COCO CORPORATION TOTAL DIETARY FIBER

DEPARTMENT DOC NO.: VERSION NO.

ANALYTICAL LAB CC-TM-41 DRAFT
DATE: PAGE:
MAY 2020 Page 1 of 2

1 SCOPE

2 DEFINITIONS

3 PRINCIPLE

4 REAGENTS /APPARATUS /EQUIPMENTS

 Digestion flask
 Kjeldahl set-up
 Graduated cylinder (25mL, 250mL)
 HgO or metallic Hg
 K2SO4 or anhydrous Na2SO4
 H2SO4
 Thiosulfate solution
 Zinc granules
 NaOH

5 REFERENCE DOCUMENTS
AOAC Official Test Method 920.87 Protein (Total) in Flour

6 HAZARDS /SAFETY /PPE

 Gloves

7 PROCEDURE
7.1 Place weighed test portion (0.7–2.2 g) in digestion flask.
7.2 Add 0.7 g HgO or 0.65 g metallic Hg, 15 g powdered K 2SO4 or anhydrous Na2SO4,
and 25 mL H2SO4. If test portion >2.2 g is used, increase H2SO4 by 10mL for each g
test portion.
7.3 Place flask in inclined position and heat gently until frothing ceases (if necessary, add
small amount of paraffin to reduce frothing)
7.4 Boil briskly until solution clears and then ≥30 min longer (2h for test portions
containing organic material).
7.5 Cool, add around 200 mL H2O
7.6 Cool to <25°C, add 25 mL of the sulfide or thiosulfate solution, and mix to precipitate
Hg.
7.7 Add few Zn granules to prevent bumping, tilt flask, and add layer of NaOH without
agitation. (For each 10 mL H 2SO4 used, or its equivalent in diluted H 2SO4, add 15 g
solid NaOH or enough solution to make contents strongly alkaline.) (Thiosulfate or
sulfide solution may be mixed with the NaOH solution before addition to flask.)
PREPARED BY : APPROVED BY :

ANALYTICAL LAB (insert name here)

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COCO CORPORATION TOTAL DIETARY FIBER
DEPARTMENT DOC NO.: VERSION NO.
ANALYTICAL LAB CC-TM-41 DRAFT
DATE: PAGE:
MAY 2020 Page 2 of 2

7.8 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).
7.9 Remove receiver, wash tip of condenser, and titrate excess standard acid in distillate
with standard NaOH solution.
7.10 Correct for blank determination on reagents.

8 CALCULATION

N, % = [(mL standard acid * molarity acid) – (mL standard NaOH * molarity NaOH)] x 1.4007
g test portion

Multiply percent N by 5.7 to obtain percent protein.

9 TEST REPORT
Proceed with Test Report Form.

10 DISPOSAL OF MATERIALS

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ANALYTICAL LAB (insert name here)

MANAGER