Am.  Jour.  Pharm.1 
October,  1899.  J 
Alkaloidal  Assays. 
467 
"  Further  Work  Upon  the  Estimation  of  Alkaloids,"  in  which  also 
are  included  a  few  results  in  comparison  with  the  U.S.P.  method, 
and  a  brief  discussion  of  the  subject. 
THE  MATERIALS  AND  UTENSILS  FOR  THE  ASSAY. 
Opium  in  very  fine  powder.  Powdered  sodium  chloride,  such  as 
is  used  for  the  table.  An  ethereo-ammoniacal  mixture  composed  of 
stronger  ammonia  water  (U.S.P.)  and  alcohol,  of  each  5  c.c.;  chloro- 
form (U.S.P.),  10  c.c,  and  ether,  20  c  c.  Benzol  boiling  at  about  8o° 
C.  A  mixture  of  one  volume  of  absolute  alcohol  and  five  volumes 
of  chloroform.  Twentieth  normal  sulphuric  acid  and  twentieth  nor- 
mal potassium  hydrate  solution.  Neutral  methyl-orange  paper. 
Standard  solution  of  iodine,  of  any  known  strength  in  the  neighbor- 
hood of  1  per  cent.,  and  standard  solution  of  sodium  thiosulphate 
of  about  twentieth  normal  strength. 
A  four  or  six  ounce  screw-top  ointment  jar,  having  a  bottom  con- 
cave within.  A  small  pestle,  just  long  enough  to  rest  half  upright 
within  the  jar  when  it  is  closed.  A  small  glass  percolator  provided 
with  a  stop-cock,  and  of  the  length  of  about  22  centimeters  and 
inner  diameter  of  about  1-3  centimeters.1 
DIRECTIONS  FOR  THE  ASSAY. 
Weigh  out  3  grammes  of  the  opium  into  the  ointment  jar,  rub  it  up 
by  means  of  the  pestle  with  a  few  cubic  centimeters  of  the  ethereo- 
ammoniacal  mixture  to  make  a  fine  paste,  taking  care  not  to  smear 
the  sides  of  the  jar  unnecessarily,  then  add  about  2  c.c.  more  of  the 
same  mixture,  so  as  to  have  the  opium  well  covered  with  liquid, 
screw  down  the  top,  leaving  the  pestle  inside,  and  set  the  jar  aside 
for  five  or  six  hours.  After  that  time  the  jar  is  opened,  about  10 
grammes  of  the  sodium  chloride  thoroughly  mixed  in  with  the 
opium,  and  the  open  jar  placed  in  a  good  current  of  air,  stirring  fre- 
quently with  the  pestle  in  order  to  prevent  formation  of  lumps.  In 
about  an  hour  the  powder  will  be  nearly  dry.  The  jar  is  then 
placed  in  a  vacuum  desiccator  containing,  besides  sulphuric  acid,  a 
vessel  of  paraffin,  and  left  there  over  night.  The  jar  is  then  taken 
out,  any  lumps  in  the  powder  carefully  crushed  with  the  pestle,  and 
the  mixture  transferred  first  to  the  glazed  paper,  and  then  to  the 
1  The  lower  part  of  a  burette  cut  in  two  answers  very  well. 
