Am.  Jonr.  Pharni.\ 
August,  1895.  J 
Determination  of  Morphine. 
399 
The  author  gives  preference  to  the  various  methods  in  the  follow- 
ing order  : 
(1)  Ash  method. 
(2)  Titration. 
(3)  Lime  water  method. 
(4)  Absolute  alcohol. 
A  comprehensive  series  of  assays  was  made  from  one  sample  of 
powdered  opium,  allowing  the  separation  of  the  crude  morphine  to 
take  place  during  periods  of  time  ranging  from  three  to  thirty-six 
hours. 
The  tabulated  results  are  as  follows : 
Number  of  hours  allowed  for  pre- 
3 
5 
8 
12 
16 
20 
24 
36 
Per  cent,  of  crude  morphia  in  the 
opium  
13*03 
14-32 
I4"35 
14-72 
14*80 
14-81 
14*85 
14*98 
i5*i7 
Per  cent,  of  ash  in  the  crude  morphia 
0*91 
-•33 
1-41 
i-8i 
1-90 
2-00 
210 
2-63 
3"oo 
Per  cent,  of  pure  morphia  in  the 
crude  morphia  by  the  ash  method. 
98'54 
97*34 
97'35 
97*63 
96  65 
96  28 
96-10 
95-06 
94*45 
Per  cent,  of  pure  morphia  in  the 
opium  by  the  ash  method.  Based 
12-84 
13  "94 
13*07 
14*22 
14-28 
1426 
14-27 
I4-24 
i4*32 
Per  cent,  of  pure   morphia  in  the 
crude  morphia  by  the  lime-water 
99-10 
98-01 
98-21 
97*32 
96-70 
96-40 
96-31 
96'02 
96*21 
Per  cent,  of  pure  morphia  in  the 
opium  by  the  lime-water  method  . 
12-91 
14*03 
14-09 
H'3i 
i4*3i 
I4-27 
14*31 
H'39 
14*59 
Per  cent,  of  pure  morphia  in  the 
crude  morphia  by  titration    .  . 
98-17 
97*26 
97*56 
97*03 
96-52 
96-31 
96-31 
95-8i 
95-02 
Per  cent,  of  crude  morphia  in  the 
12-78 
13-92 
13*99 
14-28 
14-28 
14-26 
14*30 
14*35 
14-41 
According  to  the  above  table  there  is  a  decided  increase  both  in 
impurity  and  morphine  as  time  increases;  also  an  appreciable  aug- 
mentation is  noted  in  the  twelve-hour  assay  when  compared  with 
the  eight-hour  assay,  which  immediately  precedes  it. 
The  presence  of  meconic  acid,  potassium  and  calcium  was  estab- 
lished in  morphine  of  three  hours'  precipitation,  and,  after  appro- 
priate experiments,  the  author  concludes  that  the  addition  of  the 
alcohol  in  the  assay  process  hastens  the  precipitation  of  a  part  of 
the  impurity. 
The  author  thinks  that  a  slight  modification  of  the  present  pro- 
cess would  yield  a  crude  morphine  needing  no  correction,  i.  e.,  that 
the  amount  of  impurity  associated  with  the  morphine  would  not 
exceed  the  amount  of  morphine  lost  during  the  operation. 
The  deposit  which  forms  in  the  mother  liquor,  mixed  with  the 
wash  water,  rejecting  the  alcoholic  and  ethereal  washings,  was  coi- 
