Determination of nickel as the dimethylglyoxime complex

Tin(II) chloride solution. Dissolve lOg of tin(II) chloride dihydrate in 100mL of 1M hydrochloric acid. 

Potassium thiocyanate solution. Prepare a 10 per cent aqueous solution from the pure salt. 

Determine the concentration of Mo in unknown samples supplied and containing less than 50 fig Mo per 10 mL use the calibration curve, and subject the unknown to the same treatment as the standard solutions. 

The above procedure may be adapted to the determination of molybdenum in steel. Dissolve a 1.00 g sample of the steel (accurately weighed) in 5 mL of 1 1 hydrochloric acid and 15 mL of 70 per cent perchloric acid. Heat the solution until dense fumes are evolved and then for 6-7 minutes longer. Cool, add 20 mL of water, and warm to dissolve all salts. Dilute the resulting cooled solution to volume in a 1 L flask. Pipette 10.0 mL of the diluted solution into a 50 mL separatory funnel, add 3 mL of the tin(II) chloride solution, and continue as detailed above. Measure the absorbance of the extract at 465 rnn with a spectrophotometer, and compare this value with that obtained with known amounts of molybdenum. Use the calibration curve prepared with equal amounts of iron and varying quantities of molybdenum. If preferred, a mixture of 3-methylbutanol and carbon tetrachloride, which is heavier than water, can be used as extractant. 

Under the above conditions of determination the following elements interfere in the amount specified when the amount of Mo is 10 fig (error greater than 3 per cent) V, 0.4 mg, yellow colour [interference prevented by washing extract with tin(II) chloride solution] Cr(VI), 2 mg, purple colour W( VI), 0.15 mg, yellow colour Co, 12 mg, slight green colour Cu, 5 mg Pb, 10 mg Ti(III), 30 mg (in presence of sodium fluoride). 

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