Graduate Thesis Or Dissertation
 

Determination of magnesium in zirconium based on ion exchange separation and titration with versene

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  • The Kroll Process for the production of zirconium utilizes the reduction of zirconium tetrachloride with metallic magnesium. Control of the magnesium content of the final zirconium metal is essential, as residual magnesium adversely influences the properties of zirconium. In this thesis a volumetric method has been presented for the determination of magnesium. An initial separation of the bulk of zirconium from magnesium was carried out by a rapid, batch ion exchange in hydrofluoric-hydrochloric acid solution. In this step 94% of the zirconium can be removed. The remainder was precipitated with ammonia in the presence of ammonium chloride. Magnesium is determined in the filtrate by the complexometric titration with disodium ethylenediamine tetraacetate. This method was applied to magnesium-zirconium mixtures containing from 1% to 0.1% magnesium. The lower level of 0.1% was established because the volume of versenate used in titration becomes too small for accurate determinations at concentrations lower than this.
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