An efficient, clean procedure for the measurement of element mass fractions in bulk rock nanoparticulate pressed powder pellets (PPPs) by 193 nm laser ablation ICP-MS is presented.Samples were pulverised by wet milling and pelletised with microcrystalline cellulose as a binder, allowing non-cohesive materials such as quartz or ceramics to be processed. The LA-ICP-MS PPP analytical procedure was optimised and evaluated using six different geological reference materials (JP-1, UB-N, BCR-2, GSP-2, OKUM, MUH-1), with rigorous procedural blank quantification employing synthetic quartz. Measurement trueness of the procedure was equivalent to that achieved by solution ICP-MS and LA-ICP-MS analysis of glass. The measurement repeatability was as low as 0.5 to 2% (1s, n = 6) and, accordingly, PPP homogeneity could be demonstrated. Calibration based on the reference glasses NIST SRM 610, NIST SRM 612, BCR-2G and GSD-1G revealed matrix effects for glass and PPP measurement with NIST SRM 61x; using basalt glasses eliminated this problem. Most significantly, trace elements not commonly measured (flux elements Li, B; chalcophile elements As, Sb, Tl, In, Bi) could be quantified. The PPP LA-ICP-MS method overcomes common problems and limitations in
Accepted ArticleThis article is protected by copyright. All rights reserved. analytical geochemistry, and thus represents an efficient and accurate alternative for bulk rock analysis.Bulk rock major to trace element concentration data are vital to our understanding of geochemical and petrological processes. Several analytical procedures have been established and optimised, most importantly (1) X-ray fluorescence (XRF) analysis of pressed powder pellets or fused glass discs using (for example) Li2B4O7 as a flux; (2) acid/bomb digestion and subsequent measurement in solution via inductively coupled plasma-mass spectrometry (ICP-MS); or (3) fusion techniques without addition of a flux, (e.g., on a strip heater, to produce glass blebs for measurement by laser ablation ICP-MS, LA-ICP optical emission spectroscopy, electron probe microanalysis, or secondary ion mass spectrometry). Although these techniques have been widely employed, each is limited to a series of elements due to procedural, instrumental or blank-related limitations, and some of them are very laborious.Conventional XRF determination of trace elements often suffers from high limits of detection (LODs) notably for elements emitting low energy X-rays. Only for a few elements (e.g., Rb, Sr, Zr or Nb), can LODs down to 1-10 µg g -1 be achieved (Potts 2003). However, multiple correction steps (e.g., matrix corrections, correction for flux/sample ratio in fused samples, correction for spectral line overlap) are needed, especially for elements emitting low energy X-rays. Hence, trace element data may lack accuracy and precision, limiting the application of XRF to certain trace elements and rock types. Alternatively, Li2B4O7 XRF glass pellets can be measured for trace elements by LA-ICP-MS (e.g., Ødegård and Hamester 1997, Günther et ...