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The Students' Guide in Quantitative Analysis - Free Ebooks Library

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gg QUANTITAXrVE ANALYSIS,<br />

hot cone. H,SO,, pour <strong>in</strong>to cold water, and collect the pre<br />

cipitate as before.<br />

Naie 9. Separation of SiO,.—Evaporate as <strong>in</strong> Note 5.<br />

<strong>The</strong>n add HCI quite freely and warm for some time before<br />

add<strong>in</strong>g any water, as the high heat may have produced<br />

anhydrous Fe.Oj, form<strong>in</strong>g an oxychloride which is very<br />

slow to dissolve, especially <strong>in</strong> dilute acid. Should the acid<br />

already added be too dilute, concentrate by evaporation,<br />

add cone. HCI, and digest at a moderate heat.<br />

Note II. pRECtP[TATEON OF THE BASIC ACETATES.—^^iV-<br />

//-(T/^/ comb<strong>in</strong>ed with Solutions li and cV must be very<br />

carefully neutralized with sodium carbonate. (If ammonium<br />

carbonate were used, bromide of nitrogen might form <strong>in</strong><br />

Filtrate g.) To neutralize the greater portion of the acid<br />

use crystallized sodium carbonate, and complete the neu-<br />

tralization with a very dilute solution of the carbonate, add-<br />

<strong>in</strong>g it drop by drop, agitat<strong>in</strong>g to dissolve the precipitate,<br />

until the liquid assumes a deep mahogany-red color. If a<br />

permanent precipitate forms, add a little hydrochloric acid,<br />

and repeat as above. <strong>The</strong>n dilute the solution to about i<br />

litre for each gramme of the sesquioxide present, add about<br />

20 grammes sodium acetate dissolved <strong>in</strong> a small quantity of<br />

water, and heat the whole to boil<strong>in</strong>g.<br />

It is sufficient to boil from ten to fifteen m<strong>in</strong>utes for the<br />

complete precipitation of the acetates. <strong>The</strong> fdtcr<strong>in</strong>g should<br />

be done rapidly on a ribbed filter, keep<strong>in</strong>g the fluid hot. and<br />

disturb<strong>in</strong>g the settled precipitate as little as possible.<br />

When available the Bunsen pump may here be used with<br />

advantage. After the supernatant fluid has been poured<br />

through the filter, throw on the precipitate and wash it with<br />

boil<strong>in</strong>g water conta<strong>in</strong><strong>in</strong>g a little sodium acetate. Should<br />

any basic acetate separate upon concentrat<strong>in</strong>g the filtrate,<br />

add some sodium acetate, boil, filter, dissolve the prccip<br />

itate <strong>in</strong> HCI, and unite to the solution of the ma<strong>in</strong> body.

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