Enhanced Oxygen Isotope Determination in Uranium Oxides Using BrF5 Fluorination

A new method for accurate determination of oxygen isotopes in uranium oxides encountered in the nuclear fuel cycle was developed using the conventional BrF₅ fluorination technique. Laser‐assisted fluorination was tested for comparison. We focused on fine powders of triuranium octoxide (U₃O₈), uranium dioxide (UO_2±x with 0 ≤ x ≤ 0.25), uranium trioxide (UO₃.nH₂O, with 0.8 ≤ n ≤ 2) and diuranates (M₂U₂O₇.nH₂O, with M = NH₄, Na or Mg_0.5 and 0 ≤ n ≤ 6). Fluorination at room temperature and heating under vacuum at 150 °C are shown to eliminate both adsorbed and structural water from the powder samples. Precision fit for purpose of δ¹⁸O values (± 0.3‰, 1s) and oxygen yields (close to 100%) were obtained for U₃O₈ and UO₂ where oxygen is only bound to uranium. A lower precision was observed for UO₃.nH₂O and M₂U₂O₇.nH₂O where oxygen is both present in the structural H₂O and bonded to uranium and where the extracted O_2(g) can be contaminated by NF₃ and NO_x compounds. Laser‐assisted fluorination gave shifted δ¹⁸O values between +0.8 and +1.4‰ for U₃O₈, around ?0.8‰ for UO₃.nH₂O and between ?3.9 and ?4.5‰ for M₂U₂O₇.nH₂O (± 0.3‰, 1s) compared with the conventional method.     

GGR Biennial Critical Review: Analytical Developments Since 2014

This GGR biennial critical review covers developments and innovations in key analytical methods published since January 2014, relevant to the chemical, isotopic and crystallographic characterisation of geological and environmental materials. In nine selected analytical fields, publications considered to be of wide significance are summarised, background information is provided and their importance evaluated. In addition to instrumental technologies, this review also presents a summary of new developments in the preparation and characterisation of rock, microanalytical and isotopic reference materials, including a précis of recent changes and revisions to ISO guidelines for reference material characterisation and reporting. Selected reports are provided of isotope ratio determinations by both solution nebulisation MC‐ICP‐MS and laser ablation‐ICP‐MS, as well as of radioactive isotope geochronology by LA‐ICP‐MS. Most of the analytical techniques elaborated continue to provide new applications for geochemical analysis; however, it is noted that instrumental neutron activation analysis has become less popular in recent years, mostly due to the reduced availability of nuclear reactors to act as a neutron source. Many of the newer applications reported here provide analysis at increasingly finer resolution. Examples include atom probe tomography, a very sensitive method providing atomic scale information, nanoscale SIMS, for isotopic imaging of geological and biological samples, and micro‐XRF, which has a spatial resolution many orders of magnitude smaller than conventional XRF.     

E5000型全谱直读型电弧发射光谱仪研制及其在地球化学样品分析中应用

在地球化学样品检测工作中,Ag、B、Sn等难分析元素通常采用传统的交流电弧发射光谱法(摄谱仪),随着地球化学样品数量的增加以及对检测结果质量要求的提高,该方法操作复杂、分析过程繁琐的问题与日常大量样品分析的矛盾日益突出,多道式电弧直读发射光谱也开始在行业内应用。本文基于先进的数字光源技术和CCD全谱型光谱仪技术,改进了电弧发生系统、分光系统和检测系统,将电弧激发光源与Paschen-Runge型全谱CCD光谱仪结合,研制了一款新型的台式全谱直读型电弧发射光谱仪E5000。E5000型电弧发射光谱仪通过激光定位结合程控电极技术,自动调整电极位置,提高了采谱过程的精度控制;利用CCD全谱技术获得了激发样品的全谱信息,可轻易实现光谱信号的背景扣除和干扰校正;且无需再次测定黑度,直接获得分析结果;同时结合内标法和标准加入法,可以进一步提高复杂基体样品的分析精准度。应用研制的光谱仪对水系沉积物和土壤样品进行检测,Ag、B、Sn元素的检出限分别达到了0.01μg/g、0.65μg/g、0.16μg/g,在分析水系沉积物、土壤时检测精密度基本小于10%,优于当前的摄谱法和多道电弧直读光谱法,满足了地球化学样品检测质量要求。     

具有多种断层结构岩样的形变和破裂特征的试验研究

在岩石板上切割出多条切缝并以石膏填充,将其分为3个构造特征区:A区(断层交汇区)、B区(左行左列岩桥区)、C区(右行左列岩桥区)。采用双轴加压、定点应变、声发射信息系统和实时全息干涉计量方法(激光)进行观测研究。结果表明:在岩样破坏孕育过程中,各个特征区都出现了特大破裂。每个特大破裂发生前定点应变、激光干涉条纹图(应变场)和声发射信息都出现了特征变化。特大破裂的发生有先后,其前兆特征的出现也有先后,并且各区有各自的特点,某些前兆还可能在各区之间交替出现。研究认为,三个区的断层结构性质不同,这就导致了不同的破裂顺序,甚至产生不同的前兆现象。     

Testing a new combined (U,Th)–He and U/Th dating approach on Plio-Pleistocene calcite speleothems

