Improvements in the accuracy and precision of isotope ratio measurements by double focussing inductively coupled plasma mass spectrometry
thesisposted on 12.12.2013 by Christopher P. Ingle
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Inductively coupled plasma mass spectrometry is a well-established technique for the measurement of isotope ratios. Double focussing mass analysers enable increased resolution to be applied to separate spectroscopic interferences, or the use of multi-collector detection techniques for high precision isotope ratio determinations. For the Central Science Laboratory (CSL), trace elements team, methods were developed for Zn and Fe isotope ratio measurements in acid digested faecal samples from a human nutritional study. For Zn, a novel high resolutionlmulticollector combination was employed; for Fe a single collector, high resolution method was used. In both cases, samples from the nutritional study known to contain the analytes in natural isotopic abundance were used to correct for the mass bias. Two independent methods for determining Zn and Fe isotope ratios were used to validate the measurement strategies. The team at CSL are also involved in the authentication of food products. Isotope ratio and elemental concentration data were used to determine the geographical origin of rice samples, and to distinguish between traditional and modem Basmati rice grown in India and Pakistan. NERC Isotope Geosciences Laboratory are primarily concerned with the achievable accuracy and precision of an isotope ratio measurement. Use of a mass bias correction expression appropriate to the ICP-MS instrument is essential for high quality isotope ratio measurements. Cd and Sn were used to study the variation of the mass bias in a double focussing ICP-MS system with time, absolute mass and mass difference. It was proposed that mass bias should be considered as a result of the change in the instrument response with mass, and not a fundamental parameter in its own right. A method for determination of the best mass bias correction model for an individual instrument, through examination of the instrument response function was developed.