Abstract :
The continuous flow elemental analyzer-isotopic ratio mass spectrometer (EA-IRMS) technique provides a significant improvement over conventional extraction methods for the determination of C- and S-isotope ratios in geological materials. It is faster and requires much smaller quantities of material for analysis. Sample preparation is simple, with little or no need for chemical or complete mechanical mineral phase separation, and EA-IRMS sample introduction is rapid. However, because of its simplicity and the fact that data quality depends on the control of a variety of factors, the technique requires rigid adherence to a careful sample analysis protocol.
The matching of sample and reference peak heights by sample weight adjustment minimizes non-linearity effects. An accurate calibration should be determined by using standards having a wide range of isotopic compositions, ideally bracketing the samples analysed to both low and high isotopic ratios, and a regular analysis of standards undertaken to maintain the accuracy of the calibration. The calibration equation must be monitored throughout the run by regular analysis of standards, and performance of the Cu-reduction reactor regularly checked to avoid O2 saturation. With this level of attention to analytical detail, measured precision on replicates of isotopic standards is in the order of ±0.1‰ for both C and S isotopic analyses. For S this is a significant improvement over conventional techniques, with 53% of natural samples analysed replicating to better than ±0.1‰.
