514  American  Pharmaceutical  Association.  {^pSbeMSS0" 
(a)  When  the  mixture  has  completely  separated,  pour  off  50  grammes  of  the 
chloroform-ether  mixture  into  a  flask  or  beaker,  evaporate  the  solvent  on  the 
water-bath,  add  10  c.c.  of  ether  and  evaporate  again.  Dissolve  the  varnish- 
like residue  in  15  c.c.  of  alcohol  with  heat,  add  water  to  slight  permanent  tur- 
bidity, add  indicator  and  slight  excess  of  acid  solution  and  retitrate  with  centi- 
normal  alkaline  solution. 
( b)  When  the  mixture  has  separated  entirely,  pour  off  50  grammes  into  a 
separatory  funnel,  treat  at  once  with  20  c.c.  of  acidulated  water  ;  after  thorough 
agitation  and  complete  separation,  remove  the  20  c.c.  of  water  into  a  second 
separatory  funnel.  Repeat  the  above  operation  twice  more  with  15  c.c.  of 
acidulated  water.  The  acidulated  water  in  the  second  separatory  funnel  is 
rendered  alkaline  with  ammonia  water,  the  alkaloids  removed  successively 
with  20  c.c.  and  15  c.c.  of  a  mixture  of  3  parts  (by  volume)  of  chloroform  and 
1  part  of  ether.  Collect  the  chloroform-ether  mixture  in  a  tared  flask  and 
distil  off  the  solvent.  The  varnish-like  residue  is  twice  treated  with  8  c.c.  of 
ether,  evaporated  on  a  water-bath,  finally  dried  on  a  water-bath  and  weighed. 
The  varnish-like  residue  is  now  dissolved  in  15  c.c.  of  alcohol,  with  the  aid 
of  heat ;  then  proceed  as  in  a  above. 
For  Powdered  Nux  Vomica  and  Coca  Leaf. — Place  10  grammes  of  the  dry 
drug  into  a  250  c.c.  flask,  add  25  grammes  of  chloroform  and  75  grammes  of 
ether,  stopper  flask  securely,  agitate  well  for  several  minutes,  add  10  grammes 
of  10  per  cent,  ammonia  water  ;  agitate  frequently  and  well  during  one  hour. 
The  suspended  powder  separates  almost  immediately,  and  the  alkaloids  are 
dissolved.  On  adding  10  grammes  more  of  ammonia  water  and  shaking  well, 
the  powder  agglutinates  into  a  lump,  the  liquid  becomes  clear  after  standing  a 
few  minutes,  and  can  be  poured  off  almost  completely.  Treat  50  grammes  of 
the  chloroform-ether  mixture  from  the  nux  vomica  according  to  processes 
a  and  b,  the  coca  leaf  according  to  process  b. 
The  committee  reported  the  following  conclusions  : 
(1)  Haematoxylin  is  the  indicator  par  excellence  for  titrating  alkaloids. 
Brazil  wood  and  cochineal  compare  favorably  with  haematoxylin,  but  are  not 
as  reliable  in  some  cases  ;  nor  do  they  appear  to  be  quite  as  sensitive. 
(2 )  Pure  alkaloidal  material  can  be  titrated  with  satisfactory  results,  except- 
ing the  cinchona  alkaloids.  Such  anomalous  results  were  obtained  with  the 
■cinchona  alkaloids,  that  we  are  inclined  to  think  that  the  nature  of  these  alka- 
loids is  not  fully  understood. 
(3)  The  estimation  of  alkaloids  by  means  of  volumetric  solutions  can  only 
be  carried  out  in  laboratories  where  daily  determinations  are  made.  If  the 
operator  is  not  constantly  in  touch  with  his  end-reaction  tints  he  will  be  unable 
to  secure  satisfactory  results. 
(4)  The  gravimetric  results  based  on  process  b  are  quite  satisfactory,  and  it 
is  with  this  process  that  the  average  worker  will  obtain  the  most  concordant 
results.  While  the  volumetric  process  yields  good  results  in  the  hands  of 
extremely  careful  workers  and  under  the  most  favorable  conditions,  yet  we 
feel  convinced  from  our  work  that  the  method  has  not  been  sufficiently  evolved 
to  recommend  it  for  general  use. 
Respectfully  submitted, 
A.  R.  L.  DohmB, 
Lyman  F.  Kebeer, 
Chairman. 
