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Conference Proceedings

The AusIMM Proceedings 1922

Conference Proceedings

The AusIMM Proceedings 1922

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Volumetric Determination of Iron: New Method of Reduction

THE reduction of iron from the ferric to the ferrous state prior to its titration by permanganate or dichromate may give erroneous results in the presence of other reducible metals such as titanium. Stannous chloride and metallic zinc both reduce tetravalent titanium to a lower form, and so increase the consumption of the oxidizing standard: solution. Sulphuretted hydrogen and sulphurous acid do not reduce titanium, but are slow in action and troublesome to manipulate.Sulphuretted hydrogen is considered to be the best reducing agent for iron in the presence of titanium.* In the method to be described the advantages of the H 2S reduction are retained without the disadvantages of using the gas. The reduction is carried out by the action of a metallic sulphide having a solubility product of such a value that the sulphide iom, are utilized as fast as they are formed, and but little free sulphuretted hydrogen is given off.Cadmium sulphide was the first to be tried, but its solubility product (3.6 x 10 - 2~)t was apparently too low. The reduction was satisfactory, but the excess was very difficult to remove. Zinc sulphide (S.P. = 1.2 x 10 - 23) was found to be quite satisfactoryin both respects. The zinc sulphide is preferably used in the form of an emulsion prepared from pure zinc sulphate as follows: About 100 grm. of ZnS047H20 is dissolved in 2 litres of water. H2S is passed until no further precipitate is obtained, the acid formed being barely neutralized from time to time by the addition of ammonia. The precipitation of the sulphide in a slightly acid solution gives a finer emulsion than that prepared in an alkaline solution, and any iron present remains dissolved. The precipitate is allowed to settle and the clear liquid decanted. The precipitate is then shaken up with more water, acidified with a little sulphuric acid, allowed to...
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  • Published: 1921
  • PDF Size: 0.068 Mb.
  • Unique ID: P_PROC1922_0276

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