394  Estimation  of  Morphine  in  Opium.  {^""au^'isss™" 
method  for  upwards  of  six  months  and  finding  it  not  at  all  satisfactory, 
as  something  more  than  a  rough  assay  was  desired,  I  concluded  to  try 
some  of  the  various  methods  published  and  compare  the  results  obtained. 
The  method  which  I  have  been  using  for  some  time  past  and  which 
leaves  little  to  be  desired  is  essentially  that  published  in  the  Ephemeris, 
by  Dr.  Squibb,  wdiose  kind  permission  I  have  to  describe  it  briefly, 
with  a  few  comments  which  may  not  be  amiss. 
I  have  compared  this  method  with  the  official  one  of  the  Pharma- 
copoeia and  also  with  others,  upon  a  specially  prepared  sample  of  opium 
made  up  from  selected  specimens  which  were  dried,  powdered  and 
thoroughly  mixed.  In  four  different  parts  of  this  sample  the  morphine 
was  determined  by  Dr.  Squibb's  method  and  the  average  of  the  results 
obtained  was  taken  as  the  percentage  of  morphine. 
The  following  is  a  brief  description  of  this  method  of  assay,  as  used 
in  my  own  practice.  It  consists  of  three  distinct  operations,  viz. :  1st. 
The  preparation  of  the  extract.  2d.  Separating  the  morphine  there- 
from ;  and  3d.  The  treatment  of  the  separated  alkaloid. 
1st.  A  convenient  weight  of  the  sample  (preferably  about  10  grams) 
is  introduced  into  an  ordinary  salt  month  vial  of  about  4  to  6  ounces 
capacity,  fitted  with  a  good  cork.  About  100  cc.  of  boiling  water  is 
added,  and  the  bottle  is  tightly  corked  and  allowed  to  stand,  after 
frequent  hard  shaking,  for  from  twelve  to  twenty-four  hours.  The 
n)agma  is  allowed  to  settle,  and  the  dark  extract  is  decanted  upon  a 
filter  of  convenient  size.  When  most  of  this  extract  has  run  through 
into  a  medium  size  beaker,  from  30  to  50  cc.  of  boiling  water  is  added, 
the  bottle  is  well  agitated,  and  the  contents  are  then  transferred  to  the 
filter  with  as  little  hot  water  as  possible.  When  all  the  liquid  has 
drained  through  the  filter  it  is  carefully  washed  down  with  a  very  little 
hot  water,  applied  drop  by  drop  around  the  edges,  and  allowed  to  drain 
as  much  as  it  will.  As  soon  as  the  liquid  ceases  to  drop,  the  beaker 
is  replaced  by  an  evaporating  dish  of  about  100  to  150  cc.  capacity, 
and  the  contents  of  the  filter  are  brought  back  into  the  bottle  by  means 
of  a  small  spatula,  and  again  shaken  up  with  about  50  cc.  of  hot  w^ater. 
They  are  then  thrown  upon  the  same  filter  and  are  washed  completely 
upon  the  filter  from  the  bottle,  this  washing  being  continued  until  about 
100  cc.  have  run  through  into  the  dish,  or  until  the  washings  come 
through  colorless.  The  dish  is  now  placed  upon  a  water-bath  and  the 
weak  extract  evaporated,  adding  to  it  from  time  to  time  the  stronger 
portion  from  the  beaker,  until  the  whole  is  concentrated  to  a  volume 
