Refinement of Phosphorus Determination in Quartz by LA‐ICP‐MS through Defining New Reference Material Values

Abstract

The aim of this study was to improve the quality of laser ablation inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) determination of phosphorus in crystalline quartz. Over the last decade, the Geological Survey of Norway has routinely performed trace element determinations on quartz from both operating and potential quartz deposits by LA‐ICP‐MS. The determined phosphorus concentrations were, with but few exceptions, consistently within the range of 10 to 30 μg g−1, results that seemed to be both too high and too consistent. The multi‐material calibration curve obtained from a suite of reference materials (NIST SRM 610, 612, 614, 1830, BAM No. 1 amorphous SiO2 glass) did not define a precise regression line. Published phosphorus concentrations for the reference materials are poorly constrained and the observed dispersions along the multi‐material calibration curve suggest that some of the reference values may be inaccurate. Furthermore, the calibration curve did not pass through the origin of the [(cps 31P/cps 30Si) · cone. Si] vs. P concentration diagram; thus, in addition to the uncertainties of the literature values of phosphorus, it is difficult to define the calibration curve. Three reference materials (NIST SRM 614, 1830, synthetic quartz KORTH) were sent for phosphorus accelerator implantation, providing an independent and accurate (± 3%) approach for determining phosphorus concentrations in crystalline quartz. The intrinsic phosphorus concentrations of the three implanted samples plus those for NIST SRM 610 and 612 were determined by secondary ion mass spectrometry (SIMS), yielding new phosphorus values for NIST SRM 610, 612, 614 and 1830. Using these new values resulted in a better defined LA‐ICP‐MS calibration curve. However, the source of the ICP‐MS related background could not be defined, such that it must still be empirically corrected for.