 1976 capillary), correct it, and repeat calibration. Repeat for Ni solutions.
Plot A against µg metal/mL.
Caution: See Appendix B, safety notes on AAS, wet oxidation,
nitric acid, and perchloric acid. E. Determination
Select test portion weight to give solution containing ≥0.05 but
A. Principle
≤10 µg Ni/mL, usually 3 g for teas and 6 g for instant teas.
Materials are wet ashed and after dilution Cu and Ni are deter-
(a) Wet ashing.—Accurately weigh test portion into 400 mL
mined by AA at 232.0 nm (Ni) and 324.7 nm (Cu). Matrix of stan-
beaker, add 100 mL HNO3, and swirl. Cover, and let react 10 min;
dard solutions is matched to that of test solution to avoid interference
then place on hot plate. Evaporate to near dryness and cool. Add
from Na and K.
50 mL HNO3, and for tea, add 10 mL HClO4. Continue evaporation
B. Apparatus to obtain clear solution.
Atomic absorption spectrophotometer.—Capable of measuring con- Transfer to 50 mL volumetric flask and dilute to volume with
tent or change of content of 0.05µg Ni or Cu/mL in aqueous solution. H2O. (Insoluble KClO4 which settles to bottom of flask does not in-
terfere.)
C. Preparation of Standard Solutions
Prepare reagent blank containing same amounts of acids taken
(a) Copper standard solution.—1000 µg/mL. Dissolve 1.000 g from same lots, evaporated as above.
99.99% Cu in 20 mL HNO3, cool, and dilute to 1 L with H2O. (b) Photometry.—Aspirate test and blank solutions, and record
(b) Nickel standard solution.—1000 µg/mL. Dissolve 1.000 g A. Measure A of matrix standard solution containing 10 µg/mL. If
99.99% Ni in 20 mL HNO3, cool, and dilute to 1 L with H2O. this value differs from value of average of the 6 values used to calcu-
(c) Matrix standard solutions.—Prepare solutions containing 0, late σby >2σ, repeat measurement. If these values indicate drift, de-
0.2, 0.4, 0.8, 1.6, 2.0, 4.0, 8.0, and 10 µg Ni and Cu/mL and major termine cause, correct it, and repeat calibration and test and blank
metal matrix components: (1) For 3 g sample tea.—To contain readings.
180 µg Ca, 100µg Mg, and 40µg Al/mL with final concentration of (c) Calculations.—Correct readings of test solution for blank.
8% (v/v) HClO4. (2) For 6 g sample instant tea.—To contain Convert corrected A to µg/mL from calibration curve.
7000 µg K, 70 µg Na, 700 µg Mg, and 130 µg Ca/mL with final
HNO3 concentration of (1 + 9). C×V
Concentration (mg/kg) Ni (or Cu) =
D. Preparation of Calibration Curve W
Let instrument stabilize. Optimize conditions for Cu or Ni accord-
where C = µg metal/mL from curve, V = final volume test solution
ing to manufacturer’s instructions.
(50), and W = g test portion.
Aspirate 10 µg/mL standard enough times to establish that A read-
ing is not drifting. Record 6 readings and calculate standard deviation References: JAOAC 53, 531(1970); 54, 658(1971).
(σ) = (x - y) ×0.40, where x and y are maximum and minimum read- CAS-7440-50-8 (copper)
ings, respectively, and 0.40 is factor to convert range of 6 values to σ. CAS-7440-02-0 (nickel)

© 2000 AOAC INTERNATIONAL

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