670   Monobromated  Camphor  in  Migraine  Tablets.  { AtQ JX'r  ^TcT 
In  further  explanation  of  these  results,  it  may  be  stated  that 
Expts.  1  to  10,  inclusive,  have  to  do  primarily  with  the  camphor 
derivative  alone,  13  and  14,  16  and  17,  and  19  and  20  with  com- 
mercial mixtures,  while  11  and  12,  15,  18,  and  21  deal  essentially 
with  controls  of  the  latter,  in  which  the  dominating  ingredients  were 
proportioned  to  agree  with  the  manufacturer's  label.  Accordingly, 
any  uncertainty  existing  relative  to  the  quantities  of  such  ingre- 
dients, notably  monobromated  camphor,  actually  introduced  or  pres- 
ent in  the  samples  examined,  would  necessarily  be  reflected  in  all 
computations  based  thereon — as  in  the  calculation  of  percentages — 
and  is  so  indicated.  With  the  exception  of  Expts.  3  and  4,  the 
period  of  reduction  in  all  the  experiments  was  uniform,  consisting 
of  a  Yz  hr.  treatment  under  reflux  on  the  wire  gauze  and  1  hr.  on 
the  steam  bath.  In  the  exceptions  noted,  the  reflux  period  was 
doubled,  thus  making  the  entire  digestion  cover  a  2  instead  of  V/2 
hrs.  While  no  material  advantage  in  the  longer  treatment  is  ob- 
servable there  can  be  no  objection  thereto.  A  brief  survey  of  the 
results  presented  will  suffice  to  show  the  efficacy  of  the  method. 
Method. 
Ascertain  the  weight  of  20  or  more  tablets,  reduce  to  a  fine 
powder  and  keep  in  a  small  tube  or  specimen  bottle  provided  with  a 
tightly  fitting  cork  or  glass  stopper.  On  a  metal  or  glass  scoop  weigh 
out  an  amount  of  the  sample  equivalent  to  not  less  than  100  or 
more  than  200  Mg.  of  the  camphor  derivative  alleged  to  be  present. 
Transfer  quantitatively  with  20  Cc.  of  96  per  cent,  alcohol  and  10 
Cc.  of  water,  to  a  small  (100  Cc.)  round-bottomed  flask,  containing 
15  G.  of  1  per  cent,  sodium  amalgam.  Connect  the  flask,  by  means 
of  a  rubber  stopper,  with  a  short  vertical  reflux,  preferably  of  the 
Allihn  or  of  the  worm  type.  Heat  the  mixture  over  a  wire  gauze 
just  enough  to  cause  the  liquid  to  boil  gently  for  a  period  of  not 
less  than  30  Min.  After  cooling  slightly,  wash  out  the  condenser 
tube  first  with  5  Cc.  of  alcohol,  then  with  5  Cc.  of  water,  receiving 
the  washings  in  the  flask  below.  Remove  the  flask  to  the  steam 
bath,  heating  for  another  hour,  or  until  the  evolution  of  hydrogen 
has  nearly  or  quite  ceased.  Toward  the  latter  part  of  this  operation, 
render  the  liquid  about  neutral  with  a  few  drops  of  acetic  acid  in 
order  to  further  reduction.  Transfer  the  contents  of  the  flask  to  a 
separatory  funnel,  preferably  of  the  Squibb  type,  withdrawing  and 
