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Analysis of the Rice Straw

Rice straw needs to be grinded to small particles (20-80 mm) then


extracted with methanol (ethanol) / benzene (tolune) (1:1) mixture for 8 hours.
The material needs to dry at room temperature, conditioned and moisture content
needs to be estimated. For analysis of the raw material the following methods can
applied:
Ash content
Ash can be determined by burning the material in a muffle furnace in a
porcelain crucible first at 400C for 30 minutes, then at 850C for 45 minutes and
then gravimetrically estimated (Tappi standard 211-om 85).
Lignin content
Lignin, expressed as Klason lignin can be estimated directly according to
the method of the Institute of paper chemistry, Appleton, Wisconsin 428, 1951 as
follows:
About 1 g (exactly weighed) of the extracted sample is put in a 100 ml
beaker and then treated with 20ml of 72% sulfuric acid, added to the sample drop
by drop with constant stirring by a small glass rod. After complete disintegration,
the reaction is allowed to stand and the beaker is covered with a watch glass and
left over night at room temperature. It has been then transferred quantitatively to
a 1 litre round bottom flask, diluted to 3% sulfuric acid, and boiled for four hours
under reflux. The lignin is filtered on an ashless filter paper and washed with hot
distilled water till neutrality, then gravimetrically estimated and ignited at 850C
for 45 minutes. The weight of ash is subtracted to give the ash-free lignin per
cent.
Pentosan estimation
Can be determined by using method proposed by Jayme and Sarten, 1941
and its details are given below :
For each experiment from 2-3 g of the extracted sample (exactly weighed)
are taken and placed in a flat bottom flask of 500 ml capacity together with 75 ml
of distilled water and some glass beads. After fitting the apparatus for working 75
ml of 40% hydrobromic acid are added to the reaction vessel through a dropping
funnel. The reaction vessel is then heated under controlled temperature to obtain
constant distillation rate. The distillation rate should be 50 ml in 15 minutes. The
distillation is repeated 8 times. At the end of the experiment the 400 ml distillate
obtained are completed to 500 ml in a measuring flask.
To 50 ml of the distillate, 2 ml of 13% hydrochloric acid are added, cooled
to about 12C, then 10 ml of ammonium molybdate, solution (25 g/l) are added as
a catalyst, followed by 20 ml of N/20 bromide - bromate solution (a) . After exactly
4 minutes of the appearance of the yellow colour, about 10 ml of 10% potassium
iodide solution are added. After 5 minutes the titration is carried out immediately
against N/20 sodium thiosulphate solution (b) using starch solution as indicator.
The pentosan is estimated according to the following equation :

volume of (a) volume of (b) x 1.375


pentosan % =
dry weight of sample

Holocellulose estimation
Holocellulose is the total carbohydrate fraction (cellulose and
hemicellulose) of the raw material and was estimated according to Wise et al.,
1946 as follows:
The raw material is ground in a laboratory Condux mill to pass a screen of
0.3 mm opening diameter and then extracted with an alcohol benzene (tolune)
mixture (1:1) for 6 hours. 5 gram of the raw material (exactly weighed) are
suspended in 150 ml water at 75C and the solution is stirred mechanically. 10
drops of glacial acetic acid and 1.5 g sodium chlorite are added and the reaction
has been allowed to proceed under vigorous stirring. After 1 hour the same
amount of reagents are added and this process is repeated until the total reaction
time was 4 hours . The solution is then cooled, filtered and washed with distilled
water until free of acid, then with acetone and left to dry. The holocellulose is then
estimated gravimetrically .
Alpha cellulose content
The term alpha cellulose describes that part of cellulose which does not
dissolve in 17.5% sodium hydroxide solution . Alpha cellulose can be determined
according to Zellcheming Merkblatt IV/29 A. About 3 g (exactly weighed) of the
sample (either pulp or holocellulose obtained from the raw material) are put in a
porcelain beaker (250 ml), then 25 ml of 17.5% NaOH are added and the sample
is left to swell for 4 minutes (time was exactly measured from the last drop), and
then pressed with a glass rod for 3 minutes. After pressing , another 25 ml of
sodium hydroxide are added and mixed thoroughly till a homogeneous paste is
obtained (mixing for about 1 minute). The beaker is then covered and left for 35
minutes at 20C . 100 ml of distilled water are then added and the material is
quickly filtered under suction using a sintered glass funnel. The filtrate is then
poured on the paste twice before washing with distilled water . After washing with
distilled water till neutrality 100 ml of 10% acetic acid are added dropwise
followed by distilled water . The temperature must be kept constant at 20C
during the whole experiment. The alpha cellulose is then estimated
gravimetrically after drying at 105- 106 C.

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