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The Students' Guide in Quantitative Analysis - Free Ebooks Library

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QyWtllTlTATIVE ANALYSIS.<br />

^^f, I _Somc of tho till may go <strong>in</strong>to solution as<br />

litratc of titi, H' tli*-^ "'^^'^^ '^^'^^ '^"^ '^'^^''^^' ^"^^ ^'^"^ ^J^^''''^''<br />

<strong>in</strong> Precipitate c mixed witli tlie sulphide of antimony ; <strong>in</strong><br />

this case they should be separated by F. W. Clarke's<br />

method which is based on the solubility of the sulphide<br />

of t<strong>in</strong> <strong>in</strong> oxalic acid, and details of which may he found <strong>in</strong><br />

Crookcs' Sckcl Methods, page 249- I'O!- another method<br />

sec Fres., § 165. 4. «- ^l^o § £65, 7, a-<br />

On the other hand, some of the antimony<br />

Note ->. —<br />

and lead may refuse to dissolve and rema<strong>in</strong> with Residue a,<br />

<strong>in</strong> which case proceed as follows :<br />

after ignit<strong>in</strong>g and weigh-<br />

<strong>in</strong>g tlic SnO, + Pl> ? + Sb ? fnse with Na,C03 and sulphur<br />

<strong>in</strong> a porcela<strong>in</strong> crucible. Dissolve <strong>in</strong> warm water and filter<br />

from the residue of PbS, which may be treated with HNOj<br />

<strong>in</strong> a porcela<strong>in</strong> crucible and wci:j,hed as PbSO,. To the<br />

alkal<strong>in</strong>e solution add sliglit excess of HCl and collect<br />

precipitate of SbSj + SnS, + S on filter; dry and remove<br />

excess of S by wash<strong>in</strong>g with CS„ transfer to porcela<strong>in</strong><br />

capsule, oxidi/x with UNO, evaporate to dryness, fuse<br />

with NallO <strong>in</strong> a .silver dish, dissolve the mass <strong>in</strong> a mixture<br />

uf three volumes of alcohol and one of water, and filter<br />

from the antimoniatc of sodium. For details, see Fres.,<br />

§ 165, 4, a To the solution conta<strong>in</strong><strong>in</strong>g stannatc of sodium,<br />

add UCl, saturate with ILS, and treat the precipitated<br />

SnSj as usual. See Fres., § 126, I, c, and § 9E.<br />

Consult article on the Estimation of Antimony, by E.<br />

M. Bartlcy, <strong>in</strong> American Chemist, Vol. V, page 436; also<br />

paper by Dr. Clemens W<strong>in</strong>kler, <strong>in</strong> Fresenius' Zcitschrift<br />

fur Analj'tischc Ckemic, Heft 2, 1875.

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