Determination of Crude Fiber

Method No. FSSAI 03.018:2023 Revision No. & Date 0.0

Scope This method is for determination of crude fiber in in all food grain cereal
and cereal products and is applicable to materials from which the fat can
be and is extracted to obtain workable residue, including grains, meals,
flours, feeds, and fibrous materials.
Caution 1. It is recommended to use fume-hoods.
2. Ethyl alcohol is flammable, handle with care.
3. Ensure neutralization of the acid/base used prior to disposal.
4. During digestion, heating shall be performed with care in order to
avoid over-heating and too rapid boiling.
5. The foam formed in the vessel should never be allowed to exceed a
height of 10 mm.
6. Sulfuric acid (H2S04) is a corrosive substance, destructive to the skin,
eyes. Handle with care
7. Sodium hydroxide can cause severe skin burns and severe eye
damage. Wear gloves and eye protection.
Principle Crude fiber is loss on ignition of dried residue remaining after di-gestion
of sample with 1.25% (w/v) H2SO4 and 1.25% (w/v) NaOH solutions
under specific conditions. Separation of the residue by filtration
followed by drying and ashing of the residue. The loss in weight
resulting from ashing corresponds to the crude fiber content of the
sample.
Apparatus/Instrument a. Soxhlet apparatus (optional)
b. Digestion apparatus: With condenser to fit one-litre, digestion
flask and hot plate adjustable to temperature that will bring 200
mL H2O at 25 °C to rolling boil in 15 ± 2 min
c. Digestion flask of such a size and shape that the solution will not
be less than 1 inch (25 mm), nor more than 1.5 inch (38 mm) in
depth. A one-litre Erlenmeyer flask with 45/50 ground joint is
recommended.
a. Ashing dishes: Silica, Vitreosil 70 x 16 mm; or porcelain, or
equivalent
b. Filtering device: Buchner Funnel. Alternatively, a filter cloth, of
such character that no appreciable solid matter can pass through
it during rapid filtration, may be used. Retention may be tested
by running filtrate through a Gooch crucible. Butcher's linen,
dress linen with ca. 45 threads to an inch, or No. 40 filter cloth
made by the National Filter Media Corporation, Hamden,
connection 06514, or equivalent may be used.
c. Desiccator with fresh and efficient desiccant (preferably, orange
silica gel beads with moisture indicator).
Note: Do not use silica with blue cobalt indicator, as it is not suitable
for food applications.
d. Analytical balance, accurate up to 0.0001 g

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 e. Drying oven, capable of being controlled at 105± 1 °C
f. Muffle furnace, capable of being regulated at 500 ± 25 °C
Materials/Reagents
a. Sulfuric acid, specific gravity 1.84 at 60 °F
b. Sodium hydroxide pellets
c. Ethyl alcohol, 95%, ACS grade
d. Methylene chloride, anhydrous (dichloromethane), ACS grade
e. Demineralized water
f. Petroleum ether, initial boiling temperature, 35 °–38 °C; dry-flask
end point, 52 °–60 °C; 95% distilling <54 °C, specific gravity at 60
°F, 0.630–0.660
g. Antifoam: Antifoam A compound diluted 1 + 4 with mineral spirits
or petroleum ether, or H2O-diluted antifoam B emulsion (1 + 4). Do
not use antifoam spray.
h. Blue litmus paper
i. Bumping chips or granules: Broken Alundum crucibles or
equivalent granules are satisfactory

