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USGS · 70030705

Development of a standard reference material for Cr(vi) in contaminated soil

Abstract

Over the last several decades, considerable contamination by hexavalent chromium has resulted from the land disposal of Chromite Ore Processing Residue (COPR). COPR contains a number of hexavalent chromium-bearing compounds that were produced in high temperature industrial processes. Concern over the carcinogenic potential of this chromium species, and its environmental mobility, has resulted in efforts to remediate these waste sites. To provide support to analytical measurements of hexavalent chromium, a candidate National Institute of Standards and Technology (NIST) Standard Reference Material?? (SRM 2701), having a hexavalent chromium content of approximately 500 mg kg -1, has been developed using material collected from a waste site in Hudson County, New Jersey, USA. The collection, processing, preparation and preliminary physico-chemical characterization of the material are discussed. A two-phase multi-laboratory testing study was carried out to provide data on material homogeneity and to assess the stability of the material over the duration of the study. The study was designed to incorporate several United States Environmental Protection Agency (USEPA) determinative methods for hexavalent chromium, including Method 6800 which is based on speciated isotope dilution mass spectrometry (SIDMS), an approach which can account for chromium species inter-conversion during the extraction and measurement sequence. This journal is ?? The Royal Society of Chemistry 2008.

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S.J. Nagourney, S. A. Wilson, B. Buckley, H.M.S. Kingston, S.-Y. Yang, S.E. Long. 2008. Development of a standard reference material for Cr(vi) in contaminated soil. https://doi.org/10.1039/b808488b

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Accuracy and precision of U–Pb zircon geochronology at high spatial resolution (7–20 μm spots) by laser ablation-ICP-single-collector-sector-field-mass spectrometry

Use of small spots (≤20µm) for laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) U-Pb zircon geochronology is of increasing interest in the Earth sciences because the temporal record of geologic processes is often preserved on a fine-scale within zircon grains. However the systematic biases and external sources of uncertainity of U-Pb ages is poorly defined when measured on small spots by LA-ICP-single-collector-sector-field (SF)-MS instrumentation. This study addresses the accuracy and precision for small spots and specifically the extent to which short ablation times limit Pb/U Down-Hole Fractionation (DHF), which largely controls the accuracy of the U-Pb ages. Six zircon reference materials (91500, FC-1, R33, Temora 2, Plešovice and Fish Canyon Tuff) were measured on spot sizes of 20, 15, 10 and 7 µm diameter. Laser fluence was increased from 3 to 6 J/cm2 with decreasing spot size to compensate partially for decreasing U and Pb signals. 91500 zircon was the calibration reference material. Raw count rate data were processed using Iolite version 3.63 software with the U-Pb Common Approach data reduction scheme and smoothed cubic spline DHF correction model. Samples were ablated for 30 seconds and results processed for the first 28, 15, 10 and 7 seconds of ablation (masking the initial 2 seconds) in order to assess the accuracy and precision of U-Pb ages as a function of ablation time. Measured 206Pb/238U ratios for the six zircon reference materials increase steadily with ablation time, reflecting DHF, but exhibit somewhat different patterns of increase for different zircons, producing the major source of uncertainty for the U-Pb ages. A secondary source of uncertainty is differences between the 206Pb/238U (normalized to their accepted values) for different zircons near the start of ablation, which may reflect matrix-dependent instrumental mass bias in the ICP. Nonetheless, processing data from only the first 10 to 15 seconds of ablation (50 to 75 laser pulses) restricts the extent of DHF and time-resolved Pb/U variations between different zircons to a sufficient degree to give concordant U-Pb ages on 20 to 7 µm spots that are accurate and precise to better than 1.4% using LA-ICP-single-collector-SF-MS instrumentation.

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