.Am. ,  jour^Pharm. |  ^ ssaying  Galenical  Preparations  o f  Opium,  413 
two  assays  are  given  in  the  table  braced  together  under  one  number, 
they  are  duplicate  assays  of  the  same  preparation  ;  No.  2  is  the  assay, 
made  at  a  different  time,  of  the  vinegar  examined  under  No.  I. 
Fliickiger's  process,  for  the  determination  of  morphine  in  crude 
'Opium,  188  g,  applied  to  acetum  opii,  solid  and  fluid  extracts,  tinctures 
•and  wines  of  opium. — When  Professor  Fliickiger  published  his 
method  for  the  determination  of  morphine  in  crude  opium,  it 
appeared  to  the  writer  that  it  could  be  applied  successfully  to  the 
commercial  so-called  solid  and  fluid  extracts  of  opium. 
To  obtain  pure  morphine  as  a  result  of  an  analysis  of  fluid  extract 
of  opium,  was  one  of  the  pia  vota  of  pharmaceutical  assaying.  I 
suppose  that  the  interested  reader  is  familiar  with  the  disappoint- 
ments of  the  older  processes,  the  time  they  absorb,  etc.  (Compare 
Lyons'  Manual  of  Pharmaceutical  Assaying,  1886,  and  the  admirable 
Digest  of  Criticisms  on  the  U.  S.  P.,  i  and  ii?  pages  116  and  245.) 
Fliickiger's  process,  modified  properly  for  fluid  extracts,  etc.,  will 
be  a  delight  to  the  analyst  and  a  considerable  saving  of  time.  The 
short  time  in  which  crystallization  is  effected,  is  decidedly  in  favor 
•of  obtaining  pure  morphine,  while  processes  with  slow  crystalliza- 
tion yield  the  alkaloid  impure ;  if,  when  following  Fliickiger's  pro- 
cess, crystallization  be  delayed,  the  morphine  will  be  impure.  , 
Method. — 50  cc.  of  fluid  extract,  tincture  or  wine  of  opium  are 
evaporated  in  a  waterbath  to  two-thirds  of  the  volume,  or  a  little 
less.  Acetum  opii  is  evaporated  to  dryness,  and  the  residue  treated 
as  a  solid  extract.  The  residue  is  transferred  to  a  separator, 
using  as  little  water  to  wash  as  possible.  Agitate  with  10  cc. 
of  a  mixture  of  equal  volumes  of  ether  and  chloroform.  This 
is  separated  and  rejected,  and  the  operation  is  repeated  with  a 
fresh  portion  of  ether  and  chloroform  (the  ether  must  be  free  from 
alcohol).  The  fluid  is  now  filtered  through  a  moist  filter  of  two 
inches  diameter.  The  filter  is  washed  with  the  rinsings  of  the  sepa- 
rator ;  no  unnecessary  quantity  of  water  to  be  used.  Care  is' 
needed  that  the  filter  does  not  dry  out.  The  total  fluid,  of  about 
the  same  volume  as  the  original  fluid,  is  collected  in  a'wide-mouthed 
bottle  of  100  cc.  capacity  with  round  shoulders  (an  Erlenmeyer 
flask  being  too  fragile).  Then  add  10  cc.  alcohol  of  94  per  cent.,  20 
cc.  ether  and  1  (one)  cc.  ammonia  of  0-96  s.  gr. ;  cork ;  agitate  very 
frequently  during  six  hours  ;  set  aside  in  a  cool  place  over  night ; 
absorb  the  ether  as  stated  above  ;  collect  the  fine  crystals  with  the 
filtrate  on  a  tared  filter  in  the  proper  \vay ;  wash  them  with 
