Rapid Determination of Trace and Ultra Trace Level Elements in Diverse Silicate Rocks in Pressed Powder Pellet Targets by LA‐ICP‐MS using a Matrix‐Independent Protocol

A simple, single sample preparation involving pressed rock powder pellets was utilised to determine the trace and ultra trace abundances of petrogenetically important elements including high field‐strength elements and REEs by laser ablation‐ICP‐MS. One of the elements predetermined by XRF spectrometry served as an internal standard. The influence of sample preparation parameters (grain size, pellet compactness and amount of binding media) on analytical performance was also investigated, including sample homogeneity issues at the laser sampling scale. Line scanning with a high repetition frequency (20 Hz) and large beam diameter (200 μm) ensured ablation from a larger sample surface area, eliminating issues related to sample heterogeneity. A median grain size of about 10 μm for silicate rock powders was found to be sufficiently representative at this scale of laser sampling. Granitic rocks or samples containing resistant minerals such as zircon needed extra grinding to achieve grain sizes down to < 5 μm for better precision for elements that are concentrated in these phases. Using ¹³⁷Ba as an internal standard, reasonable accuracies within 15–20% for most of the high mass trace elements were achieved; in the case of low mass elements, it may deviate up to 40%. Precision of measurements rarely exceeded 15% RSD.     

安徽石马超高压变质地体构造演化的流体包裹体响应

安徽石马超高压变质地体经历 5次构造变形 ,其特征是由深层次挤压韧性变形到浅层次的伸展脆性变形。相应地发育有 5期流体 ,它们的演化规律为 :早期以硅酸盐熔体和流体熔融体为主 ,随后富CO2 流体占优势 ,后期H2 O溶液起主导作用。总体而言 ,从老到新流体均一温度和含盐度均由高变低。在构造作用和流体作用的共同推动下 ,石马超高压变质地体经历了复杂的演化过程 :洋壳俯冲 ,超高压榴辉岩形成与形变→陆壳碰撞 ,榴辉岩折返→地体构造分异 ,榴辉岩就位→地体均衡隆起 ,榴辉岩抬升→地体差异隆起 ,榴辉岩剥露。因此 ,流体作用在研究超高压变质地体中占有重要地位。流体直接影响超高压变质地体形成的物理化学环境 ,在分析其形成深度时 ,应充分考虑流体超压问题。总之 ,在超高压地体演化过程中 ,流体一直是积极推动其发展的最活跃的因素。     

我国首次发现的硅钾铀矿

硅钾铀矿属罕见的次生铀矿物,1986年我国首次发现于甘肃龙首山铀矿床氧化。带。对该矿物进行了多种测试工作。矿物为层状结构的铀酰硅酸盐矿物。晶胞参数a=6.62,b=7.03,c=7.06,β=105.2°。化学式:(K_(0·58) Na_(0·33)0.91(H_3O)[UO_2SiO_4]·0.8H_2O     

Routine Control of Accuracy in Silicate Rock Analysis by X-Ray Fluorescence Spectrometry

In this study, we used the modified Horwitz expression (H_c= 0.01c^0.8495, which gives the precision as a function of concentration) to evaluate and control the accuracy of results of silicate rock analysis obtained by X-ray fluorescence spectrometry. This expression is currently used by the organisers of the GeoPT international proficiency tests, to assign the precision limits of each analyte and subsequently to evaluate the data provided by laboratories whose main application is geochemistry. Results for major and trace elements, determined in glass disk and pressed pellets, respectively, were evaluated. Nine international silicate rock reference materials were analysed and results were compared to the recommended values plus and minus the limits given by the above expression. Those limits are easily attained for most major elements, but not for trace elements. Sample preparation and sub-sampling contributions to precision were evaluated by analysis of an in-house reference sample. In our results, precision does not follow the Horwitz expression relationship with concentration. It is known that the final accuracy in XRF analysis depends strongly on instrumental settings and on the uncertainties associated with the certified or recommended values of the reference materials used to calibrate the spectrometer, but our results indicate that the precision expression can be useful, especially to inspect and correct calibration curves and to check routine instrumental accuracy.     

Structural characterisation of the high-pressure phase CaAl4Si2O11

Single crystals of CaAl₄Si₂O₁₁ were synthesised at 1,500?°C and 14 GPa in a multi-anvil press, and the structure of the phase determined by single-crystal X-ray diffraction at room conditions. The structure-type is that of the “hexagonal barium ferrites”. The space group of the average structure is P6 ₃ /mmc and the cell parameters are a?=?5.4223(4) Å, c?=?12.7041(6) Å, V?=?323.28(5) ų, with Z?=?2, and its density is 3.905?g?cm^?3, which is reasonable for a high-pressure alumino-silicate phase. The 22 oxygen and two calcium atoms within the unit-cell form an approximate hexagonal-close-packed array. Ten of the twelve octahedral interstices within this array that have only oxygen atoms for apices are filled with Si and/or Al. M1 octahedra share edges to form a spinel-like sheet of octahedra. The average bond length ?=?1.833 Å suggests mixed occupancy by Si and Al. The M1 octahedral sheets are linked by shared corners to pairs of face-sharing M2 octahedra containing Al, with ?= 1.918 Å. The remaining two cations of the unit-cell contents statistically occupy four tetrahedrally-coordinated interstices, which occur as face-sharing pairs. The average bond length for these sites (1.742 Å) suggests that they are occupied by Al, although Si occupancy cannot be excluded by the data. It is proposed that only one interstice of each pair is locally occupied, with the possibility of some short-range ordering of such occupancies. Complete long-range order leading to the acentric space group P6 ₃ mc is excluded by the data, as is the possibility of the average structure being comprised of merohedral (0?0?0?1) twins of P6 ₃ mc symmetry.     

Properties of circumstellar silicate dust (Review)

Es wird eine Übersicht über den gegenwärtigen Stand des Wissens über die Eigenschaften des zirkumstellaren Silikatstaubes gegeben. Nach der Darstellung der Entdeckungsgeschichte werden die Objekte zusammengestellt, in deren Spektren Silikatbanden beobachtet werden. Der Zusam-menhang zwischen den optischen Eigenschaften der Silikatteilchen und der Struktur der zirkumstellaren Hüllen bei der Bestimmung der ausgesandten Infrarotstrahlung wird analysiert, und alle wichtigeren Untersuchungen von Staubhüllen mit Silikatteilchen werden zusammengetragen. Wir diskutieren die optischen Eigenschaften des zirkumstellaren Silikatstaubes, wobei die amorphe Struktur besonders betont wird. Abschließend wird auf die Bedeutung von Feinstrukturen innerhalb der 10-μm-Bande, die bei verschiedenen Objekten beobachtet wurden, eingegangen.