Determination of calcium substitution titration

Discussion. When calcium ions are titrated with EDTA a relatively stable calcium complex is formed  

With calcium ions alone, no sharp end point can be obtained with solochrome black indicator and the transition from red to pure blue is not observed. With magnesium ions, a somewhat less stable complex is formed  

Traces of many metals interfere in the determination of calcium and magnesium using solochrome black indicator, e.g. Co, Ni, Cu, Zn, Hg, and Mn. Their interference can be overcome by the addition of a little hydroxylammonium chloride (which reduces some of the metals to their lower oxidation states), or also of sodium cyanide or potassium cyanide which form very stable cyanide complexes ( masking ). Iron may be rendered harmless by the addition of a little sodium sulphide. 

The titration with EDTA, using solochrome black as indicator, will yield the calcium content of the sample (if no magnesium is present) or the total calcium and magnesium content if both metals are present. To determine the individual elements, calcium may be evaluated by titration using a suitable indicator, e.g., Patton and Reeder s indicator or calcon — see Sections 10.48 and 10.60, or by titration with EGTA using zincon as indicator — see Section 10.61. The difference between the two titrations is a measure of the magnesium content. 

Procedure. Prepare an ammonia-ammonium chloride buffer solution (pH 10), by adding 142 mL concentrated ammonia solution (sp. gr. 0.88-0.90) to 17.5 g ammonium chloride and diluting to 250 mL with de-ionised water. 

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