1.0 PURPOSE
The purpose of the document is to establish a general and uniform method for the determination of the unsaponified matter in oil and fat.
The purpose of the document is to establish a general and uniform method for the determination of the unsaponified matter in oil and fat.
3.0 SCOPE
This standard testing procedure is suitable for the determination of the unsaponified matter in oil & fat.
4.0 RESPONSIBILITY
The expert and trained chemist are responsible for following this procedure. The technical manager is responsible for implementing this procedure.
5.0 REQUIREMENTS
5.1 Apparatus
5.1.1 Reflux condenser
5.1.2 Water bath or Hot plate
5.1.3 Analytical Balance
6.0 Glassware
6.1.1 Round Bottom Flask-250ml
6.1.2 Separating funnels-500ml
6.1.3 Pipette-10ml
6.1.4 Measuring Cylinder-50 ml
7.0 Reagent
7.1.1 Alcoholic KOH: Dissolve 70-80 g KOH in equal quantity of distill water and make with 95% ethanol.
7.1.2 Ethyl alcohol 95 %
7.1.3 Phenolphthalein indicator solution –1 g in 100 ml ethyl alcohol
7.1.4 Petroleum ether
7.1.5 Aqueous alcohol - 10 % v/v
7.1.6 Standard NaOH – approx. 0.02N
7.1.7 Acetone
8.0 PROCEDURE
8.1.1 Weigh 5 g of the well mixed sample into a flask
8.1.2 Add 50 ml alcoholic KOH solution.
8.1.3 Boil gently under reflux condenser for1 hr or until the saponification is complete.
8.1.4 Wash the condenser with 10 ml of ethyl alcohol.
8.1.5 Cool the mixture& transfer into a separating funnel.
8.1.6 Complete the transfer by washing the flask with some ethyl alcohol and then with cold water.
8.1.7 Add 50 ml water to the separating funnel followed by addition of 50 ml petroleum ether
8.1.8 Insert the stopper and shake vigorously for at least 1 min and allow to settle until both the layers are clear.
8.1.9 Transfer the lower layer containing soap solution to another separating funnel & repeat the ether extraction at least six times using 50 ml ether each. (If emulsion is formed add a little quantity of ethyl alcohol or alcoholic KOH solution)
8.1.10 Collect all the ether extracts in a separating funnel, wash the combined extracts in the funnel with 25 ml aq. alcohol each for 3 times (shake vigorously and draw the alcohol – water layer)
8.1.11 Again wash the ether layer with 20 ml portions of water until the wash water no longer turns pink on addition of few drop of phenolphthalein indicator.
8.1.12 Do not remove any of the ether layers.
8.1.13 Transfer the ether layer to a flask & add 3-4 glass beads & evaporate to dryness on a water bath under a gentle stream of clean dry air.
8.1,14 Place the flask in an air oven at 80-90 0C for 1 hr. to remove the moisture.
8.1.15 Add a few ml of acetone & pass a gentle stream of clean dry over the surface of the material or evacuate using a water vacuum pump at about 50°C for about 15 minutes.
8.1.16 Cool in the desiccator and weigh.
8.1.17 Repeat evacuating, cooling and weighing until constant weight is obtained.
8.1.18 After weighing take up the residue in 50 ml of warm neutral ethyl alcohol.
8.1.19 Containing a few drops of phenolphthalein indicator and titrating with standard NaOH solution.
Weight of fatty acids in the
extract (as Oleic acid, in g) = B = 0.282 XSTVX N
Where,
V = Vol. of standard NaOH used in sample (STV)
N = Normality of 0.02 N NaOH
Unsaponifiable
matter (% by wt) = (100×(A-B)/W
Where,
A = Weight
in g of residue
B = Weight
in g of fatty acids in the extract
W =Weight
of the sample (in g)
10.0 REVISION/CHANGE HISTORY
11.0 REFERENCE & FORMATS
· Appendix-1: FLOW CHART OF UNSAPONIFIED MATTER
12.0 REVISION HISTORY
· Clause no. 8 of IS 548 Part I:1964; (RA 2015), Amd.-5,1996
END OF THE DOCUMENT
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