Department of Chemistry, M. L. C. Govt. Girls P. G. College, Khandwa-450 001, India E-mail : sandhyagandhe@rediffmail.com Department of Chemistry, Government Holkar Science Autonomous College, Indore-452 017, India Manuscript received 28 March 2003, revised 14 November 2003. accepted 18 February 2004 Trace amount of CdII and NiII have been estimated quantitatively with 4-p-tolyl thiosemicarhazide (4-PTTSC) using amperometric titration technique. The titrations have been performed at pH 6.0 ± 0.02, 1.1 = 0.1 M at RT. The ratio of metal/4-PTTSC Is found to be 1 : 2 with L shaped curve. Reverse L shaped curve may be obtained on interchanging the position of' 4-PTTSC and metal ion.