School of Industrial

Technology
Faculty of Applied Sciences
____________________________________________________

FST 556
PRACTICAL 6:
DETERMINATION OF CRUDE FIBRE
Date of experiment: 19th May 2020
Laboratory Group: Tuesday

Name : NUR NADHIRAH BINTI HAMZAH

Student ID : 2019362053
Group : AS2464C

MARK:
 PRACTICAL 6
DETERMINATION OF CRUDE FIBRE

Acid and Alkali Digestion Method

INTRODUCTION

Dietary fibre can be defined as the sum of polysaccharides and lignin that are not
digested by human digestive enzymes. Dietary fibre can be classified as soluble
dietary fibre (SDF) and insoluble dietary fibre (IDF) depending on the physical
characteristics and effects on the body. Cellulose, non-cellulose like hemicelluloses
and pectin, lignin, and hydrocolloids (gums, mucilages, and algal polysaccharides)
are the major components of dietary fibre. Human foods mostly contain non-cellulose
polysaccharides, some cellulose and a small amount of lignin. The average
proportions of polysaccharides which are not cellulose. For common foods, cellulose
and lignin are about 70%, 20% and 10% respectively.

Crude fibre is the fuel residue left after the other carbohydrates and proteins
extracted by sequential digestion of a sample by acid hydrolysis with H2SO4 is used
for sugar and starch extraction followed by alkaline hydrolysis with NaOH, which
extracts proteins and some hemicellulose and lignin under different conditions. Crude
fibre is determined by treating a sample with ether to remove fats, then boil it in a
weak acid and a weak alkali or base alternately.

In the analysis of cellulose-containing foods, the determination of crude fibre is

widely used. Crude fibre includes theoretically, materials that are indigestible in the
human and animal organism. It is determined as material insoluble in dilute acid and
dilute alkali under specific conditions.

Cellulose and lignin comprise around 97% of the residue from a determination of
synthetic fibre. However, it does not initially represent all of the cellulose and lignin
available. Additionally, crude fibre is a mixture of cellulosic materials and does not
reflect any specific compound or compound group.

In addition, despite its non-specific structure, crude fibre is a useful parameter in

food and feed analysis. Crude fibre is widely used as an index of the feeding value of
poultry and stock feeds, to evaluate the efficiency of friction and bran separation from
starchy endosperm and to determine the chemical succulence of fresh vegetables
and fruit.
OBJECTIVE

To determine the amount of crude fibre in samples using acid and alkali digestion
method.

MATERIALS

0.255 N sulphuric acid, 0.313 N sodium hydroxide, 1% hydrochloric acid, beaker,

crude fibre apparatus, analytic balance, oven, muffle furnace, desiccator and
measuring cylinder.

METHODS

1. 2 g ±0.0001(W1) of dried ground sample was weighed into 600 ml beaker fitted with
a reflux condenser.

2. 200 ml warm 0.225 N H2SO4 was added and was boiled for 30 minutes exactly from
the onset of boiling (if heated using hotplate, use watch glass to prevent loss of
solvent during digestion)

3. The weight of filter paper used was recorded throughout the experiment.

4. Contents was filtered while hot through with ashless filter paper Whatman No 541
or equivalent and the residue was washed with hot water until free from acid (check
with litmus paper)

5. The insoluble materials were transfer quantitatively into original beaker.

6. 200 ml warm 0.313 N NaOH was added and was boiled for exactly 30 minutes.

7. 3-5 drops of n-octanol was added as antifoam agent.

8. Contents were filtered and the residue was washed with hot water, then with 15 ml
of 1% hydrochloric acid twice.

9. Washed with hot water again until neutral or free from acid.

10. The insoluble material was transfer into a weigh crucible and dried in oven at
105°C overnight to constant weight.

11. The weight of residue and crucible was recorded

12. The dried sample was burned gently over a Bunsen burner until smoke was no
longer evolved when heated strongly.

13. The residue was ignited in a muffle furnace at 550°C for 3 hours.

14. The crucible was cooled in the desiccator and was weighed.

15. The weight of ash and crucible (W3) was recorded. The loss in weight on ignition
represent the weight of crude fibre.

