358 
Spirit  of  Nitrous  Ether. 
j  Am.  Jour.  Pharm. 
I      July,  1877. 
drop,  and  the  reaction  had  ceased,  temp.  1800  F.  ;  the  retort  was  now- 
allowed  to  cool.     Yield  of  distillate,  6f  fluidounces. 
Second  Heating.  Added  the  reserved  portion  of  nitric  acid  at  12.35 
P.M.,  temp.  900  F.  ;  commenced  to  simmer  at  1400  F.  ;  at  12.57  t^le 
temp,  was  1700  F.  ;  at  1.25  the  distillation  was  ended.  Yield  of  dis- 
tillate, 2  fluidounces. 
Into  the  absorbing  bottle  6  fluidounces  of  alcohol  had  been  placed. 
After  the  conclusion  of  the  process  this  measured  fluidounces,  show- 
ing an  additional  yield  of  |  fluidounce,  and  making  a  total  yield  of  9J 
fluidounces  of  distillate. 
The  reaction  proceeded  with  the  utmost  regularity,  and  the  end  was 
characterized  by  the  sudden  disappearance  of  the  abundant  frothy 
ebullition,  followed  by  gentle  simmering  for  a  short  time.  Upon  dilut- 
ing the  distillate  with  the  reserved  quantity  of  stronger  alcohol,  a  spirit 
was  obtained  which,  like  the  first,  correspond  with  the  officinal  require- 
ments in  every  resptct,  except  in  its  sp.  gr.,  which  was  0-8225  at  6o°F. 
Second  Experimental  Distillation. — It  was  observed  in  the  previous  opera- 
tions that,  after  the  reaction  ceased,  if  the  temperature  was  maintained 
at  i8o°F.,  distillation  would  proceed  drop  by  drop.  It  was  therefore  re- 
solved in  this  experiment  to  continue  the  heating  until  the  pharmacopoeial 
quantities  of  distillate  had  been  obtained.  It  had  also  been  suggested 
to  me  that  if  more  sulphuric  acid  was  added  after  the  reaction,  an 
additional  quantity  of  distillate  might  be  readily  obtained.  For  this 
reason  an  ounce  of  sulphuric  acid  was  added  after  the  first  heating  with 
the  result  below  indicated.  As  in  the  previous  operation,  the  acids 
were  somewhat  weaker  than  officinal  in  this  instance,  and  correspond- 
ingly larger  quantities  were  used.  The  nitric  acid  had  a  sp.  gr.  of 
1*372  (=64*5  per  cent.,  HON05) ;  the  sulphuric  acid  was  of  sp.  gr. 
1*838  (=95  per  cent.,  HOSOs)  ;  the  alcohol  was  of  sp.  gr.  0  817,  and 
neutral  ;  the  copper  was  in  thin  sheets.  With  a  view  of  obtaining 
absolutely  true  measures,  the  volume  of  alcohol  necessary  was  obtained 
by  measures  of  weight  instead  of  measures  of  capacity,  the  fluidounce 
being  taken  at  372*216  grains,  that  of  water  weighing  455*669  (Pile's 
average,  "U.  S.  Dispensatory,"  13th  edit.,  1735).  The  mixture  of 
sulphuric  acid  and  alcohol  was  made  in  the  evening,  and  the  distillation 
commenced  next  morning,  the  temperature  of  the  room  ranging  between 
6o°  and  65°F.,  that  of  the  condensing  water  being  56°F. 
