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  Gooch 
  and 
  Danner 
  — 
  Method 
  for 
  the 
  

  

  Aet. 
  XXIX. 
  — 
  A 
  Method 
  for 
  the 
  Separation 
  of 
  Antimony 
  

   from 
  Arsenic 
  oy 
  the 
  Simultaneous 
  Action 
  of 
  Hydrochloric 
  

   and 
  Hydriodic 
  Acids; 
  by 
  F. 
  A. 
  Gooch 
  and 
  E. 
  W. 
  

   Dannee. 
  

  

  [Contributions 
  from 
  the 
  Kent 
  Chemical 
  Laboratory 
  of 
  Yale 
  College 
  — 
  IX.] 
  

  

  A 
  method 
  for 
  the 
  separation 
  of 
  arsenic 
  from 
  antimony- 
  

   based 
  npon 
  the 
  difference 
  in 
  volatility 
  of 
  the 
  lower 
  chlorides 
  

   was 
  introduced 
  originally 
  by 
  Fischer.* 
  This 
  method 
  of 
  treat- 
  

   ment 
  consisted 
  in 
  the 
  reduction 
  of 
  the 
  chlorides 
  by 
  means 
  of 
  

   ferrous 
  chloride 
  and 
  the 
  volatilization 
  of 
  the 
  arsenic 
  by 
  

   repeated 
  distillations 
  of 
  the 
  mixture 
  with 
  hydrochloric 
  acid 
  of 
  

   twenty 
  per 
  cent 
  strength 
  added 
  in 
  successive 
  portions. 
  The 
  

   process 
  has 
  been 
  subsequently 
  modified 
  by 
  Hufschmidtf 
  by 
  

   the 
  substitution 
  of 
  gaseous 
  hydrochloric 
  acid, 
  introduced 
  in 
  

   continuous 
  current 
  into 
  the 
  distilling 
  mixture, 
  for 
  the 
  aqueous 
  

   acid, 
  and 
  later 
  changed 
  further 
  and 
  improved 
  by 
  Classen 
  and 
  

   Ludwig,J 
  who 
  employ 
  ferrous 
  sulphate, 
  or 
  ammonio-ferrous 
  

   sulphate, 
  in 
  place 
  of 
  the 
  less 
  easily 
  prepared 
  ferrous 
  chloride. 
  

   In 
  its 
  latest 
  form 
  the 
  method 
  is 
  exceedingly 
  exact, 
  but 
  the 
  con- 
  

   ditions 
  are 
  such 
  that 
  the 
  antimony 
  in 
  the 
  residue 
  must 
  be 
  

   determined 
  gravimetrically. 
  It 
  has 
  been 
  our 
  endeavor 
  to 
  so 
  

   arrange 
  the 
  process 
  that 
  the 
  determination 
  of 
  the 
  antimony 
  

   may 
  be 
  made 
  by 
  a 
  rapid 
  volumetric 
  method, 
  and 
  this 
  we 
  have 
  

   attempted 
  to 
  accomplish 
  by 
  substituting 
  for 
  the 
  iron 
  salt, 
  

   which 
  utterly 
  precludes 
  the 
  direct 
  volumetric 
  estimation 
  of 
  the 
  

   antimony, 
  another 
  reducer 
  — 
  hydriodic 
  acid 
  — 
  rwhich 
  can 
  inter- 
  

   fere 
  in 
  no 
  way 
  with 
  the 
  subsequent 
  determination 
  of 
  the 
  

   antimony 
  by 
  the 
  well 
  known 
  iodometric 
  method. 
  

  

  It 
  has 
  been 
  shown 
  in 
  previous 
  work 
  in 
  this 
  laboratory 
  that 
  

   arsenic§and 
  antimony! 
  may 
  both 
  be 
  reduced 
  by 
  the 
  action 
  of 
  

   hydriodic 
  acid 
  applied 
  under 
  appropriate 
  conditions. 
  In 
  those 
  

   processes, 
  however, 
  it 
  was 
  essential 
  that 
  the 
  arsenic 
  should 
  not 
  

   volatilize, 
  and 
  the 
  conditions 
  were 
  adjusted 
  accordingly. 
  In 
  

   the 
  present 
  case 
  we 
  have 
  to 
  test 
  the 
  reducing 
  action 
  of 
  hydrio- 
  

   dic 
  acid 
  in 
  the 
  presence 
  of 
  strong 
  hydrochloric 
  acid 
  and 
  at 
  the 
  

   boiling 
  temperature 
  of 
  the 
  solution 
  — 
  conditions 
  arranged 
  to 
  

   bring 
  about 
  the 
  volatilization 
  of 
  the 
  arsenic 
  as 
  rapidly 
  as 
  pos- 
  

   sible. 
  Certain 
  preliminary 
  experiments 
  gave 
  indication 
  that 
  a 
  

   half 
  gram 
  of 
  arsenic 
  oxide 
  could 
  be 
  completely 
  volatilized 
  

   by 
  the 
  action 
  of 
  potassium 
  iodide 
  in 
  excess 
  in 
  the 
  manner 
  

   described, 
  and 
  that 
  an 
  equivalent 
  weight 
  of 
  antimonious 
  oxide 
  

  

  * 
  Ann. 
  Chem. 
  u. 
  Pharm. 
  208, 
  182. 
  f 
  Ber. 
  d. 
  deutsch. 
  chem. 
  Ges., 
  xvii, 
  2245. 
  

  

  \ 
  Ber. 
  d. 
  deutsch. 
  chem. 
  Ges. 
  xviii, 
  1110. 
  

  

  § 
  Gooch 
  and 
  Browning, 
  this 
  Journal, 
  vol. 
  xl, 
  p. 
  66. 
  

  

  || 
  Gooch 
  and 
  Gruoner, 
  this 
  Journal, 
  vol. 
  xlii, 
  p. 
  213. 
  

  

  