Calculation

W 2 −W 3
X 100
g crude fibre per 100g sample = W1

Where,

W1 = weigh in gram of sample taken

W2 = weigh in gram of weigh of crucible + dried residue

W3 = weigh in gram of weight of crucible + ash

 RESULTS

Table 6.1: Raw data for crude fibre analysis using acid-alkali digestion method

Sample: Popcorn kernel

Weight of Weight of
Weight of Weight of empty crucible + Weight of
% crude fibre
Replicate sample filter paper crucible dried crucible + ash
content
(g) (g) (g) residue (g)
(g)

1 2.0036 2.2493 62.4706 63.2611 63.2033 2.8848

2 2.0022 2.3073 72.1662 72.9802 72.9206 2.9767

3 2.0028 2.3311 65.8866 66.6915 66.6323 2.9559

Average±SD 2.9391±0.0482

Sample: Chickpeas

Weight of Weight of
Weight of Weight of empty crucible + Weight of
% crude fibre
Replicate sample filter paper crucible dried crucible + ash
content
(g) (g) (g) residue (g)
(g)

1 2.0012 2.1935 72.0087 72.4093 72.3833 1.2992

2 2.0016 2.2985 65.9743 66.3537 66.3268 1.3439

3 2.0007 2.3018 71.9874 72.4102 72.3827 1.3745

Average±SD 1.3392±0.0378
QUESTIONS

1. Differentiate between crude fibre and dietary fibre.

Dietary fibres perform essential biological functions as indigestible complex
carbohydrates but they do not supply any calories or nutrients and are immune to
digestive enzymes. Dietary fibre comes from plant cell walls and consists of cellulose,
hemicellulose, lignin, pectin, mucilage, and gum. Many food products list total grams
of fibre, which includes both soluble and insoluble fibre.
Crude fibre refers to one type of dietary fibre, the form that persists as a residue
after food receives standardized dilute acid and alkali laboratory treatment. The
treatment dissolves all the soluble fibre in a food and some of the insoluble fibre. The
residual or crude fibre is composed primarily of cellulose and lignin. According to the
Commission on Life Sciences of the National Research Council, crude fibre is a
nutritionally obsolete term. Crude fibre measurements, the result of laboratory study,
could underestimate 50% or more of the actual dietary fibre in a food item.

2. What are the factors that greatly affect the accuracy of crude fibre analysis?
Factor that are greatly affected the accuracy of crude fibre determination is the
manipulation and the procedures of the experiment itself.
DISCUSSIONS

In this practical, acid and alkali digestion method was used to determine the
crude fibre content in food sample. Two different food samples have been used in this
practical. The food samples that were used are popcorn kernel and chickpeas. Crude
fibre refers to the residue of a feed that is insoluble after successive, boiling with dilute
acid and alkali. The alkaline hydrolysis will remove protein and some carbohydrates.
This process also removes some hemi-cellulose and lignin. Besides, only partial
recovery of fibre components is achieved. The portion of the total carbohydrate of a
food that is resistant to the acid and alkali treatment is the crude fibre. In this practical,
2g was needed for each kind of dried sample for analysis. During the acid digestion,
some soluble hemicelluloses are solubilised and are also extensively and variably
solubilised in the alkaline digestion. In addition, this indigestible components will be
considered as part of the nitrogen-free extract, causing a serious error in the
calculated nutritive value of the food. The chemical reagent that was used in this
practical was 0.255 N sulphuric acid (H2SO4), 0.313 N sodium hydroxide (NaOH) and
hydrochloric acid (HCl) 1%.

The results of experiment acid and alkali digestion method for three trials were
taken for each samples and percentage were calculated by formula given. For
popcorn kernel, the mean percentage of crude fibre that was obtained is 2.9391%
while chickpeas is 1.3392%.

CONCLUSION

In conclusion, the objective of the experiment was successfully achieved after

conducting the experiment. The amount of crude fibre in popcorn kernel and
chickpeas have been successfully determined by using acid and alkali digestion
method. The popcorn kernel was determined to have 2.9391% of crude fibre while
chickpeas is 1.3392%.
REFERENCE

National Research Council. (1989). Recommended Dietary Allowances (10th Edition).

Washington, DC: The National Academies Press.
Van Soest, P., & McQueen, R. (1973). The chemistry and estimation of fibre.
Proceedings of the Nutrition Society, 32(3), 123-130.
doi:10.1079/PNS19730029
Wolters, A. (n.d.). Differences Between Crude and Dietary Fiber. Retrieved from
LiveStrong.com:
https://www.livestrong.com/article/480986-differences-of-crude-and-dietary-fib
er/