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Estimation of Crude Protein- Macro Kjeldhal Method  Suguna Management System  Ver 1.0 / SOP / FQL / P2 - 03  Page  2 of 3


                                                                   250 ml of distilled water, AR grade

                                                                FNitrogen  free  concentrated  sulphuric  acid,  AR
                                                                   Grade.


                                                                BLANK
                                                                FTake 5gm activated sodium sulphate + 0.5gm of
                                                                   cupric  sulphate  and  25  ml  of  concentrated
                                                                   sulphuric acid to the Kjeldhal flask and do digestion
                   Picture-5               Picture-6
                                                                   and distillation as per the crude protein procedure.
                                                                   This is reagent blank. The reagent blank and direct
                                                                   blank should be identical.

                                                                RECOVERY
                                                                FTake 0.1 gm of urea and add 5gm activated sodium
                                                                   sulphate + 0.5gm of cupric sulphate and 25 ml of
                                                                   concentrated sulphuric acid to the Kjeldhal flask
                                                                   and do digestion and distillation as per the crude
                                                                   protein procedure.
                   Picture-7               Picture-8
                                                                Calculation:
                                                                   A = (28/60.06)x100
                                                                   B = % of Nitrogen  after distillation
                                                                   Then (A/B) x 100 =recovery should
                                                                   be 100+/- 1%


                                                                PROCEDURE
                                                                FTake accurately 2gm of ground sample on butter
                                                                   paper.  Fold  the  above  sample  and  transfer  to
                                                                   Kjeldhal flask. (Picture-11)
                   Picture-9               Picture-10
                                                                FAdd 10gm activated sodium sulphate + 0.5gm of
                                                                   cupric  sulphate  and  25  ml  of  concentrated
           REAGENTS
           F40% sodium hydroxide w/v, AR grade                     sulphuric acid to Kjeldhal flask. (Picture-12)

           FSodium Sulphate , AR grade                          FDigest  for  90  minutes  to  105  minutes,  till  the
                                                                   solution turns green/straw yellow colour. Cool the
           FCupric Sulphate                                        flask and add approximate 100 ml to 200 ml water.
                                                                   Then shake well. (Picture-13)
           F0.25  N  sodium  hydroxide  (10.1g  of  sodium
              hydroxide in one litre of water).                 FAfter  cooling  the  flask,  it  is  fitted  to  Kjeldhal
                                                                   distillation  apparatus  and  fit  to  all  glassware's
           F0.5 N sulphuric acid (14 ml of sulphuric acid in 1 litre
              of water).                                           properly without any leakage. (Picture-14)
                                                                FTake 20 ml of 0.5N sulphuric acid with 2 drops of
           FMethyl red indicator.
                                                                   methyl red indicator in the conical flask, which is
           FPhenolphthalein indicator.                             receiver solution. (Picture-15)

           F0.1 N Potassium Hydrogen Phthalate - 5.1055 g /





          Prepared by :                                                             Approved by :
                                                             52                                    Director - Technical
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