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AOAC 920 - 87 - Kjeldahl Harinas

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32.1.

22
AOAC Official Method 920.87
Protein (Total) in Flour
First Action 1920
Final Action
Place weighed test portion (0.7–2.2 g) in digestion flask. Add 0.7 g
HgO or 0.65 g metallic Hg, 15 g powdered K2SO4 or anhydrous
Na2SO4, and 25 mL H2SO4. If test portion >2.2 g is used, increase
H2SO4 by 10 mL for each g test portion. Place flask in inclined position
and heat gently until frothing ceases (if necessary, add small amount of
paraffin to reduce frothing); boil briskly until solution clears and
then ≥30 min longer (2 h for test portions containing organic mate-
rial).
Cool, add ca 200 mL H2O, cool <25°C, add 25 mL of the sulfide or
thiosulfate solution, and mix to precipitate Hg. Add few Zn granules to
prevent bumping, tilt flask, and add layer of NaOH without agitation.
(For each 10 mL H2SO4 used, or its equivalent in diluted H2SO4, add
15 g solid NaOH or enough solution to make contents strongly alka-
line.) (Thiosulfate or sulfide solution may be mixed with the NaOH so-
lution before addition to flask.) Immediately connect flask to distilling
bulb on condenser, and, with tip of condenser immersed in standard
acid and 5–7 drops indicator in receiver, rotate flask to mix contents
thoroughly; then heat until all NH3 had distilled (≥150 mL distillate).
Remove receiver, wash tip of condenser, and titrate excess standard
acid in distillate with standard NaOH solution. Correct for blank deter-
mination on reagents.

N, % = [(mL standard acid molarity acid)


– (mL standard NaOH molarity NaOH)] × 1.4007/g test portion

Multiply percent N by 5.7 to obtain percent protein.

© 2000 AOAC INTERNATIONAL

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