Am.  Jour.  Pharm.  ] 
Aug.,  1885.  J 
Estimation  of  3Iorphine  in  Opium. 
393 
extract  and  washings  are  obtained.  If  the  extract  conies  through 
cloudy,  which  is  sometimes  the  case,  it  will  have  to  be  refiitered  through 
paper.  The  paper  is  then  washed,  and  the  extract,  then  more  than 
100  cc,  must  be  concentrated  to  that  volume  or  exactly  one  half  taken. 
If  the  extract  in  the  flask  is  exactly  100  co.,  as  it  should  be,  it  is  well 
shaken  to  insure  thorough  mixture  and  allowed  to  stand  and  settle  for 
about  one  hour ;  50  cc,  representing  5  grams,  are  drawn  oflP  with  a 
pipette  and  transferred  to  a  small  beaker,  a  very  slight  excess  of  a 
solution  of  equal  parts  of  ammonia  and  alcohol  is  added,  and  the  liquid 
well  stirred  and  allowed  to  stand  over  night,  when  the  impure  mor- 
phine will  crystallize  out.  These  crystals  (which  it  will  often  be 
found  necessary  to  detach  from  the  sides  of  the  beaker  with  a  small 
steel  spatula)  are  collected  upon  a  tared  filter  and  washed  with  a  little 
cold  water,  applied  drop  by  drop  around  the  edges  of  the  filter,  until 
it  runs  through  almost  colorless.  The  filter  and  contents  are  now 
dried  at  a  temperature  not  exceeding  100°  C,  and  washed  with  about 
25  cc.  of  ether  to  remove  the  narcotine,  again  dried  and  then  weighed. 
From  repeated  ex})eriments  85  per  cent,  of  this  weight  was  found  to 
represent  approximately  the  weight  of  the  morphine. 
The  only  advantages  of  tliis  method  are  its  extreme  simplicity  and 
economy  of  time.  It  Avas  originally  adopted  because  of  the  very  great 
number  of  samples  which  then  required  daily  examination.  In  ordi- 
nary cases  its  disadvantages,  however,  were  found  to  be  many.  It  is 
only  applicable  to  a  moist  opium,  as  this  is  the  only  one  which  will 
yield  an  extract  running  clear  through  the  linen  or  flannel  filter.  It 
is  also  difficult  to  extract  the  opium  completely  in  this  manner  with 
100  cc.  of  water ;  at  least  double  that  amount  is  required.  This  increased 
volume,  however,  would  involve  the  necessity  of  concentrating  the 
liquid,  which,  otherwise,  would  be  too  dilute,  and  thus  time  would  be 
lost.  The  precipitated  morphine  (it  can  hardly  be  called  crystallized) 
is  always  very  impure  and  dark  colored  and  requires  a  great  deal  too 
much  water  to  wash  it,  and  always  carries  with  it  a  large  proportion  of 
narcotine  which  the  ether  will  not  remove  unless  a  large  quantity  is 
used,  and  then  only  imperfectly  ;  the  precipitate  usually  forming  large, 
hard  lumps.  It  is  also  difficult  to  remove  all  the  precipitate  from  the 
sides  of  the  beaker,  which,  however,  would  make  no  difference  if  the 
beaker  were  tared.  The  time  occupied  by  this  method  is  ordinarily 
about  forty-eight  hours,  and  not  more  than  five,  or  at  most  eight 
samples  can  be  conveniently  run  at  the  same  time.    Having  used  this 
