Determination of Ca and Mg in Limestone

Reagents required: KOH 5% solution, Buffer 10 for Mg, 0.01 M EDTA, Murexide Indicator, Solochrome Black

Spl prep: 1. Weigh 0.5 g of sample (Wt sample, W) 2. Add 10 ml of HCl (1+1) 3. Evaporate to dryness on a hotplate 4. Cool. Dissolve residue with 25 ml HCl (1+9), dilute to about 100ml and digest at low heat for 15 mins. 5. Cool and make up to 250 ml in a volumetric flask. Let it settle or filter. 6. Suck up 25 ml aliquots for titrations.

CaO determination: 1. Add 4-5 ml of KOH 5%. Must be alkaline for color change, around 10-11 pH 2. Use Murexide as indicator. 3. Titrate against 0.01 EDTA. End point is purple.

Calc: Avg Volume used, A ml. Wt Ca in spl, C= A x 0.4008 x 250/25 % Ca in spl= C/W x 100% % CaO in spl= %Ca x 56.08/40.08 % CaCO3 in spl= %Ca x 100.09/40.08

MgO determination: 1. Add 30 ml Buffer 10. 2. Use Solochrome black as indicator. 3. Titrate against 0.01 EDTA. End point is dark blue.

Calc: Avg Volume used, B ml. Wt Mg in spl, D= B x 0.2431 x 250/25 % Mg in spl= D/W x 100% % MgO in spl= %Mg x 40.32/24.32 % MgCO3 in spl= %Mg x 84.32/24.32

Note: CaCO3 +MgCO3 = around 99%