Page 78 - Feed Lab
P. 78

Estimation of Calcium                         Suguna Management System     Ver 1.0 / SOP / FQL / P2 - 09  Page  2 of 2


                                                                FTransfer a 25 ml aliquot to a 250 ml beaker and add
                                                                   75ml of distilled water with 2drops of methyl red
                                                                   indicator solution. Add 50% ammonium hydroxide
                                                                   solution  drop  wise  till  brownish  orange  colour
                                                                   obtained.  Add  1  or  2  drops  of  concentrated
                                                                   hydrochloric acid so that the colour of the solution
                                                                   is pink. Add 45ml of distilled water and bring it to
                                                                   boil. (Picture - 10)

                                                                FAfter boiling, add 10ml hot saturated ammonium
                  Picture - 6              Picture - 7
                                                                   oxalate  slowly  with  constant  stirring.  The  stirring
                                                                   time should be one minute. If the red colour of the
           REAGENTS
                                                                   solution  changes  to  orange  or  yellow,  add
           FConcentrated Hydrochloric acid.                        concentrated hydrochloric acid drop wise until the
                                                                   colour again changes to pink. (Picture - 11)
           FMethyl red indicator
                                                                FLeave  for  minimum  4  hours  and  allow  the
           F50% Ammonium Hydroxide solution (v/v).
                                                                   precipitate  to  settle.  Filter  the  supernatant  liquid
           F2% Ammonium Hydroxide solution (v/v).                  through ash less filter paper (Whatman No.1/615A)
                                                                   and wash the precipitate thoroughly with 250ml of
           FAmmonium oxalate solution-saturated.
                                                                   2% ammonium hydroxide solution. (Picture - 12)
           FConcentrated sulphuric acid, AR grade
                                                                FPlace the paper with the precipitate in mixture of
           F0.1N Potassium permanganate (3.2 g / 1litre) AR        125 ml of distilled water and 5 ml of concentrated
                                                                                                   o
                                                                                                           o
              grade.                                               sulphuric acid in a beaker. Heat 70  C to 90  C and
                                                                   titrate with the standard potassium permanganate
                                                                   solution until the first slight pink colour is obtained.
           Standardization of std. Potassium permanganate
                                                                   (Picture - 13)
           Take 125ml of distilled water with 5ml of concentrated
           sulphuric acid in a beaker and add 10ml of 0.1N oxalic
                                       o
                                               o
           acid. Heat above solution to 70  C - 90  C and Titrate
           against potassium permanganate.

           PROCEDURE
           FWeigh  approximately  1g  for  mineral  supplement
              and 2g for feed and feed stuffs in a silica crucible.
              Ignite the sample on a burner till smoke cease off.
                                   o
                          o
              Ignite at 600  C +/- 20  C in muffle furnace for 90
              minutes  to  get  carbon  free  ash.  Remove  the        Picture - 8              Picture - 9
              crucible  from  the  furnace  carefully  and  cool.
              (Picture - 8)

           FTransfer the ash to the 250 ml beaker and add 20
              ml  of  1:3  hydrochloric  acid  till  effervescence
              ceases and add 5 drops of 1:3 nitric acid. Give
              slight  boiling  to  the  solution  and  cool.  Transfer
              through filter paper (Whatman No.1/615A) to 250
              ml volumetric flask. Cool, dilute to the mark and mix
              thoroughly. The solution is also to be used for the
                                                                       Picture - 10             Picture - 11
              estimation of Phosphorus. (Picture - 9)



          Prepared by :                                                             Approved by :
                                                             66                                    Director - Technical
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