Identification of Uranyl Minerals Using Oxygen K‐Edge X‐Ray Absorption Spectroscopy

Although most of the world's uranium exists as pitchblende or uraninite, this mineral can be weathered to a great variety of secondary uranium minerals, most containing the uranyl cation. Anthropogenic uranium compounds can also react in the environment, leading to spatial–chemical alterations that could be useful for nuclear forensics analyses. Soft X‐ray absorption spectroscopy (XAS) has the advantages of being non‐destructive, element‐specific and sensitive to electronic and physical structure. The soft X‐ray probe can also be focused to a spot size on the order of tens of nanometres, providing chemical information with high spatial resolution. However, before XAS can be applied at high spatial resolution, it is necessary to find spectroscopic signatures for a variety of uranium compounds in the soft X‐ray spectral region. To that end, we collected the near edge X‐ray absorption fine structure (NEXAFS) spectra of a variety of common uranyl‐bearing minerals, including uranyl carbonates, oxyhydroxides, phosphates and silicates. We find that uranyl compounds can be distinguished by class (carbonate, oxyhydroxide, phosphate or silicate) based on their oxygen K‐edge absorption spectra. This work establishes a database of reference spectra for future spatially resolved analyses. We proceed to show scanning X‐ray transmission microscopy (STXM) data from a schoepite particle in the presence of an unknown contaminant.     

Community‐Derived Standards for LA‐ICP‐MS U‐(Th‐)Pb Geochronology – Uncertainty Propagation,Age Interpretation and Data Reporting

The LA‐ICP‐MS U‐(Th‐)Pb geochronology international community has defined new standards for the determination of U‐(Th‐)Pb ages. A new workflow defines the appropriate propagation of uncertainties for these data, identifying random and systematic components. Only data with uncertainties relating to random error should be used in weighted mean calculations of population ages; uncertainty components for systematic errors are propagated after this stage, preventing their erroneous reduction. Following this improved uncertainty propagation protocol, data can be compared at different uncertainty levels to better resolve age differences. New reference values for commonly used zircon, monazite and titanite reference materials are defined (based on ID‐TIMS) after removing corrections for common lead and the effects of excess ²³⁰Th. These values more accurately reflect the material sampled during the determination of calibration factors by LA‐ICP‐MS analysis. Recommendations are made to graphically represent data only with uncertainty ellipses at 2s and to submit or cite validation data with sample data when submitting data for publication. New data‐reporting standards are defined to help improve the peer‐review process. With these improvements, LA‐ICP‐MS U‐(Th‐)Pb data can be considered more robust, accurate, better documented and quantified, directly contributing to their improved scientific interpretation.     

Automated Extraction of a Five‐Year LA‐ICP‐MS Trace Element Data Set of Ten Common Glass and Carbonate Reference Materials: Long‐Term Data Quality,Optimisation and Laser Cell Homogeneity

LA‐ICP‐MS is increasingly applied to obtain quantitative multi‐element data with minimal sample preparation, usually achieved by calibration using reference materials (RMs). However, some ubiquitous RMs, for example the NIST SRM 61× series glasses, suffer from reported value uncertainties for certain elements. Moreover, no long‐term data set of analyses conducted over a range of ablation and tuning conditions exists. Thus, there has been little rigorous examination of the extent to which offsets between measured and reported values are the result of error in these values rather than analytically induced fractionation. We present new software (‘LA‐MINE’), capable of extracting LA‐ICP‐MS data with no user input, and apply this to our system, yielding over 5 years of data (~ 5700 analyses of ten glass and carbonate RMs). We examine the relative importance of systematic analytical bias and possible error in reported values through a mass‐specific breakdown of fourteen of the most commonly determined elements. Furthermore, these data, obtained under a wide range of different ablation conditions, enable specific recommendations of how data quality may be improved, for example the role of diatomic gas, the effect of differential inter‐glass fractionation factors and choice of transport tubing material. Finally, these data demonstrate that the two‐volume Laurin ablation cell is characterised by no discernible spatial heterogeneity in measured trace element ratios.     

Petrophysical characterisation of tight sandstone gas reservoirs using nuclear magnetic resonance: a case study of the upper Paleozoic strata in the Kangning area,eastern margin of the Ordos Basin,China

Residual and movable porosity are significant parameters for characterising petrophysical properties, especially in tight reservoirs. Eight tight sandstone samples from the upper Paleozoic gas-bearing strata in the Kangning area, from the eastern margin of the Ordos Basin, were analysed using nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), petrography, and porosity and permeability tests. The lithology and pore types were identified and classified using petrography and SEM. The residual and movable porosity were obtained with NMR. In addition, NMR was used to visualise pore structure and pore size distribution. The results suggest that the upper Paleozoic sandstones in the study area mainly comprise feldspathic litharenite and litharenite. The sandstone porosity and permeability are low, with means of 5.9% and 0.549 mD, respectively. Four pore types exist in the tight sandstones: residual primary pores, grain dissolution pores, micropores (clay-dominated) and microfractures. The T₂ spectra under water-saturated conditions correlate with pore size and can be used to distinguish small and large pores based on the transverse relaxation time cutoff value of 10 ms, which corresponds to a pore diameter of 0.232 μm. Small pores account for 72% of the pores in the tight sandstones. The continuous bimodal T₂ spectra suggest good connectivity between small and large pores, despite the low porosity and permeability. In this study, the movable porosity of the major tight sandstone gas reservoirs is higher than the residual porosity, which confirms the effective evaluation of movable porosity to tight sandstone reservoirs, based on NMR experiments.     

