AOAC Official Method 977.

10
Moisture in Cacao Products
Karl Fischer Method
First Action 1977
Final Action 1979
(Applicable to milk chocolate and confectionary coatings.)
A. Apparatus and Reagents
(a) Karl Fischer titration assembly.—Manual or automatic, with
stirrer.
(b) Syringes.—1 mL with needle end cap (0–40 unit insulin type
is satisfactory) and 10 mL without needle (disposable plastic type is
satisfactory).
(c) Karl Fischer reagent.—Stabilized, with H2O equivalent of ca
5 mg H2O/mL reagent. Available commercially or prepare as
follows: Dissolve 133 g I2 in 425 mL dry pyridine in dry glassstoppered
bottle. Add 425 mL dry ethylene glycol monomethyl
ether. Cool to 4° in ice bath and bubble in 102–105 g SO2. Mix
well and let stand 12 h. Reagent is reasonably stable, but restandardize
for each series of determinations. Place 50 mL formamide,
practical grade, into 200 mL Berzelius beaker
containing magnetic stirrer. Place in titrimeter and titrate (Titrate
slowly near end point until 0.1 mL addition causes meter to
deflect to right of 0 and remain 60 s.) Quickly add accurately
weighed amount (0.250–0.350 g) disodium tartrate×2H2O. Titrate
immediately to same end point. Repeat determination and calculate
average.
mg H2O/mL reagent =
(mg Na2C4H4O6×2H2O ´ 0.1566)/mL reagent
(d) Karl Fischer solvent.—Mix equal volumes anhydrous methanol
and CHCl3.
B. Determination
Standardize reagent, (c), by accurately weighing ca 125 mg H2O
from 1 mL syringe (5 units) into 30–50 mL pretitrated solvent. (Keep
needle capped except while delivering H2O, to eliminate evaporation.)
Titrate with reagent, (c), until near end point; then add in 0.1
mL increments until end point remains 1 min (usually >50 mamp).
Calculate C = g H2O/mL reagent. Duplicates must agree within 0.1
mg H2O/mL reagent.
Melt sample in closed Whirl-Pak bag supported in 400 mL beaker
£2 h in oven at 40 ± 2°. Mix thoroughly by first gently squeezing
bag and then stirring ca 1 min with glass rod or spatula. Remove
portion with 10 mL syringe, weigh, add portion containing ca 100
mg H2O to 30–50 mL pretitrated reagent, and reweigh. Titrate as in
standardization.
% H2O = mL reagent ´ C ´ 100/g sample