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 •'"1 \„: 
 
 PAPERS 
 
 PROM TUB 
 
 CHEMICAL Laboratory. 
 
 No. 22.-Solubility of the Sulphides of Arsenic, 
 
 Antimony and Tin. 
 
 BY 
 
 W. R. LANG and C M. CARSON. 
 
 Reprinted from the >oamal of the Society of Chemical InduHtn. 
 
 Aucnst 1?, 1902. 
 
 TORONTO, lfK)2. 
 
 ^^mm 
 
 mw- 
 
 H!^|m 
 
1^7% '^"yt J :j<^) 
 
 BEPRINTED FROM THE JOURNAL 
 
 of TBB 
 
 SocictY of Cticmical ^nbu^try, 
 
 15 AUGUST 1902. 
 
 mUBILin OF THE SULPHIDES OF ARSENIC, 
 ANTIMONY, AND TIN. 
 
 hZ 
 
 W. E. LANG AHD C. M. CARBON. 
 
 ♦-^sl 
 
 I ^'J 
 
 LONDON: 
 EYBK AMD SrOTTIBWOODB, KABT UAKOIMO 8TBKKT, B.C. 
 . 180S. 
 

 jVSM 
 
[^Ri'priHteil from the Joitrua} of Ike Suriefp of Chfmicnl 
 rndmtry, 15 iiiguit WYi. Ko. 13, Vol. XXI.} 
 
 SOLUBILITY OF THE SULPHIDES OF AKSKNIC. 
 ANTIMONY, AND TIN. 
 
 BT W. R. LANS AND C. X. CARMON, 
 
 In a former paper (thia Jonmal, Jane 16. 19«)2, T^H), an 
 account was giren of a nhort investigution into the aoeuracy 
 of the method! reoonimen<led for the deparation of the 
 Bulphidea of arsenic, antimony, and tin. The following are 
 the reRults of further ex[>criment8 with reference to the 
 ■olnbility of the three aulphid s in hydrochloric acid : — 
 
 I. Arsenic Sulphide in Hydrochloric Acid. — Onepramme 
 of arsenioui oxide WHH dissolved in hydrochloric acid, iind 
 the solution made up to 250 c.c. Into each of several tlasks 
 25 c.c. of the solution were measured, the arsenic precipitated 
 as the sulphide, and filtered. 
 
 (a) The precipitates were treated with equal volumes of 
 hydrochloric acid of different concentrations and allowed to 
 stand, at the room tempf rature, for four hours, when they 
 were again filtered, the filtrates diluted with water, and 
 tested by passing in hydrogen i>?lphidc. 
 
 Hydrochloric Acid 
 
 Water. 
 
 Filtrate after passsKe of 
 
 (Sp. Gr., 1 
 
 16). 
 
 lI>iirojren Sulpiiide. 
 
 c.c. 
 
 
 c.c. 
 
 
 « 
 
 
 
 
 Slightly coloured. 
 
 SO 
 
 
 l(t 
 
 .* *t 
 
 40 
 
 
 20 
 
 
 M 
 
 
 .HO 
 
 ColourlHsMi. 
 
 W 
 
 
 40 
 
 ,, 
 
 10 
 
 
 «> 
 
 „ 
 
 
 
 
 60 
 
 M 
 
 (fe) The sulphides were treated with hydrochloric acid 
 a» 'u (a), but, before Litering, hydrogen sulpiiide was passed 
 p 3145.— 0. 
 
 ■■1' 
 
iKrniNTKn fwow the journal or 
 
 into cmh. Th«s filtrntes were tettei an before with h)«lroj{eu 
 »ulphide 
 
 Il.vdnMhI-iric A<-ul. Wntcr. 
 
 Filtmtt' lifter pHNsnjti' of 
 li.vilniiri'ii Siil|iliiilo. 
 
 fjn. 
 
 c.c. 
 
 m 
 
 
 
 ¥t 
 
 so 
 
 m 
 
 rm 
 
 ta 
 
 41) 
 
 e 
 
 ti'j 
 
 Kho«eii no (■(iloiirtition. 
 
 (c) Ihe sulphide* were obtained at in (a), and were 
 afStiiD treated with hjdrochloric acid, but, instead of being 
 allowed to stand at the room temperature, were boiled for 
 15 minutes. -The roiaturea were then fll'ercd, and the 
 filtratt ■ tested. 
 
 Filtrate with Hydrogcu 
 8ulphid«. 
 
 Sulphide had almost com- 
 pletely din^^«lv»xl. 
 
