An Introductory Course of Quantitative Chemical Analysis eBook

This eBook from the Gutenberg Project consists of approximately 188 pages of information about An Introductory Course of Quantitative Chemical Analysis.

[Note 3:  The gravimetric determination of aluminium or chromium is comparable with that of iron just described, with the additional precaution that the solution must be boiled until it contains but a very slight excess of ammonia, since the hydroxides of aluminium and chromium are more soluble than ferric hydroxide.

The most important properties of these hydroxides, from a quantitative standpoint, other than those mentioned, are the following:  All are precipitable by the hydroxides of sodium and potassium, but always inclose some of the precipitant, and should be reprecipitated with ammonium hydroxide before ignition to oxides.  Chromium and aluminium hydroxides dissolve in an excess of the caustic alkalies and form anions, probably of the formula AlO_2^{-} and CrO_{2}^{-}.  Chromium hydroxide is reprecipitated from this solution on boiling.  When first precipitated the hydroxides are all readily soluble in acids, but aluminium hydroxide dissolves with considerable difficulty after standing or boiling for some time.  The precipitation of the hydroxides is promoted by the presence of ammonium chloride, but is partially or entirely prevented by the presence of tartaric or citric acids, glycerine, sugars, and some other forms of soluble organic matter.  The hydroxides yield on ignition an oxide suitable for weighing (Al_{2}O_{3}, Cr_{2}O_{3}, Fe_{2}O_{3}).]

DETERMINATION OF SULPHUR

Procedure.—­Add to the combined filtrates from the ferric hydroxide about 0.6 gram of anhydrous sodium carbonate; cover the beaker, and then add dilute hydrochloric acid (sp. gr. 1.12) in moderate excess and evaporate to dryness on the water bath.  Add 10 cc. of concentrated hydrochloric acid (sp. gr. 1.20) to the residue, and again evaporate to dryness on the bath.  Dissolve the residue in water, filter if not clear, transfer to a 700 cc. beaker, dilute to about 400 cc., and cautiously add hydrochloric acid until the solution shows a distinctly acid reaction (Note 1).  Heat the solution to boiling, and add !very slowly! and with constant stirring, 20 cc. in excess of the calculated amount of a hot barium chloride solution, containing about 20 grams BaCl_{2}.2H_{2}O per liter (Notes 2 and 3).  Continue the boiling for about two minutes, allow the precipitate to settle, and decant the liquid at the end of half an hour (Note 4).  Replace the beaker containing the original filtrate by a clean beaker, wash the precipitated sulphate by decantation with hot water, and subsequently upon the filter until it is freed from chlorides, testing the washings as described in the determination of iron.  The filter is then transferred to a platinum or porcelain crucible and ignited, as described above, until the weight is constant (Note 5).  From the weight of barium sulphate (BaSO_{4}) obtained, calculate the percentage of sulphur (S) in the sample.

[Note 1:  Barium sulphate is slightly soluble in hydrochloric acid, even dilute, probably as a result of the reduction in the degree of dissociation of sulphuric acid in the presence of the H^{+} ions of the hydrochloric acid, and possibly because of the formation of a complex anion made up of barium and chlorine; hence only the smallest excess should be added over the amount required to acidify the solution.]

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An Introductory Course of Quantitative Chemical Analysis from Project Gutenberg. Public domain.
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