7.2.28 H2O, mix thoroly, and filter thru dry filter.

AOAC Official Surplus Method 920.30 i Transfer 50 mL aliquot to 400 mL beaker; add 200
Sodium and Potassium Cyanides mL H2O, 5 mL NaOH soln (100 g/L2 H O), and 10
drops satd KI soln (or few crystals); and titr. to faint
Pesticide Formulataions opalescence with the AgNO3 soln. (In making this titrn,
it is advantageous to have beaker over black surface.)
Final Action From mL 0.1N AgNO3 used calc. % CN. Reaction is
Surplus 1965 represented by equation: 2NaCN + AgNO3 =
NaCN.AgCN + NaNO3 (1 mL 0.1N AgNO 3 = 0.005204
g CN).
4.088 - 4.089, 10th ed.
Reference: J. Assoc. Offic. Agr. Chemists 10,
4.088 Reagents 27(1927).
Silver nitrate soln.—0.1N. Stdze as in 941.18(B) (see
A.1.11). Chloride
Final Action
4.089 Determination
Method I
Break sample into small lumps in mortar (do not
4.090 Reagent
grind). Weigh quickly ca 5 g in weighing bottle and
Ammonium or potassium thiocyanate soln.—0.1N.
wash into 500 mL vol. flask contg ca 200 mL H2O. Add
little PbCO3 to ppt sulfides, if present, dil. to mark with Stdze by titrg against 0.1N Ag No3, 4.088.

4.091 Determination
Dil. 50 mL aliquot prepd soln, 4.089, in beaker with
equal vol. H2O, add 1–2 mL 40% Cl-free HCHO soln,
stir well, and let stand 15 min. Acidify with 5 mL
HNO3 (1 + 1), add measured vol. 0.1N AgNO3, 4.088,
enough to give excess, stir well, filter, wash, and titr.
excess of Ag in combined filtrate and washings with the
0.1N thiocyanate soln, using the ferric indicator,
929.04(A)(e). From mL 0.1N AgNO3 minus mL
thiocyanate soln used, calc. % Cl.

Method II
4.092
Dil. 50 mL aliquot prepd soln, 4.089, in distg flask to
100–150 mL with H2O, acidify with slight excess of
HOAc, and distill, passing vapors thru condenser,
delivery end of which dips into 25 mL 10% NaOH soln,
to absorb HCN. After distg all HCN (50 mL distillate),
wash liquid remaining in distg flask into beaker, add 5
mL HNO3 (1 + 1), and then measured vol. 0.1N
AgNO3, 4.088, enough to give excess. Stir well, filter,
wash, and titr. excess Ag in combined filtrate and
washings with thiocyanate soln, 4.090, using ferric
indicator, 929.04(A)(e). From mL 0.1N AgNO3 minus
mL 0.1N thiocyanate soln used, calc. % CI.

Reference: J. Assoc. Offic. Agr. Chemists 28.

© AOAC INTERNATIONAL

FIG. 4:4—Apparatus used in volatilization

method for determination of mercury