AnoctJrer  ^9i4m'l  Estimation  of  Morphine  and  Lloyd's  Reagent.  461 
NOTES  ON  THE  ESTIMATION  OF  MORPHINE  AND  ON 
LLOYD'S  REAGENT.1 
By  H.  M.  GoRDiN  and  J.  Kaplan. 
1.  Attempt  to  shake  out  morphine  with  a  mixture  of  alcohol  and 
chloroform  from  a  saturated  solution  of  potassium  carbonate. 
When  a  saturated  solution  of  potassium  carbonate  is  shaken  with 
alcohol  or  a  mixture  of  equal  volumes  of  alcohol  and  chloroform,  most 
of  the  alcoholic  solvent  very  quickly  separates  out  on  the  surface  of 
the  heavier  aqueous  layer.  This  was  proved  by  adding  a  definite 
volume  of  the  alcoholic  liquid  to  an  equal  volume  of  the  saturated 
solution  of  potassium  carbonate,  shaking  the  mixture  vigorously,  and 
reading  off  the  volume  of  the  upper  layer  after  the  liquid  has  sepa- 
rated in  two  layers.  In  all  cases  the  volume  of  the  alcoholic  layer 
was  only  a  little  less  than  the  volume  of  the  alcoholic  liquid  originally 
taken. 
Owing  to  there  being  no  good  immiscible  solvent  for  the  extrac- 
tion of  morphine  from  the  solution  of  its  salts  in  water,  an  attempt 
was  made  to  saturate  such  a  solution  with  potassium  carbonate  and 
to  use  a  mixture  of  equal  volumes  of  alcohol  and  chloroform  as  im- 
miscible solvent.  The  aqueous  liquid,  after  being  shaken  once  with 
an  equal  volume  of  the  alcoholic  liquid,  using  about  40  c.c.  of  each 
for  about  0.1  g.  of  morphine  in  the  form  of  salt,  gave  no  test,  in 
acidified  solution,  with  Mayer's  or  Wagner's  reagent,  while,  on  the 
other  hand,  the  alcoholic  liquid  was  found  to  contain,  besides  mor- 
phine, small  amounts  of  potassium  carbonate,  together  with  small 
amounts  of  other  substances,  coming  either  from  impurities  in  the 
carbonate,  or  from  a  partial  decomposition  of  morphine  by  the  latter, 
or  from  both  sources.  Even  when  the  potassium  carbonate  was  pre- 
viously washed  with  alcohol  and  dried,  the  alcoholic  solution  of  the 
morphine  contained  small  amounts  of  other  substances. 
It  was  thought  that  by  washing  the  residue  left  after  distilling 
off  the  alcoholic  liquid  from  the  morphine  with  a  saturated  solution 
of  the  alkaloid  the  impurities  could  be  eliminated  so  that  the  morphine 
could  be  determined  alkalimetrically.  For  this  purpose  definite 
amounts  of  morphine  were  dissolved  in  acidified  water,  the  solution 
1  Read  at  the  Detroit  meeting  of  the  American  Pharmaceutical  Associa- 
tion, 1914. 
