Determination of isotope ratios of chromium nickel, zinc and copper by gas chromatography-mass spectrometry by using volatile metal chelates

Abstract

A gas chromatographic-mass spectrometric (GC-MS) method involving thermally stable, volatile chelates was investigated for measurements of isotope ratios of chromium, nickel, zinc and copper. The chelating agents acetylacetone, trifluoroacetylacetone, sodium diethyldithiocarbamate and lithium bis (trifluoroethyl)dithiocarbamate [Li(FDEDTC])] were used. Experimental conditions for the preparation of chelates and the mass spectrometric operating parameters for precise and accurate measurement of isotope ratios were optimized using a general-purpose mass spectrometer. Imprecision values of 1–4% were obtained for measurements of different isotope ratios using chelates containing about 10 ng of metal. The capability of this technique for the accurate determination of natural and altered isotope ratios was also evaluated for these elements using Li(FDEDTC) as a chelating agent. This GC-MS method obviates the need for a more specialized mass spectrometer such as a thermal ionization or inductively coupled plasma mass spectrometer for trace metal determination. The technique gives detection limits down to parts per 109 levels and offers considerable potential for isotope dilution measurements.