482 
Tincture  of  Ojnum. 
f  Am.  Jour.  Pharm. 
t       Oct.,  1883. 
with  alcohol,  and  the  filtrate  and  washings  evaporated  until  the  alcohol 
was  expelled,  a  little  water  being  added.  When  the  contents  of  the 
dish  again  weighed  10  grams,  2*5  cc.  of  alcohol  were  added,  and  a  uni- 
form solution  was  generally  obtained.  This  was  transferred  to  a  small 
flask  with  as  little  additional  water  as  possible,  2'5  cc.  more  alcohol 
added,  and  the  flask  well  shaken.  There  were  now  15  cc.  of  stronger 
ether  added,  the  shaking  repeated,  and  lastly  2  cc.  of  ammoiiia  water 
(10  p.  c.  NH3)  were  added,  and  the  whole  shaken  until  the  crystals  began 
to  separate,  the  shaking  after  this  being  frequently  repeated  for  half  an 
hour.  After  standing  over  night  the  ethereafstratum  Avas  carefully  poured 
oif  on  to  a  filter,  10  cc.  more  ether  added,  and  the  contents  of  the  flask 
rinsed  around  without  shaking.  When  the  ethereal  layer  had  separated, 
it  Avas  poured  off  through  the  filter,  and  the  latter  washed  with  5  cc.  of 
ether,  carefully  dropped  on  to  the  edges  from  a  pipette,  and  allowed 
to  dry.  The  remaining  contents  of  the  flask  were  poured  on,  the 
flask  and  filter  washed,  using  in  all  only  about  10  cc.  of  wash  water. 
The  filter  and  contents  were  then  dried  at  100°C.  (212°F.),  weighed, 
the  morphia  removed,  and  the  weight  of  the  filter  taken  and  sub- 
tracted.   The  result  was  then  calculated  to  grains  to  a  fluidounce. 
The  samples  were  treated  as  nearly  as  possible  alike,  the  quantities 
of  ether,  alcohol  and  ammonia  being  the  same,  and  the  time  allowed 
for  precipitation  about  24  hours  in  all  cases.  It  was  found  impossible 
to  assay  most  of  them  successfully  without  the  alcoholic  precipitation, 
the  morphia  obtained  being  dark-colored  and  impure,  and  in  3  out  of 
4  samples  where  comparative  tests  w^ere  made,  less  in  amount,  tlie 
gummy  matter  separated  by  the  alcohol  apparently  hindering  the  pre- 
cipitation. 
The  U.  S.  P.  process,  as  given  by  Henry  B.  Parsons,  in  his  interesting 
report,  read  before  the  New  York  State  Pharmaceutical  Association 
("Weekly  Drug  News  and  Am.  Pharmacist,''  June  23,  1883)  was 
tried  with  4  of  the  samples,  the  results  being  always  lower,  by  a  vary- 
ing amount  (from  -2  to  '8  grain  to  the  fluidounce),  than  those  obtained 
by  the  other  process.  It  appears  also  that  weighing  the  morphia  on 
balanced  filters,  when  the  U.  S.  P.  process  is  employed,  gives  a  higher 
result  than  that  obtained  by  subtracting  the  weight  of  the  filter  on 
removing  the  morphia.  As  the  crystals  are  remarkably  clean  and  easy 
to  remove,  the  latter  would  seem  to  be  the  more  correct  method.  The 
increase  in  weight  may  possibly  be  due  to  the  formation  of  CaCOg  to 
a  greater  extent  in  the  pores  of  the  inner  filter,  which  is  more  exposed 
to  the  air  during  filtration. 
