Development of sulfide calibration standards for the laser ablation inductively-coupled plasma mass spectrometry technique

The requirements of standard materials for LA-ICP-MS analysis have been difficult to meet for the determination of trace elements in sulfides. We describe a method for the production of synthetic sulfides by precipitation from solution. The method is detailed by the production of approximately 200 g of a material, PS-1, with a suite of chalcophilic trace elements in an Fe-Zn-Cu-S matrix. Preliminary composition data, together with an evaluation of the homogeneity for individual elements, suggests that this type of material meets the requirements for a sulfide calibration standard that allows for quantitative analysis. Contamination of the standard with Na suggests that H2S gas may prove a better sulfur source for future experiments. We recommend that calibration data be collected in whatever mode is closest to that employed for the analysis of the unknown material, because of variable fractionation effects as a function of analytical mode. For instance, if individual spot analyses are attempted on unknown sample, then a raster of several individual spot analyses, not a continuous scan, should be collected and averaged for the standard. Hg and Au are exceptions to the above and calibration data should always be collected in a scanning mode. Au is more heterogeneously distributed than other trace metals and large-area scans are required to provide an average value for calibration purposes. We emphasize that the values given in Table 1 are preliminary values. Further chemical characterization of this standard, through a round-robin analysis program, will allow the USGS to provide both certified and recommended values for individual elements. The USGS has developed PS-1 as a potential new LA-ICP-MS standard for use by the analytical community, and requests for this material should be addressed to S. Wilson. However, it is stressed that an important aspect of the method described here is the flexibility for individual investigators to produce sulfides with a wide range of trace metals in variable matrices. For example, PS-1 is not well suited to the analysis of galena, and it would be relatively straightforward for other standards to be developed with Pb present in the matrix as a major constituent. These standards can be made easily and cheaply in a standard wet chemistry laboratory using equipment and chemicals that are readily available.