Am.jour  Pharm.  j        Determination  of  Morphine.  699 
and  5  Cc.  of  dilute  ammonium  hydroxide.  The  now  alkaline  mix- 
ture was  well  shaken,  then  allowed  to  stand  over  night.  It  was 
filtered  through  a  cotton  plug  and  washed  with  20  Cc.  of  ether  and 
a  sufficient  quantity  of  morphinated  water,  in  the  manner  laid  down 
by  Stevens  for  the  assay  of  opium  (Pharm.  Arch.,  1903,  V,  41-45). 
The  cotton  plug  was  transferred  back  to  the  precipitation  flask,  into 
which  all  morphine  in  the  funnel  was  washed  by  a  stream  of 
sulphuric  acid.  When  all  the  morphine  had  dissolved  in  this  meas- 
ured quantity  of  acid,  the  solution  was  titrated  with  standard  sodium 
hydroxide,  lacmoid  being  the  indicator. 
Total  acid  used  in  titration  =  25.00  Cc. 
Acid  equivalent  to  the  alkali  =  12.88  Cc. 
Acid  equivalent  to  the  morphine  =  12.12  Cc. 
This  corresponds  to  0.3672  Gm.  morphine  found. 
Weight  of  morphine  originally  taken  =  0.4172  Gm. 
Loss  in  precipitation  =  0.0500  Gm. 
Experiment  p. — In  this  case  also  precipitation  was  effected  in 
the  presence  of  alcohol  and  ether,  but  the  total  volume  of  solution 
was  smaller,  and  the  amount  of  ammonium  hydroxide  in  excess  was 
observed.  Crystallized  morphine  was  weighed  into  a  stoppered 
flask  and  dissolved  in  2.5  Cc.  N  sulphuric  acid.  To  this  2.5  Cc.  of 
alcohol,  10  Cc.  of  ether  and  7.5  Cc.  of  0.36  N  ammonium  hydroxide 
were  added  successively.  The  manipulation  which  followed  was  the 
same  as  in  Experiment  8,  except  that  the  washing  was  conducted 
with  distilled  water  (10  Cc.)  instead  of  water  saturated  with  mor- 
phine. 
Since  1  Cc.  of  this  standard  acid  =  0.0300  Gm. 
Titration  results  : 
Total  acid  used  =  15.00  Cc. 
Acid  equivalent  to  the  alkali  =  5.80  Cc. 
Acid  equivalent  to  the  morphine  =  9.20  Cc. 
Since  1  Cc.  of  this  standard  acid  =  0.0300  Gm.  morphine 
Weight  of  morphine  found  =  0.2760  Gm. 
Weight'  of  morphine  originally  taken  =  0.3000  Gm. 
Loss  in  precipitation  =  0.0240  Gm. 
Experiment  10.- — The  excess  of  ammonium  hydroxide  used  in 
precipitation  was  larger,  but  the  total  amount  of  ammonium  salt 