 Filtrate gave precipitate with 
 hydrogen 8ul|)hide. 
 
 (rf) The procf dure was the ssire as in (c), cxctpt that, 
 before filterinjj, the niixtnie was cooled and then ta^urattd 
 with hjdrogen sulphide. 
 
 Hydroolilorio Acid. 
 
 c.c. 
 
 CO. 
 
 At 
 
 
 
 4'» 
 
 £0 
 
 3U 
 
 3tt 
 
 5!0 
 
 4ii 
 
 
 
 m 
 
 Vat«r. 
 
 Filtrate »hen tested with 
 Hydrogen Sulphide. 
 
 No colouration. 
 
TUE 80C1KTY Or CUEMICAL ISDt'STRT. 
 
 3 
 
 Ar»ieiu()U«iulpl.ideiii»y,t>t,Mi. betrt-atfd with hjdroclilorie 
 ttria (np. Rr , 1 • Jfi) witlo' .bnger of ^olutlOD. if hy.lrt.neii 
 MtlphHle be |)B^e<l iuto the mixture H> Haturation. 
 
 II. The Svluhilil!/ >/ Antimowtf Trisulphide in Hudro- 
 rUvrir Acid.-A mAuXwu wu- uiutle coi.tuining 1 giTii. 
 of nntiir.oity t.troxide in -^M c.c. ; 25 c.c. of the .olut.on 
 w(r<! ni"ju>ur.'d out, the antimony precipitiitei an tne 
 .alphide, ard iho preclpitatp filtertd. The sulph.de wbk 
 then washed into a flatk by means of 8 c.o. of com-ei.trated 
 hjdroch''>Tic acid (-p. gr 1 • 16) being completely d.*»olvcd. 
 but ttiv) V' an oranjje wration lo the i-olation. On 
 addition c. another 2 c.c. aid the « lo-ralion dieappeared. 
 The i.alph=de oi av-tlmony was again obtained by precipi- 
 tation of a.'ic.c .t the original solution. Thia wan hittred 
 and •'••«»oKed i r.C c.c. of concentrated hydrochloric and. 
 Into 1 . solatloj hydrogen «ulphide wm passed con- 
 tinuo-;iy. whilst water was added from a burette. ^^ hen 
 18 c.c. of water had been added, a slight colouration was 
 visible, and when the amount of water had reached 21 c.c, 
 the f ulphide began to precipitate. To again obtoin a clear 
 Bolution, 8 c.c. of hydrochloric acid were nqmred. 
 
 The sulphide of antimony is soluble, then, in a mixture 
 of hydrochoric acid (Kp. gr., 1-16) and water in the pro- 
 portion of 50 to 1«, even when hydrogen sulphide w passed 
 in to complete saturation. 
 
 IIT Stannoua Sulphide is »oluMo in hydroehlcric aiid 
 slightly more dilute than that which is required to dissolve 
 antimony trisr -,>hide. 
 
 In order to separate the sulphide* of arsenic from tho-e 
 of antimony and tin, the mixture shouki be treated with 
 hydrochloric acid diluted with not more than one-third uf 
 its volume of water, and then couioletely saturated with 
 hvdrocen sulphde. The arsenious sulphide will be un- 
 dissolved, and on filtering, will be loft free from antimony 
 and tin. The precipitite may be washed with a ni.xt.ire ot 
 h^diochloricacid and water in the proportion of .H) to 18. 
 or with hydrochloric aeid (sp. gr., 1 -16). if hydrogen sulphide 
 be passed into the acid before washing. 
 
 This metho.:, which is substantially the same as mat 
 given by rattin^^n atd Pattinson (this Journal, 1898, 211. 
 •'14), was employed to estimate the arsenic in 25 c.c. of 
 a soution containing*! grm. of aiseuuus oxidf, 1 gim. 
 
4 THE SOCIETY Of CHEMICAL INDU8TBY. 
 
 Of antimony tetroxide. and 1 grm. of tin oxide in 250 c.c 
 The sulphide of arseuic, after separation, was dissolved in 
 nitric acid, the anenic precipitated by magnesia mixture, 
 and weighed as magnesium pyro-arsemate :— 
 
 In qualitative work, the solution of the sulphides in yellow 
 ammonium iulphide may first be precipitated by dilute 
 hydrochloric acid. The mixture of sulphides, on being 
 filtered and washed, may then be separated as described 
 alwve. This is preferable to the method of pouring the 
 solution into concentrated hydrochlorie acid. 
 
 ►••-<- 
 
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