Am.  Jour.  Pbarm.l 
April,  1907.  / 
Acetanilid  and  Phenacetin. 
153 
out  twice  with  water  in  order  to  recover  traces  of  sodium  acetate, 
which  is  somewhat  soluble  in  ether,  and  the  washings  united  with 
the  original  aqueous  residue. 
The  water  solution  is  then  transferred  to  a  flask  of  I  litre  capacity, 
acidified  with  about  25  c.c.  of  85  per  cent,  phosphoric  acid,  and  the 
acetic  acid  is  distilled  off  with  steam.  (It  is  advisable  to  connect 
the  flask  with  the  condenser  by  means  of  a  Kjeldahl's  connecting 
bulb  tube,  so  as  to  prevent  the  carrying  over  of  phosphoric  acid 
into  the  distillate.)  The  distillation  is  interrupted  when  the  distil- 
late no  longer  reacts  acid  to  litmus.  Usually  about  two  hours  are 
required,  and  from  800  to  1000  c.c.  of  distillate  will  have  been  col- 
lected before  this  point  is  reached. 
The  distillate  is  then  titrated  against  sodium  hydroxide,  using 
phenolphtalein  as  indicator.  We  have  found  it  best  to  titrate  against 
N/'i  sodium  hydroxide  with  the  addition  of  1  c.c.  of  1  per  cent, 
solution  of  phenolphtalein.  In  spite  of  the  large  amount  of  liquid, 
the  end-reaction  is  distinctive  under  these  conditions  to  within  002^ 
c.c.  of  N /  I  sodium  hydroxide. 
One  cubic  centimeter  of  N/i  sodium  hydroxide  is  equivalent  to 
0-13409  gramme  acetanilid. 
The  following  results  were  obtained,  working  on  pure  acetan- 
ilid :— . 
I.  Acetanilid  taken,  roo  gramme  ;  amount  found,  0-9953  gramme. 
II.  Acetanilid  taken,  roo  gramme  ;  amount  found,  0*9972  gramme. 
In  order  to  determine  the  general  applicability  of  this  method  to 
miscellaneous  pharmaceutical  preparations,  the  three  following 
mixtures  were  analyzed  for  acetanilid  : 
I. — AN  ELIXIR  CONTAINING  IN  ADDITION  TO  3  5  PER  CENT.  OF  ALCOHOL 
AND  O  947  GRAMME  OF  ACETANILID  IN  IOO  C.C,  THE  FOLLOWING 
INGREDIENTS  :  
Extract  of  Indian  Cannabis, 
Caffeine, 
Sodium  Bicarbonate, 
Sodium  Salicylate, 
Monobromated  Camphor, 
Extract  of  Hyoscyamus, 
Fluid  Extract  of  Gelsemium, 
Fluid  Extract  of  Celery  Seed, 
Aromatic  Spirits  of  Ammonia. 
