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71.
Analysis of Sediments and Soils by X-Ray Fluorescence Spectrometry Using Matrix Corrections Based on Fundamental Parameters 总被引:2,自引:0,他引:2
Jacinta Enzweiler Maria Aparecida Vendemiatto 《Geostandards and Geoanalytical Research》2004,28(1):103-112
Wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) is widely used for the analysis of soils and sediments using well characterised procedures. However, difficulties can occur with samples such as unknowns containing small amounts of ore materials and samples collected from contaminated sites where trace elemental concentrations can exceed the concentration range for routine analysis. We studied the performance of a commercially available method, based on fundamental parameters (FP) to correct matrix effects. The spectrometer was originally calibrated with elemental or simple compound calibrants. Samples were analysed as pressed powder pellets. Eighteen sediment and soil reference materials, three of them with certified values for some of their constituents, were used to evaluate accuracy, by comparing results with recommended values and their standard deviations (RV ± 2s) or certified values and their confidence intervals (CV ± Cl). When results fell systematically outside these intervals, calibrations were refined with geochemical reference materials. The best agreement of results with recommended and certified values was obtained when the contents of H2 O and C in each sample were included as matrix constituents during calculations. The detection limits of trace elements tended to be relatively high, because the measuring conditions employed were not maximised for sensitivity. The main advantage of the method tested was that it enabled the analysis of samples with high concentrations of trace elements and the determination of elements such as F, Bi, Sb and W, which are not commonly included in quantitative XRF analysis of geological samples. 相似文献
72.
A Reflection on Mg, Cd, Ca, Li and Si Isotopic Measurements and Related Reference Materials 总被引:6,自引:1,他引:6
Jean Carignan Damien Cardinal Anton Eisenhauer Albert Galy Mark Rehkamper Frank Wombacher Nathalie Vigier 《Geostandards and Geoanalytical Research》2004,28(1):139-148
This contribution aims to report the reflections we had with the scientific community during two international workshops on reference materials for stable isotopes in Davos (2002) and Nice (2003). After evaluating the isotopic homogeneity of some existing reference materials, based on either certificates, literature data or specific inter-laboratory rounds, we confirm these as primary reference materials or propose new ones relative to which stable isotope compositions should be reported. We propose DSM-3 for Mg, NIST SRM 915a for Ca, L-SVEC for Li and NBS28 for Si. Cadmium does not yet have a well identified delta zero material, although three commercial mono-elemental Cd solutions have yielded the same isotopic composition relative to one another. In order to scale the linearity of any mass spectrometer, some secondary reference materials are also proposed: Cambridge-1 solution for Mg, the "Münster-Cd" and JEPPIM Cd solutions for Cd and the "Big Batch" silicate for Si. The team from Nancy propose to prepare a mixed spike solution for Li isotopes. Well-characterised natural samples such as ocean or continental waters, diatoms, sponges, rocks and minerals are needed to validate the entire analytical procedure, particularly to take into account the effect of sample mineralisation and of chemical manipulations for elemental separation prior to analysis. 相似文献
73.
Precise/ Small Sample Size Determinations of Lithium Isotopic Compositions of Geological Reference Materials and Modern Seawater by MC-ICP-MS 总被引:6,自引:1,他引:6
Alistair B. Jeffcoate Tim Elliott Alex Thomas Claudia Bouman 《Geostandards and Geoanalytical Research》2004,28(1):161-172
The Li isotope ratios of four international rock reference materials, USGS BHVO-2, GSJ JB-2, JG-2, JA-1 and modern seawater (Mediterranean, Pacific and North Atlantic) were determined using multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS). These reference materials of natural samples were chosen to span a considerable range in Li isotope ratios and cover several different matrices in order to provide a useful benchmark for future studies. Our new analytical technique achieves significantly higher precision and reproducibility (< ± O.3%o 2s) than previous methods, with the additional advantage of requiring very low sample masses of ca . 2 ng of Li. 相似文献
74.
Marcel Guillong Kathrin Hametner Eric Reusser Stephen A. Wilson Detlef Günther 《Geostandards and Geoanalytical Research》2005,29(3):315-331
New glass reference materials GSA-1G, GSC-1G, GSD-1G and GSE-1G have been characterised using a prototype solid state laser ablation system capable of producing wavelengths of 193 nm, 213 nm and 266 nm. This system allowed comparison of the effects of different laser wavelengths under nearly identical ablation and ICP operating conditions. The wavelengths 213 nm and 266 nm were also used at higher energy densities to evaluate the influence of energy density on quantitative analysis. In addition, the glass reference materials were analysed using commercially available 266 nm Nd:YAG and 193 nm ArF excimer lasers. Laser ablation analysis was carried out using both single spot and scanning mode ablation. Using laser ablation ICP-MS, concentrations of fifty-eight elements were determined with external calibration to the NIST SRM 610 glass reference material. Instead of applying the more common internal standardisation procedure, the total concentration of all element oxide concentrations was normalised to 100%. Major element concentrations were compared with those determined by electron microprobe. In addition to NIST SRM 610 for external calibration, USGS BCR-2G was used as a more closely matrix-matched reference material in order to compare the effect of matrix-matched and non matrix-matched calibration on quantitative analysis. The results show that the various laser wavelengths and energy densities applied produced similar results, with the exception of scanning mode ablation at 266 nm without matrix-matched calibration where deviations up to 60% from the average were found. However, results acquired using a scanning mode with a matrix-matched calibration agreed with results obtained by spot analysis. The increased abundance of large particles produced when using a scanning ablation mode with NIST SRM 610, is responsible for elemental fractionation effects caused by incomplete vaporisation of large particles in the ICP. 相似文献
75.
在邻海地区富含高承压水的土层中施工预应力锚杆支护工程的难度很大.介绍了锚杆的构造、作用机理、施工工艺以及决定锚杆施工质量的关键技术.以深圳某商住楼基坑施工为例,探讨了在承压水土层中采用锚杆支护的方法,创造性地提出了"先堵水后注浆"的施工工艺,可供沿海、沿江地区的类似工程借鉴. 相似文献
76.
77.
通过对桩侧和桩底后压浆,可大幅度提高钻孔灌注桩单桩承载力.应用桩-土理论分析了后压浆中浆液对土体及桩体的作用,并从分析影响桩基承载力的因素出发,研究了后压浆的作用机理.在渗透率小的地层中后压浆以压密注浆为主,在渗透率大的地层中后压浆以渗透注浆为主.为避免过分压裂土层,在压浆过程中应控制灌浆压力.压浆量是影响后压浆质量和提高单桩承载力的关键因素之一. 相似文献
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