Analytical applications of condensed phosphoric acid-II: determination of aluminium, iron and titanium in bauxites after decomposition with condensed phosphoric acid.
Bauxites can be decomposed by condensed phosphoric acid (CPA) very rapidly without the need for subsequent manipulations such as elimination of silica, digestion of fused products and filtration. It is best to heat the samples at about 700 degrees prior to the decomposition, to prevent them from floating on the surface of the CPA. Under the proposed conditions (100 mg of sample, 10 g of CPA, heating at 300 degrees for 30 min), aluminium, iron and titanium are dissolved quantitatively. Iron is determined by photometry with 1,10-phenanthroline after solvent extraction with MIBK, while titanium is determined with N-benzoyl-N-phenylhydroxylamine (BPHA). The effect of phosphate on the determination of titanium is reduced to a minimum at a BPHA concentration of 0.3% and a hydrochloric acid concentration of 7.2M. Aluminium and iron are precipitated quantitatively as the oxinates at pH 5.5 in the presence of orthophosphoric acid or hydrolysed CPA, while the precipitation of titanium oxinate is completely suppressed by the addition of hydrogen peroxide. The total amount of aluminium and iron is obtained by determining the amount of oxine by bromination method. The amount of aluminium is obtained by subtracting the amount of iron from the sum of the two.
Mizoguchi
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Chemical Research Institute of Non-Aqueous Solutions, Tohoku University, Katahira, Sendai-shi, Japan.
Ishii
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