微束分析测试技术十年(2011~2020)进展与展望

现代地球科学研究的重大突破在很大程度上取决于观测和分析技术的创新。新世纪以来,我国地球科学领域引进了一批高性能新型微束分析仪器设备,建立了一批高规格的实验室。本文回顾了近十年来微束分析技术与方法的主要进展及其在地球科学研究中的应用实例,包括电子探针、扫描电镜、透射电镜、大型离子探针、纳米离子探针、飞行时间二次离子质谱、激光剥蚀等离子体质谱、激光诱导原子探针、原子探针技术、显微红外光谱、同步辐射等,这些分析技术的进步和广泛应用极大地提高了我们对地球和行星演化历史及许多地质过程的理解。今后,应加快微束分析的新技术、新方法和新标准的开发,特别是高水平人才队伍建设,提高创新能力并在国际学术舞台上发挥重要作用。     

Rapid U‐Pb Geochronology by Laser Ablation Multi‐Collector ICP‐MS

Detrital zircon (DZ) U‐Pb laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) has revolutionised the way geologists approach many Earth science questions. Although recent research has focused on rapid sample throughput, acquisition rates are limited to 100–300 analyses h^?1. We present a method to acquire zircon U‐Pb dates at rates of 120, 300, 600 and 1200 analyses h^?1 (30, 12, 6 and 3 s per analysis) by multi‐collector LA‐ICP‐MS. We demonstrate the efficacy of this method by analysing twelve zircon reference materials with dates from ~ 3465 to ~ 28 Ma. Mean offset from high‐precision dates increases with faster rates from 0.9% to 1.1%; mean random 1s uncertainty increases from 0.6% to 1.3%. We tested this new method on a sandstone sample previously characterised by large‐n DZ geochronology. Quantitative comparison shows increased correspondence among age distributions comprising > 300 dates. This new method holds promise for DZ geochronology because (a) it requires no major changes to hardware, but rather modifications to software; (b) it yields robust age distributions well‐suited for quantitative analysis and maximum depositional age calculations; (c) there is only a minor sacrifice of accuracy and measurement uncertainty; and (d) there is less burden to researchers in terms of time investment and analytical cost.     

基于三维激光扫描技术的岩质边坡泥化夹层空间分布和几何形态

为了定量研究泥化夹层的空间分布和几何形态,以云南省玉溪市生活垃圾焚烧发电厂高边坡局部开挖剖面为对象,利用徕卡ScanStation C10三维激光扫描仪和瑞典ROMER RA-7520-2六轴关节臂三维测量仪进行扫描,得到了开挖剖面和泥化夹层的原始点云数据;然后采用Cyclone和Geomagic Wrap软件对点云数据进行一系列处理,分析了泥化夹层的三维空间分布、层面产状、间距、层面粗糙度和几何形态。结果表明：大部分泥化夹层横向分布于整个扫描剖面,少数呈局部分布;泥化夹层的平均倾向为196.41°±5.51°,平均倾角为22.27°±2.23°,间距在3.7~49.1 cm之间,平均值为（20.4±12.0）cm;不同层位及同一层位不同横向位置的泥化夹层厚度都不等,最厚约20 mm,最薄小于1 mm;泥化夹层顶面局部典型区域的平面拟合偏差在-22.4~32.5 mm之间,沿夹层倾向的粗糙度系数在5.67~16.77之间,平均值为10.11±3.25;泥化夹层的表面积与体积之比在5.14~5.86 cm^-1之间。运用三维激光扫描技术研究泥化夹层的空间分布和几何形态是可行的。玉溪市生活垃圾焚烧发电厂高边坡的泥化夹层具有宏观整体上相对平直、相互近似平行、非等距分布、间距小、层数多、厚度薄,细观上顶面粗糙底面相对光滑、三维形态复杂的特点。     

北部湾悬浮颗粒现场剖面测量与粒度分析

应用LISST-100现场激光粒度仪于2006年8月在北部湾首次进行了悬浮颗粒剖面测量,获得了整个垂直剖面的悬浮颗粒现场粒径分布、体积比和光衰减系数,并计算得到了垂直剖面的总浓度和各层的粒度参数及粒级组成。结果表明,悬浮颗粒自上而下均为双峰分布,只是表层的双峰位于5．57μm和34．4μm,中间层和底层的双峰位于34．4μm和129．4μm。悬浮颗粒体积比自上而下逐渐增大,到达底层时达到最大。光衰减系数的变化趋势与颗粒体积比非常相似,且二者存在很好的相关性,相关系数高达0．98。整个垂直剖面上,表层粒度较细,随着深度增加粒度逐渐变粗,到达底层时粒度最粗。悬浮体总体上正偏,峰态值较小,分选较差。粒度以砂为主,粉砂含量次之,不舍黏土。     

主成分分析法在油荧光光谱波段选择中的应用

355nm激光器发射激光入射到海水表面,激发海表面溢油的荧光光谱,运用高光谱图像降维中应用广泛的分段主成分分析算法对油荧光光谱进行波段选择。该算法把每个分段被映射到主成分的信息量的大小作为是否被选择的标准,保证了选择波段的信息丰富;通过分段分析消除了传统主成分分析的全局性引起的波段忽略问题,获得较为满意的降维效果。     

DZJ2激光垂准仪使用方法及指标的校正

介绍了DZJ2激光垂准仪的性能及基本指标的校正方法,为用户在使用DZJ2激光垂准仪过程中几种基本指标参数的校正提供参考.