Practical No.

23

Determination of total fibre in cereal sample by gravimetry

Gravimetry
This type of analysis is based upon the measurement of mass obtained either by precipitation or
removed by volatilization. The quantitative determination the former involves isolation of an ion
in solution by a precipitation reaction, filtering, washing the precipitate free of contaminants,
conversion of the precipitate to a product of known composition, and finally weighing the
precipitate and determining its mass by difference.

Experiment methodology:

1- Take 5 g of the cereal powder and defat it by continuous extraction using petroleum
ether.
2- Add 2.50 g of defatted material in a flask containing 200 mL of 1.25%, v/v sulphuric
acid.
3- Heat the mixture was under reflux condensation for 4 h with occasional shaking.
4- Allow the contents to cool to room temperature and filter under vacuum using a Buchner
funnel.
5- Wash the residue on filter paper with boiling water and transfer to the flask followed by
addition of 200 mL of 1.25%, w/v sodium hydroxide solution.
6- Heat the mixture was under reflux condensation for 4 h with occasional shaking.
7- Allow the contents to cool to room temperature and filter under vacuum using a Buchner
funnel.
8- Wash the residue sequentially with boiling water, hydrochloric acid and petroleum ether,
and dry in an oven.
9- Place the dried residue in a tarred crucible and ignite at 550° C until free from carbon.
10- Allow the ash to cool to room temperature in desiccator and weigh.

Observations

W1 (empty dish) =​ ​55.92 g

W2 (dish + dry powder) = 57.22 g

W3 (dish + ash) = 55.93

Calculations

W1 W2 (dish W3 (dish W4 (dry W5 (ash) % yield Crude %

(empty + dry + ash) powder) fiber fiber
dish) powder)

55.92 57.22 55.93 W​2 ​-w​ 1​= W​3​ -W​1​= W5/W4*100 W2-W3/2 51.6*100
=0.76923077 .5
=51.6
0.01
1.3 =0.56

Conclusion:​Hence the total percentage of crude fibre in 2.50g of cereal sample as determined by
gravimetry is 51.6%