激光剥蚀等离子体质谱分析中激光剥蚀参数对信号响应的影响

探讨了激光剥蚀等离子体质谱固体微区分析中激光剥蚀参数对元素分析信号灵敏度及稳定性的影响。这些参数包括激光功率、脉冲频率、剥蚀孔经、散焦距离、剥蚀方式等。讨论了优化的激光剥蚀等离子体质谱信号采集及数据处理方式。在全质量范围内选用具有代表性的元素作为研究对象,建立了激光剥蚀的一般性特征规律和266nm紫外激光系统的最佳操作条件。在选定的激光剥蚀参数下,大多数被测元素的检出限为22.8~457ng/g,能够满足固体微区分析的要求。     

原子荧光光谱法测定化探样品时有机质对As,Sb,Bi的干扰

通过研究黑龙江省森林沼泽景观区有机水系沉积物（泥炭）、土壤中As,Sb,Bi的测定结果，发现样品中的有机质对王水消解氢化物原子荧光法测定上述元素存在极大的干扰，提出采用低温（＜450℃）灰化处理可完全消除干扰。对比研究还发现，过去森林沼泽景观区的区域化探扫面资料中的As,Sb,Bi数据存在问题，应专门对其进行评价研究。     

A Reappraisal of Rb, Y, Zr, Pb and Th Values in Geochemical Reference Material BHVO-1

The geochemical reference material BHVO-1 was analysed by a variety of techniques over a six year period. These techniques included inductively coupled plasma-mass spectrometry and atomic emission spectroscopy (ICP-MS and ICP-AES, respectively), laser ablation ICP-MS and spark source mass spectroscopy. Inconsistencies between the published consensus values reported by Gladney and Roelandts (1988, Geostandards Newsletter) and the results of our study are noted for Rb, Y, Zr, Pb and Th. The values reported here for Rb, Y, Zr and Pb are generally lower, while Th is higher than the consensus value. This is not an analytical artefact unique to the University of Notre Dame ICP-MS facility, as most of the BHVO-1 analyses reported over the last ten to twenty years are in agreement with our results. We propose new consensus values for each of these elements as follows: Rb = 9.3 ± 0.2 μg g-1 (compared to 11 ± 2 μg g-1), Y = 24.4 ± 1.3 μg g-1 (compared to 27.6 ± 1.7 μg g-1), Zr = 172 ± 10 μg g-1 (compared to 179 ± 21 μg g-1), Pb = 2.2 ± 0.2 μg g-1 (compared to 2.6 ± 0.9 μg g-1) and Th = 1.22 ± 0.02 μg g-1 (compared to 1.08 ± 0.15 μg g-1).     

Raman scattering and X-ray diffraction study of the thermal decomposition of an ettringite-group crystal

 A Raman scattering and X-ray diffraction study of the thermal decomposition of a naturally occurring, ettringite-group crystal is presented. Raman spectra, recorded with increasing temperature, indicate that the thermal decomposition begins at ≈55 °C, accompanied by dehydration of water molecules from the mineral. This is in contrast to previous studies that reported higher temperature breakdown of ettringite. The dehydration is completed by 175 °C and this results in total collapse of the crystalline structure and the material becomes amorphous. The Raman scattering results are supported by X-ray diffraction results obtained at increasing temperatures. Received: 9 July 2001 / Accepted: 14 August 2002     

Advances in energy-dispersive X-ray fluorescence

Recently, two new instruments for X-ray fluorescence analysis (XRF) with interesting features for geochemical applications came to the market. Both instruments were designed to improve the peak to background ratio, the principal factor limiting the sensitivity of XRF. Total reflection XRF (TXRF) was designed to analyse extremely small sample amounts. An instrument, using polarised X-rays (P-XRF) for excitation, is designed to reduce scattered background in spectra of bulk samples. The performance of both instruments was compared with conventional XRF-methods and ICP/MS. Results for GXR-1, GXR-2, GXR-3, GXR-4 and GXR-6 obtained with TXRF and P-XRF are in good agreement with literature data. The effective amount of sample, analysed by TXRF was 200 μg only and detection limits of ~ l μg/g were achieved. P-XRF shows considerable improved detection limits (0.25–0.5 μg/g) for bulk samples for elements with atomic numbers 42–51 (Mo-Sb) compared with conventional XRF-methods.     

