Am.  Jour.  Pharm.  \ 
September,  1894.  / 
The  Opium  Assay  Method. 
439 
allowing  to  settle  and  washing  by  decantation,  In  experiments 
made  by  Dr.  Squibb  upon  the  respective  merits  of  the  alcohol  and 
the  lime-water  corrections  for  the  impurities  in  the  crude  morphine, 
reference  is  made  to  the  difficulty  of  filtering  the  alcoholic  solution ; 
the  insoluble  matter,  owing  to  its  being  an  extremely  fine  powder, 
was  very  apt  to  run  through  the  filter.  Finding  that  both  methods 
gave  practically  the  same  correction,  Dr.  Squibb  determined  to  con- 
tinue to  use  the  lime-water  test  as  here  give,n,  there  was  no  difficulty 
in  filtering.  To  one  of  these  mother-liquors  (No.  5),  after  standing 
for  about  a  month,  was  added  as  much  water  as  was  used  in  wash- 
ing and  set  aside  for  a  week,  when,  to  all  appearances,  a  somewhat 
increased  precipitate  was  to  be  noticed ;  lack  of  time  not  permit- 
ting an  investigation  of  this  precipitate,  it  would  not  seem  justifiable 
to  state  this  additional  precipitate  to  be  morphine  thrown  out  by 
diluting  the  alcoholic  mother-liquor  with  water. 
In  determining  the  purity  of  the  morphine  by  the  ignition  method 
one  gram  was  taken  and  by  the  careful  application  of  heat,  the 
morphine  was  first  charred  (in  this  part  of  the  operation  it  was  pos- 
sible to  find  in  the  upper  part  of  the  crucible  or  on  the  lid,  very 
well  formed  crystals  of  morphine)  and  then  by  the  application  of 
more  heat,  the  crucible  contents  incinerated  at  a  low  red  heat;  the 
ignition  of  the  ash  so  as  to  form  calcium  oxide,  while  suitable 
for  those  having  all  laboratory  conveniences,  is  not  often  suitable 
for  the  pharmacist,  therefore,  the  ash  obtained  at  a  low  red  heat  is 
best  moistened,  after  cooling,  with  a  few  drops  of  solution  of 
ammonium  carbonate,  and  gently  heated  first  until  dry  and  then  at 
a  very  low  red  heat ;  this  will  insure  the  ash  to  consist  of  carbonate 
which,  multiplied  by  the  factor  2-56,  gives  the  corresponding  quan- 
tity of  meconate.  This  alteration  had,  as  a  consequence,  the  exam- 
ination of  the  ash,  for  on  moistening  with  water  and  ascertaining  its 
effect  upon  litmus  paper,  I  was  surprised  to  find  a  very  strong  alka- 
line reaction  (no  matter  how  small  the  quantity  of  ash,  an  alkaline 
reaction  was  always  observed  with  litmus  paper) ;  as  this  could  not 
be  due  to  caustic  lime,  because  the  treatment  with  ammonium  car- 
bonate was  for  the  express  purpose  of  changing  any  caustic  lime 
into  the  carbonate,  the  only  other  explanation,  which  was  verified, 
was  that  alkaline  carbonates  were  present ;  upon  filtering  off  the  ash 
insoluble  in  water  and  adding  hydrochloric  acid  to  the  filtrate,  a 
very  distinct  effervescence  was  noticeable  ;  this  acid  solution  gave 
