Page 116 - Feed Lab
P. 116

Suguna Management System      Ver 1.0 / SOP / FQL / P2 - 30  Page  1 of 2



























           30. Estimation of Unsaponifiable Matter


                                                                FBoil gently but steadily under reflux for 1 hr or until
           SCOPE
                                                                   completely saponified .Complete saponification is
           To determine Unsapanifiable matter in vegetable oils    essential.
           and this applicable to testing of vegetable fats and oils.
                                                                FTransfer  sample  quantitatively  to  the  500  ml
                                                                   separating funnel with 3- 4 washings of 25 ml of
           APPARATUS
           FSoxhelt flask - 250 ml Capacity.                       petroleum ether and then add 50 ml of petroleum
                                                                   ether.
           FLei big condenser
                                                                FInsert  the  stopper  and  shake  vigorously  the
           FSeparating funnel - 500 ml                             separating  funnel  for  at  least  1  min.  Then  allow
                                                                   settling till the charge is clearly split in two layers.
           FExtraction Cylinder -Graduated with Glass stopper
              Cap. 200ml                                        FRemove the lower layer as completely as possible
                                                                   in a 500 ml beaker (B-1) without including any of the
           CHEMICALS
                                                                   upper  Portions.  Transfer  upper  layers  to  500  ml
           FEthyl alcohol, 95%.                                    beaker (B-2).
           FAqueous potassium hydroxide (KOH) : 50% by          FTransfer the contents of beaker (B-1) to separating
              weight,  prepared  by  dissolving  50  g  of  reagent   funnel and  repeat  the extraction at least six  times,
              grade KOH in 50 ml of distilled water with cooling.   using 50 ml   portions of petroleum   ether   each
                                                                   time    and    shaking    vigorously    with  each
           FPetroleum ether; AR grade
                                                                   extraction.
           FSodium  hydroxide  (NaOH)  solution  0.02  N  -
                                                                FAllow  the  contents  to  settle  and  remove  lower
              accurately standardized
                                                                   portion  to  (B-1).Transfer  upper  layer  to  (B-
           FPhenolphthalein indicator solution : 1.0% in 95%       2).Transfer contents of (B-2) to separating funnel.
              ethyl alcohol.
                                                                FWash  the  combined  extracts  in  the  separating
                                                                   funnel  three  times,  using  25ml  portions  of  10%
           PROCEDURE
                                                                   ethyl  alcohol  in  Hot  distilled  water,  shaking
           FWeigh about 5 gm ± 0.1 mg of well mixed sample in      vigorously and drawing out the aqueous alcohol
              to a Soxhelt flask. Add 30 ml of 95% ethyl alcohol   layer after each extraction.
              and 5 ml of 50% KOH solution.




          Prepared by :                                                             Approved by :
                                                            104                                    Director - Technical
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