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Alcoholic content determination
Introduction
    Alcohol is present as a major
     component in most of gelanicals
    There are 2 methods for its
     determination
3.   Distillation method.
4.   Chromatographic method.
Things to consider- special treatments
       Volatile acids & bases: render the
        preparation containing volatile
        bases slightly acidic and vice versa.
       Glycerin: preparation should be
        diluted.
       Iodine: treat solutions with
        powdered zinc, decolorize with sod.
        thiosulphate add few drops of
        NaOH.
Conti…
1.   For liquids presumed to contain 50% v/v
     alcohol or less.
    Mix 25ml sample with equal volume of water in
     a separator.
    Saturate with NaCl & add 25ml solvent hexane.
     shake well to remove any interfering volatile
     substance.
    Draw lower layer and extract twice with hexane.
    Extract this solution thrice with 10ml portions of
     saturated saline.
    Combine these portions and distil as usual
    Take volume having simple ratio to original
     specimen.
Conti…

2. For liquids presumed to contain
   more than 50% v/v alcohol.
 Adjust the conc. of alcohol to
   approximately 25% v/v by diluting
   with water.
 Perform the same procedure as
   above.
Distillation method
   Some precaution are taken
¡   Distillate should be clear if cloudy add
    talc or CaCO3 and filter, adjust temp.
¡   Loss of alcohol should be minimized.
¡   Size of the flask should be 3-4 time
    larger than volume of sample used.
¡   Frothing should be avoided by adding
    H3PO4, H2SO4, tannic acid.
¡   Bumping can be avoided by adding
    small pieces of broken glass, glass
    beads or porous chips.
Method: For liquids presumed to contain
less than 30 % v/v alcohol

   Take 25ml sample add equal volume of
    water and distillate.
   Collect distillate 2 ml less than original
    volume (23ml).
   Add water to make 25ml.
   Adjust temp and find specific gravity or
    refractive index.
   From Alcoholometric table find the %age
    of alcohol.
For liquids presumed to contain more than 30 % v/v
alcohol

   Take 25ml sample add 50ml water and
    distillate.
   Collect distillate 2 ml less than 50ml
    (48ml).
   Add water to make 50ml.
   Adjust temp and find specific gravity or
    refractive index.
   From Alcoholometric table find the % age
    of alcohol.
   (the proportion of alcohol is ½ of liquid so multiply it
    with 2 to get exact % age of alcohol in sample)

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Alcohol distilation

  • 2. Introduction  Alcohol is present as a major component in most of gelanicals  There are 2 methods for its determination 3. Distillation method. 4. Chromatographic method.
  • 3. Things to consider- special treatments  Volatile acids & bases: render the preparation containing volatile bases slightly acidic and vice versa.  Glycerin: preparation should be diluted.  Iodine: treat solutions with powdered zinc, decolorize with sod. thiosulphate add few drops of NaOH.
  • 4. Conti… 1. For liquids presumed to contain 50% v/v alcohol or less.  Mix 25ml sample with equal volume of water in a separator.  Saturate with NaCl & add 25ml solvent hexane. shake well to remove any interfering volatile substance.  Draw lower layer and extract twice with hexane.  Extract this solution thrice with 10ml portions of saturated saline.  Combine these portions and distil as usual  Take volume having simple ratio to original specimen.
  • 5. Conti… 2. For liquids presumed to contain more than 50% v/v alcohol.  Adjust the conc. of alcohol to approximately 25% v/v by diluting with water.  Perform the same procedure as above.
  • 6. Distillation method  Some precaution are taken ¡ Distillate should be clear if cloudy add talc or CaCO3 and filter, adjust temp. ¡ Loss of alcohol should be minimized. ¡ Size of the flask should be 3-4 time larger than volume of sample used. ¡ Frothing should be avoided by adding H3PO4, H2SO4, tannic acid. ¡ Bumping can be avoided by adding small pieces of broken glass, glass beads or porous chips.
  • 7. Method: For liquids presumed to contain less than 30 % v/v alcohol  Take 25ml sample add equal volume of water and distillate.  Collect distillate 2 ml less than original volume (23ml).  Add water to make 25ml.  Adjust temp and find specific gravity or refractive index.  From Alcoholometric table find the %age of alcohol.
  • 8. For liquids presumed to contain more than 30 % v/v alcohol  Take 25ml sample add 50ml water and distillate.  Collect distillate 2 ml less than 50ml (48ml).  Add water to make 50ml.  Adjust temp and find specific gravity or refractive index.  From Alcoholometric table find the % age of alcohol.  (the proportion of alcohol is ½ of liquid so multiply it with 2 to get exact % age of alcohol in sample)