Surface chemical analysis in coal preparation research: complementary information from XPS and ToF-SIMS

The application of X-ray photoelectron spectroscopy (XPS) to coal surface characterisation for preparation research is described. Progress towards the acquisition of complementary surface chemical information by time-of-flight secondary ion mass spectrometry (ToF-SIMS) is also discussed. Surface-based beneficiation techniques such as flotation are assuming greater importance as the proportion of fines in raw coal increases due to the proliferation of high capacity mining methods. A necessary condition for the floatability of a coal particle is adequate hydrophobicity, and the degree of hydrophobicity of the flotation concentrate is one factor influencing the ease with which its dewatering can be affected. The hydrophobicity of a coal is very difficult to measure directly because of microporosity, and it is often necessary to deduce the degree of hydrophobicity from a knowledge of the surface chemistry. XPS is able to provide sufficient analytical data to allow relative levels of hydrophobicity to be estimated. In principle, ToF-SIMS should be able to supply additional information enabling refinement of such estimates; however, there are insufficient data at present to allow the ionic fragments detected to be related to specific functional groups at the coal surface.     

X射线荧光测井的井液效应及其校正

本文从Ｘ射线的性质，以及Ｘ射线与物质作用的机理出发，对井液效应进行了研究，并对其影响过程进行模拟。在理想井液模型上，推导出Ｘ射线活度与钻孔参数的数理关系。在此基础上，进一步研究得到了能适应野外多变情况的井液效应校正公式（ＣＢＷＥ）和方法。     

原位磁化X射线粉末衍射法测还原铁粉的微观磁致伸缩系数

首次报导X射线粉末衍射法测量铁粉晶胞的磁致伸缩系数。还原铁粉样品原位磁化后 ,铁立方晶胞产生磁致伸缩效应 ,晶胞参数的变化引起衍射峰位置和晶面间距的变化。实验测得铁晶胞λ1 0 0 为 3 .3 3× 10 - 4,此结果表明铁晶胞的微观磁致伸缩系数比棒状、薄膜或粉末压片的系数大约 16倍。对此现象进行了合理的理论解释 ,指出大块材料中的粉末多晶之间具有较大的空隙 ,从而使得宏观磁致伸缩系数变小     

CHARACTERIZATION OF DEFORMATION AND X-RAY PETROFABRICS IN THE MIDDLE PART OF THE WAHONGSHAN FAULT ZONE, QINGHAI PROVINCE, NORTHWESTERN CHINA

The Wahongshan fault zone in Qinghai province is one of the most important faults in westem China. In this paper, deformation and X-ray petrofabrics have been studied in the middle segment of the fault. The results show that the formation of the fault zones can be divided into two major stages: ductile shear deformation stage and brittle deformation stage. The early stage ductile shearing leads to the formation of the NW-NNW trending mylonite zones along the fault, which is intensely cut by the late-formed brittle faults. X-ray petrofabrics of rocks near the faults indicate that the minerals in the tectonites show a great degree of orientation in the alignment. The quartz, which is a very important mineral in the tectonites, is deformed by basal face gliding or near basal face gliding, and sometimes by prismatic face sliding, which indicates that the rocks are deformed in epithermal to mesothermal or mesothermal environment, and the dynamic recrystallization also plays an important role in the formation     

发射光谱载体蒸馏法测定地质样品中微量硼铍锡银

选择了适合的缓冲剂,利用载体蒸馏法将被测元素与基体元素分离,使Be转变为易挥发的氟化物与B、Sn、Ag同时蒸发;降低了谱线背景及元素检出限;加入内标元素Au、Bi,提高了方法的准确度和精密度;采用普通 3mm×3mm×0.7mm杯型电极,装样量少,操作简单。方法检出限(wB/10-6)分别可达B1.5、Be0.3、Sn0.8、Ag0.02;准确度(Δlog C)基本在-0.05～0.05,精密度(RSD,n=8)为2.9%～17%。