Am.  Jour.  Pharm. 
July,  1897. 
Notes  on  Opium  Assaying. 
349 
cinerated  for  total  ash  ;  this,  macerated  with  ioc.c.  water  for  one-half 
hour,  filtered,  and  filter  and  contents  washed  with  water,  I  c.c.  at  a 
time,  until  the  filtrate  measured  20  c.c;  the  filter,  with  insoluble 
portion  of  the  ash,  was  dried,  ignited  and  weighed,  the  difference 
between  that  and  the  total  ash  giving  ash  soluble  in  water.  The  fig- 
ures are  in  terms  of  percentage  and  relate  to  perfectly  dried  opium  ; 
for  convenience  of  comparison  the  percentage  of  impurity  in  the 
crude  morphine  is  appended.  The  figures  in  the  last  column  are 
results  of  another  series  of  experiments,  to  be  mentioned  a  little  later. 
Number. 
Moisture. 
Total  Ash. 
Soluble  Ash. 
Insoluble 
Ash. 
Impurity  in 
Crude 
Morphine. 
Ash  of 
Dregs. 
8 
5-00 
6-37 
3-21 
316 
0*20 
2*68 
10 
5'22 
5  51 
2*95 
2-56 
O'20 
2-56 
4-90 
6-68 
3*50 
3-iS 
14*20 
_  2*92 
5*27 
5-36 
3'i7 
2-I9 
13-20 
1-87 
16 
5-65 
7*15 
3'6o 
3*55 
10*00 
2-94 
17 
5"o5 
5  "53 
3'53 
TOO 
1060 
1  79 
is 
4*95 
7'59 
3,7 
4*42 
10  80 
37i 
19 
3  "47 
5-36 
3"29 
2-07 
470 
r8i 
There  is  no  clue  here  for  an  explanation,  as  comparison  of  No.  8 
with  Nos.  15,  18  and  19  will  prove,  unless  it  were  by  quantitative 
analysis,  which  the  quantity  of  ash  did  not  permit.  The  aqueous 
solutions,  excepting  Nos.  8  and  15  and  all  of  the  insoluble  ashes 
moistened  with  water,  gave  pink  or  red  colorations  with  phenol- 
pthalein,  but  a  single  drop  of  a  very  dilute  sulphuric  acid  dis- 
charged the  color ;  the  insoluble  ashes  were  mixed  with  water  and 
titrated  with  dilute  sulphuric  acid  using  methyl-orange  as  indicator, 
but  the  results  were  as  conflicting  as  the  above  ash  determinations. 
As  a  further  probable  explanation  was  based  upon  the  acidity  of 
the  aqueous  opium  infusion  dissolving  some  of  what  in  the  preceding 
table  is  called  insoluble  ash,  and  the  addition  of  ammonia  afterwards 
reprecipitating  this,  a  series  of  experiments  were  made,  in  which  2 
grammes  were  extracted  with  water,  as  in  the  official  assay,  to  make 
64  c.c.  filtrate ;  the  dregs  were  dried  and  ignited,  and  the  results, 
representing  percentage  of  ash  left  in  the  dregs  of  perfectly  dried 
opium,  are  found  in  the  last  column  of  the  preceding  table.  The 
determination  with  No.  8  was  made  last,  and  was  sufficient  to  shatter 
