110 
NEW  PROCESS  FOR  VALERIANATE  OF  AMMONIA. 
water  to  prevent  perfect  crystallization)  should  be  poured  into 
a  cylindrical  jar,  and  treated  with  a  small  portion  of  oil  of  vitriol, 
and  agitated  by  inserting  a  tube  through  the  acid  and  blowing 
with  the  mouth;  the  passage  and  regurgitation  of  the  air  bubbles 
mixes  the  whole  thoroughly ;  allow  the  mixture  to  stand  a  few 
minutes ;  the  oil  of  vitriol  seizes  the  water  and  subsides  with  it. 
Now  test  with  a  hydrometer  the  supernatant  acid,  and  should 
it  mark  a  sp.  gr.  of  -950,  this  part  of  the  process  is  complete; 
if  above  this,  add  a  second  portion  of  oil  of  vitriol,  which  should 
bring  it  to  this  degree  of  strength.  The  acid,  after  thorough 
subsidence  may  now  be  drawn  olf  by  either  of  the  processes 
above  indicated.  As  thus  prepared  it  is  somewhat  colored,  con- 
tains a  small  portion  of  sulphuric  acid,  and  also  a  portion  of 
water.  From  these  impurities  it  is  freed  by  distillation  from  a 
glass  retort.  In  this  process  there  are  a  few  points  to  be  at- 
tended to  upon  which  perfect  success  must  depend.  The  dis- 
tillate should  be  received  into  a  hydrometer  jar,  and  each  por- 
tion tested  with  a  hydrometer.  The  first  portion  that  comes 
over  contains  considerable  water,  and  must  be  rejected  and  laid 
aside  for  further  manipulation  ;  when  the  distillate  marks  «940 
it  may  be  retained.  The  distillation  is  now  proceeded  with, 
producing  a  portion  of  acid  of  -930,  until  white  vapors  appear 
in  the  retort,  when  the  gas  flame  is  immediately  withdrawn.  The 
portion  coming  over  first  should  be  treated  with  oil  of  vitriol, 
the  water  abstracted  and  added  to  the  retort,  and  the  operation 
finished  with  care.  The  mixed  distillates  indicate  a  sp.  gr.  of 
about  «933,  perfectly  clear,  colorless,  and  of  high  refractive 
power.  When  thrown  into  water,  it  rises  immediately  to  the  sur- 
face, floating  like  an  oil,  burns  with  a  blue  flame,  and  acts  with 
much  energy  upon  the  tongue  and  lips,  producing  a  white  spot  and 
destroying  the  cuticle.  The  next  stage  of  the  process  is  far 
more  simple  and  easy  of  execution,  and  consists  in  the  satura- 
tion of  the  acid  with  dry  gaseous  ammonia,  prepared  by  heating, 
in  a  suitable  vessel,  hydrate  of  lime  and  muriate  of  ammonia,  in 
proper  proportions,  and  passing  the  gas  through  a  bottle  contain- 
ing fragments  of  quick  lime.  Ammonia  is  passed  in  until  litmus 
paper  is  not  acted  on.  No  attention  is  paid  to  keeping  the  acid 
cool.  The  temperature  rises  to  about  150°,  keeping  the  liquid 
thin,  and  thus  preventing  the  stoppage  of  the  tube  with  crystals. 