Preparation of a. Sulphuric acid (H2SO4) solution, 0.255 N: Into a 1000 mL

reagents volumetric flask add about 200 mL of demineralized water then
slowly introduce 12.5 g of conc. sulphuric acid and make up to the
mark with demineralized water. Concentration must be checked by
titration. If the concentration differs by more than ± 0.01 N from the
nominal values adjust it within the range
b. Sodium hydroxide (NaOH) solution, 0.312 N: Into a 1000 mL
volumetric flask introduce 12.5 g of carbonate free sodium
hydroxide pellets and make up to the mark with demineralized
water. Concentration must be checked by titration
c. Prepared ceramic fiber: Place 60 g ceramic fiber in blender, add 800
mL H2O, and blend 1 min at low speed. Determine blank by treating
2 g (dry weight) of prepared ceramic fiber with acid and alkali as in
determination. Correct crude fiber results for any blank, which
should be negligible (2 mg).
Method of analysis
1. Weigh accurately about 2.5-3 g sample and transfer to an extraction
apparatus (Soxhlet extractor) and extract with petroleum ether. Air
dry the extracted sample and transfer to a dry 1 L conical flask. If
percentage of fat in the product is high (>10%), then treat it with a
mixture of acetone and petroleum benzene. Excess of fat, if not
removed on initial defatting may affect the end result.
2. Add 200 mL of the H2SO4 solution connect the digestion flask to the
condenser and place on a preheated hot plate or digestion rack
adjusted so that the acid will boil in ca. 5 min. Continue boiling
briskly for 30±1 min with frequent rotation of the flask to ensure
thorough wetting and mixing of the sample. Material should not be
allowed to remain on the sides of the flask out of contact with the
solution. Add one drop diluted antifoam (Excess antifoam may give
high results; use only if necessary, to control foaming.). Bumping

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 chips or granules may also be added. Successive sample digestions
should be started at ca. 3 min intervals to facilitate accurate timing.
3. After boiling 30 min, remove the flask and filter immediately
through the Buchner funnel or through a filter cloth in a fluted funnel
using a suction flask to speed filtration. Wash with boiling water
until washings are no longer acid. Check alkalinity with litmus
paper.
4. Transfer the sample and ceramic fiber quantitatively in digestion
flask, washing the filter cloth or Buchner filter with 200 mL of
NaOH solution. A wash bottle to deliver 200 mL is convenient.
5. Connect the flask to the reflux condenser, place on the preheated hot
plate or heating mantle or digestion rack, bring to a boil in ca. 5 min,
and boil exactly 28 min. Successive sample digestions should be
started at ca. 3 min intervals to facilitate accurate timing.
6. Remove the flask and filter through fine linen (about 18 threads to a
cm) held in a funnel and wash with boiling water until the washings
are no longer acid to litmus (Crucible filter may be used in filtration
steps as accidental tearing of linen may lead to safety concerns and
also accuracy of results may be better with use of crucibles, Porosity
2 filter crucible, 50 mL volume- can be used).Note: Filter aids can
be added for better filtration and recovery of the analyte (filter aid
Celite (R) 545).
7. Bring to boil some quantity of sodium hydroxide solution. Wash the
residue on the linen into the flask with 200 mL of boiling sodium
hydroxide solution.
8. Immediately connect the flask to the reflux condenser and boil for
exactly 30 minutes.
9. Remove the flask and immediately filter through the filtering cloth.
10. Thoroughly wash the residue with boiling water and transfer to a
Gooch crucible prepared with a thin compact layer of ignited
asbestos.
11. Wash the residue thoroughly first with hot water and then with about
15 mL of ethyl alcohol.
12. Dry the Gooch crucible and contents at 105±2 °C in an air oven until
constant weight is achieved.
13. Cool and weigh.
14. Incinerate the contents of the Gooch crucible in a muffle furnace
until all carbonaceous matter is burnt.
15. Cool the Gooch crucible containing ash in a desiccator and weigh
(Dry the crucible with its residues in an oven at 130 °C for 2 h).
 Limit of detection of approx 0.2g/100g crude fibre in the
product.
 Repeatability limit of 0.3 g/100 g when the crude fibre content
is less than 10 g/100 g product and 3% of the average when the
crude fibre content is equal to or greater than 10 g/100 g product.

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  Against use of asbestos, it is recommended to use filter aid
Celite® 545, 22140 Fluka.
Note: Fully automated Crude Fibre Analyzer with filter bags or
crucibles can be used in place of the conventional system described.
Follow the manufacturer’s instructions.
Calculation and
The difference in weight of the crucible before and after ashing is
expression of units
reported as the crude fibre content of the test sample
𝑊1 − 𝑊2
𝐶𝑟𝑢𝑑𝑒 𝐹𝑖𝑏𝑟𝑒 (% 𝑏𝑦 𝑚𝑎𝑠𝑠) = × 100
𝑊
Where:
W = Mass in g of the moisture free test material
W1 = Mass in g of Gooch crucible and contents before ashing
W2 = mass in g of Gooch crucible containing asbestos and ash
Calculate crude fibre on dry wt. basis by giving correction for the
moisture content.
Reference AOAC, 2005, 962.09 Determination of crude fibre

Approved by Scientific Panel on Methods of Sampling and Analysis

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