^vS'^im'}     Alkaloids  and  Alkaloidal  Drugs.  519 
hours.  The  powder  is  then  put  into  a  filter-paper  cell,  placed  in 
a  Soxhlet  extraction  apparatus,  the  jar  rinsed  out  several  times 
with  powdered  glass,  or,  in  the  absence  of  this,  with  coarsely  pow- 
dered barium  nitrate,  the  rinsings  added  to  the  Soxhlet,  the  latter 
connected  with  an  Erlenmeyer  flask  containing  about  40  or  50  c.c. 
absolute  ether,  and  the  extraction  conducted  in  the  usual  way,  till 
a  few  drops  after  evaporation  of  the  ether  and  acidulation  give  no 
reaction  with  Mayer's  or  Wagner's  reagent.  The  ethereal  extract 
will  be  found  to  have  only  a  very  slight  yellow  color.  The  Erlen- 
meyer is  then  detached  from  the  Soxhlet,  the  ether  poured  out  into 
a  flat  evaporating  dish,  the  Erlenmeyer  washed  out  several  times 
with  water  containing  about  2  per  cent,  sulphuric  acid,  the  wash- 
ings added  to  the  contents  of  the  evaporating  dish,  and  the  latter 
put  into  a  draught  at  about  300  C,  till  the  ether  has  disappeared. 
The  contents  of  the  dish  are  poured  into  a  1 00  c.c.  flask,  the  dish 
washed,  the  washings  added  in  the  flask,  and  the  latter  filled  up  to 
the  100  c.c.  mark.  The  solution  containing  hydrastine  sulphate, 
and  of  which  10  c.c.  represent  1  gramme  of  the  root,  is  used  for 
the  estimation  of  hydrastine. 
For  the  iodometric  estimation  20  c.c.  of  the  filtered  solution 
(representing  2  grammes  of  the  drug)  are  run  from  a  burette  into 
a  IOD  c.c.  flask,  containing  20  or  30  c.c.  of  a  standardized  solution 
of  iodine  of  any  known  strength  (that  in  the  neighborhood  of  1 
per  cent,  is  the  best),  and  the  analysis  carried  out  exactly  as  de- 
scribed in  the  accompanying  paper  (Amer.  Jour.  Pharm.,  1899,  p. 
462).  From  the  amount  of  iodine  consumed  the  amount  of  hydras- 
tine is  deduced  by  using  the  factor  of  the  hydrastine  hexiodide,  i.  e.f 
0-60403  of  hydrastine  for  one  of  iodine  consumed. 
For  a  gravimetric  estimation  another  portion  of  20  c.c.  of  the 
filtered  solution  is  run  into  a  separator  and  the  hydrastine  shaken 
out  with  benzol  and  ammonia,  all  the  coloring  matter  remaining  in 
the  aqueous  fluid,  and  a  perfectly  colorless  solution  of  hydrastine 
in  benzol  is  obtained.  The  benzol  solution  is  then  filtered  through 
a  small  filter  into  another  separator,  the  first  separator  and  filter 
washed  with  benzol,  and  the  hydrastine  again  shaken  out  with 
water  acidulated  with  sulphuric  acid.  At  last,  from  the  watery 
solution,  the  hydrastine  is  shaken  out  with  ether  and  ammonia,  the 
ether  poured  into  a  tared  beaker  and  slowly  evaporated  in  a  dark 
place.    After  drying  in  a  vacuum  over  sulphuric  acid  and  paraffine, 
