7.1.
10 cess, and boil to expel excess NH3, as shown by color change in liq-
AOAC Official Method 922.05
Copper in Pesticide Formulations
First Action 1922
Final Action
(Applicable to such preparations as Bordeaux–lead arsenate, Bor-
deaux–zinc arsenite, Bordeaux–Paris green, and Bordeaux–calcium
arsenate.)
A. Electrolytic Method
Evaporate filtrate and washings from PbSO4 precipitation, 922.04
(see 7.1.09), to fuming; add few mL fuming HNO3 to destroy or-
ganic matter, and continue evaporation to ca 3 mL. Take up with ca
150 mL H2O, add 5 mL HNO3, and filter if necessary. Wash into
250 mL beaker, adjust volume to 200 mL, and electrolyze, using ro-
tating anode and weighed gauze cathode with current of 2–3 amp.
After all Cu has apparently deposited (ca 30 min), add 15–20 mL
H2O to electrolyte and continue electrolysis few min. If no further
deposition occurs on newly exposed surface of electrode, wash with
H2O without breaking current either by siphoning or quickly replac-
ing beaker with electrolyte successively with 2 beakers of H2O. In-
terrupt current, rinse cathode with alcohol, dry few moments in
oven, and weigh. Calculate percent Cu in test portion.
B. Volumetric Thiosulfate Method
Proceed as in A to point at which filtrate and washings from
PbSO4 precipitation are treated with fuming HNO3 and evaporated
to volume of ca 3 mL. Take up in ca 50 mL H2O, add NH4OH in ex-
uid and partial precipitation. Add 3–4 mL CH3COOH (4 + 1), boil
1–2 min, cool, add 10 mL 30% KI solution (w/v), and titrate with
standard Na2S2O3 solution until brown color becomes faint. Add
starch indicator, 922.03A(f) (see 7.1.05), and continue titration cau-
tiously until blue color due to free I2 entirely disappears. From mL
standard Na2S2O3 solution used, calculate percent Cu in test portion.
Thiosulfate standard solution.—Prepare solution containing 39 g
Na2S2O3⋅5H2O/L. Accurately weigh 0.2–0.4 g pure electrolytic Cu
and transfer to 250 mL Erlenmeyer roughly marked at 20 mL inter-
vals. Dissolve Cu in 5 mL HNO3 (1 + 1), dilute to 20 or 30 mL, boil to
expel red fumes, add slight excess saturated Br2–H2O, and boil until
Br2 is completely removed. Cool, and add 10 mL NaCH3COO solu-
tion (574 g trihydrate/L). Prepare 42 g/100 mL KI solution made
very slightly alkaline to avoid formation and oxidation of HI. Add
10 mL of the KI solution and titrate with Na2S2O3 solution to light
yellow. Add enough starch indicator, 922.03A(f) (see 7.1.05), to
produce marked blue. As end point nears, add 2 g KSCN and stir un-
til completely dissolved. Continue titration until precipitate is per-
fectly white. 1 mL Na2S2O3 solution = ca 10 mg Cu.
It is essential for Na2S2O3 titration that concentration of KI in so-
lution be carefully regulated. If solution contains <320 mg Cu, at
completion of titration 4.2–5 g KI should have been added for each
100 mL total solution. If greater amounts of Cu are present, add KI
solution slowly from buret with constant agitation in amounts pro-
portionately greater.
Reference: JAOAC 5, 398(1922).
CAS-7440-50-8 (copper)
© 2000 AOAC INTERNATIONAL