Potentiometric microdetermination of cadmium in organic compounds after oxygen flask combustion

The sample is burnt in an oxygen flask and the combustion products are absorbed in lM HNO₃. After removal of interfering gases by boiling, the solution is transferred to the titration cell and neutralized with NaOH in the presence of methyl red; Cd(II) is finally titrated potentiometrically in a buffered 50% ethanolic medium with 0.01M sodium diethyldithiocarbamate in 50% ethanol. A silver/sulphide ion-selective electrode and a double junction reference electrode containing a 10% KNO₃ solution in 26% ethanol in the outer compartment are used in combination with a Titroprocessor to detect the end point. The results obtained are very accurate and reproducible: the maximum error does not exceed 0.09%, the recovery of cadmium is in the range 99.67 to 99.95% and the rel. standard deviation is 0.05%. The potentiometric titration with diethyldithiocarbamate, which is useful to determine small Cd(II) amounts down to 30g (2g ml^–1), as well as the oxygen flask combustion of organic cadmium compounds are discussed.