Am.  Jour.  Pharm. 
Feb.,  1891. 
Bromoform. 
83 
it,  on  separation,  is  considerably  darkened  and  resinified.  Tried  on  an 
experimental  scale  neither  the  yield  nor  product  were  satisfactory, 
and  hence  this  process  was  abandoned. 
The  following  modification  of  Dumas  process  was  adopted,  the 
quantities  given  being  those  found  convenient  for  experimental 
purposes. 
Four  ounces  of  marble  lime  were  slaked  and  then  mixed  with  one 
quart  of  water,  and  the  milk  of  lime  thus  made  transferred  to  a  flask 
connected  with  an  inverted  condenser.  A  funnel  tube  is  passed 
through  the  cork  and  reaches  below  the  surface  of  the  liquid.  In 
order  to  obtain  mechanical  agitation  so  as  to  keep  the  lime  dispersed 
through  the  liquid,  a  small  glass  tube  was  run  to  near  the  bottom  of 
the  flask,  and  extending  through  the  cork  was  attached  to  a  rubber 
atomizer  bulb.  By  pressing  this  bulb  sufficient  air  was  forced  into  the 
mixture  to  keep  it  thoroughly  agitated,  thus  supplying  the  place  of 
the  mechanical  agitator  of  the  manufacturer.  Four  ounces  of  acetone 
was  added  in  portions,  one-half  being  added  at  once  and  the 
remainder  gradually  during  the  operation.  The  contents  of  the 
flask  are  maintained  at  a  temperature  of  45 °  to  500  C,  slightly 
below  that  of  the  boiling  point  of  acetone,  and  bromine  is  gradually 
added  in  small  quantities  through  the  funnel  tube,  the  mixture  being 
thoroughly  agitated  as  each  portion  is  added.  When  the  reaction 
is  completed  and  the  further  addition  of  bromine  yields  a  yellow 
color,  a  sufficient  quantity  of  milk  of  lime  is  added  to  render  the  solution 
decidedly  alkaline  and*  distilled  at  once.  The  bromoform,  although 
boiling  at  a  much  higher  temperature  than  water,  comes  over  in 
the  first  portion  of  the  distillate.  The  aqueous  portion  of  the  distil- 
late usually  contains  considerable  acetone,  and  may  be  returned  to 
the  flask  and  used  in  a  subsequent  operation. 
The  bromoform  obtained  was  repeatedly  washed  with  water,  sepa- 
rated and  treated  with  calcium  chloride  and  then  distilled.  I  was 
surprised  on  attempting  to  fractionate  the  liquid  to  find  that  a  por- 
tion of  the  distillate  was  obtained  below  100°  C,  a  fraction  being 
collected  between  900  and  100°  C.  On  agitating  5  cc.  of  this  fraction 
with  20  cc.  water  in  a  stoppered  graduated  cylinder,  but  I  cc.  separated, 
the  remainder  being  dissolved.  The  aqueous  portion  separated,  pos- 
sessed the  odor  of  acetone,  and  yielded  iodoform,  with  iodine  and 
potassium  iodide  in  an  alkaline  solution.  The  heavy  oily  liquid  pos- 
sessed the  odor  and  taste  of  bromoform,  but  the  small  amount 
