Am'jJu°ne;  iP906arm'  1    Assay  of  Opium  and  its  Preparations.  263 
labor  was  to  ascertain  where  the  error  lay  and  to  correct  the  same, 
if  possible. 
The  full  modified  process  will  first  be  given.  (The  portions  in 
italics  are  the  additions.)  After  which,  such  points  will  be  dilated 
upon  as  may  prove  of  interest,  as  well  as  giving  reasons  for  the 
changes. 
Place  4  grammes  of  dried  or  powdered  opium  in  a  100  c.c.  tared 
porcelain  evaporating  dish,  "  add  5  c  c.  of  KOH  solution,  5  per  cent, 
or  its  equivalent  of  a  stronger  solution,  mix  thoroughly  with  a  rubber- 
tipped  glass  rod  and  evaporate  on  water -bath  or  drying  closet \  until  of 
constant  weight"  then  add  2  grammes  of  dry,  freshly-slaked  lime  and 
10  c.c.  of  water  and  triturate  continually  for  fifteen  minutes  until  a 
perfectly  smooth  mixture  results.  Finally,  add  19  c.c.  of  water, 
triturating  frequently  during  half  an  hour  and  filter  through  a  dry 
filter  about  10  centimeters  in  diameter.  Transfer  exactly  15  c.c.  to 
a  100  c.c.  Erlenmeyer  flask  and  add  to  this  4  c.c.  of  alcohol  and  10 
c.c.  of  concentrated  ether  and  shake  the  mixture.  Then  add  -500 
gramme  ammonium  chloride.  Shake  well  and  frequently  during  half 
an  hour.    Set  aside  in  a  cool  place  for  twelve  hours. 
Remove  the  stopper  carefully  and  preserve  with  any  adhering 
crystals,  for  future  use.  Pour  the  ethereal  layer  into  a  small  funnel, 
the  neck  of  which  has  been  previously  closed  with  a  piece  of  ab- 
sorbent cotton.  Rinse  the  flask  with  10  c.c.  of  ether,  shake  con- 
tinually  for  five  minutes  and  pour  as  before  into  the  funnel,  and  when 
this  has  passed  through,  pour  the  contents  of  the  flask  into  the  funnel. 
Add j  c.c. of  ether  to  the  flask,  rotate  gently  and  pour  into  funnel,  repeating 
with  5  c.c.  more  of  ether.  Without  trying  to  remove  all  the  crystals  from 
the  bottle,  wash  the  flask  and  contents  of  the  funnel  with  saturated 
solution  of  morphine,  small  portions  at  a  time,  using  13  c.c.  in  all. 
When  the  crystals  have  drained,  place  the  funnel  in  the  bottle  con- 
taining adhering  crystals,  and  with  a  small  rod  drawn  out  to  a  curved 
point,  lift  the  cotton  and  rinse  the  crystals  into  the  bottle  with  12  c.c. 
of  decinormal  sulphuric  acid,  using  the  cotton  on  the  end  of  the  rod 
to  detach  any  adhering  crystals.  Place  the  cotton  carefully  into  the 
flask,  replace  the  stopper  and  agitate  until  the  crystals  are  all  dis- 
solved. Rinse  the  cork  and  funnel  with  water,  titrate  the  excess  of 
acid  with  fortieth  normal  potassium  hydroxide  solution,  using 
hematoxylin  as  an  indicator. 
Divide  the  number  of  cubic  centimeters  of  potassium  hydroxide 
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