The geochronology of cave deposits in the Cradle of Humankind UNESCO World Heritage Site in South Africa provides a timeframe essential for the interpretation of its fossils. The uranium-lead (U–Pb) and uranium-thorium disequilibrium (U/Th) dating of speleothems, mostly flowstones that underlie and blanket the fossil-bearing sediments, have been effective in this sense, but U–Pb is limited by the requirement of ∼1 ppm U concentrations and low common Pb contents, and U/Th has a c. 500 ka limit of applicability. Here we report age results for calcite-aragonite speleothems obtained using a new combined uranium-thorium-helium ((U,Th)–He) and U/Th dating routine. We reproduced within analytical uncertainty, the published U–Pb or U/Th ages for (a) flowstone in three drill core samples in the range 2000–3000 ka, (b) a flowstone hand sample taken at surface with an age of 1800 ka, and (c) five underground flowstone samples in the range 100–800 ka. Calcite retentivity for He under cave conditions is thus demonstrated. In the few cases where helium loss was observed in speleothems, only some of the subsamples were affected, and to varying degrees, suggesting loss by lattice damage not related to diagenetic processes, rather than volume diffusion. In the 100 to 800 ka range, the combined U/Th disequilibrium and (U,Th)–He method also yielded reliable values for initial (²³⁰Th/²³⁸U) and (²³⁴U/²³⁸U) activity ratios. Importantly, most subsamples had high initial (²³⁰Th/²³⁸U) values, ranging from 1.0 to 19.7, although having low Th/U ratios. This is probably due to incorporation of Fe–Mn oxides-hydroxides dust, on which ²³⁰Th was previously adsorbed. Such samples are mostly not dateable by U/Th without the additional input from the He analysis. If not detected and corrected for, such high initial (²³⁰Th/²³⁸U) values can lead to inaccurate U/Th and U–Pb ages. Our study shows that the incorporation of He analysis in U/Th dating has broad potential application, with four methods for calculating the ages, in carbonates from different environments where U-Pb or U/Th dating would not work.     

Normal Point Algorithm For Reduction Of Two Colour Slr Observations

Two colour laser ranging to artificial satellites is an attractivetechnique, which is capable to provide refraction corrected ranges without the need of an atmospheric model by measuring the dispersive delay of laser pulses of different wavelength. Although the required accuracy of the detection scheme is stringent, the technique has matured so far, that routine two colour observationsbecame feasible.The present paper describes a normal point procedure reducing two colour laser range observations with respect to the dispersive delay,exploiting the knowledge of satellite response signatures in conjunction with detector characteristics and the appropriate center of mass correction models.Moreover the dispersion model of the atmosphere is briefly reviewed, paying attention to the wavelength domains provided by modern twocolour ranging lasers, e.g., the Ti:SAP laser.Preliminary data is presented and compared to both, normal point data reduced with a standard procedure and zenith path equivalent meteorological parameters.     

193nmLA-ICPMS对国际地质标准参考物质中42种主量和微量元素的分析

本文采用配备有 193nm Ar F准分子 (excimer)激光器的 Geo L as2 0 0 M剥蚀系统和 Elan6 10 0 DRC ICP- MS对 4个美国地质调查所 (USGS)玻璃标准参考物质以及 3个美国国家标准技术研究院 (NIST)人工合成硅酸盐玻璃标准参考物质中几乎覆盖整个质量数范围 (从 7L i到 2 38U)的 38个微量和 4个主量 (Na、Mg、Ti和 Mn)元素进行了分析。分析结果表明 ,无论是对 USGS还是 NIST玻璃 ,元素分析的相对标准偏差 RSDs和分析值与参考值之间的相对偏差 (RDs)一般优于 10 % ,RSD和RD较大的元素主要出现在含量很低或不均匀样品中。稀土元素的 RSD显示 ,除 AGV- 2 G可能存在不均匀现象外 ,其它所测样品在 6 0 μm尺度上 ,元素分布是均匀的。本研究证明 ,由于 ICP- MS具有 10 8cps(每秒计数 )的动态线性范围 ,本实验室的L A- ICPMS系统可定量分析含量在百分之几的主量元素及微量元素。分析精密度和准确度可与常规溶液雾化进样 ICP- MS方法相媲美     

吐哈盆地及二连盆地侏罗系煤微类脂组分的共聚焦激光扫描显微镜（CLSM）研究及油气意义

吐哈盆地产出有比较丰富的侏罗系煤成油气田，本文用共聚焦激光扫描显微镜和热解分析等手段研究了煤中类脂组及微类脂组的类型、含量、分布与煤成烃性能和产出的关系。观察分析结果表明：在一般煤岩组分观测中主要含煤的西山窑组和八道湾组煤层类脂组含量很少超过１０％，但是一些煤样的热解分析中Ｓ＿１可高达５－２３ｍｇ／ｇ，Ｓ＿２可达１５０─２００ｍｇ／ｇ，ＨＩ（烃／有机碳）可高达１５０─３５０ｍｇ／ｇ生烃、含烃性能较好。进一步用共聚焦激光显微镜观测结果表明：本区一些薄层状、条带状煤层的基质镜质体和叶结构镜质体中微类脂组含量比较丰富，微区定量统计含量在３％─１８％左右。这种富含微类脂组的基质镜质体和结构镜质体在煤成油气中有重要意义，而且由于多数微类脂体在煤中常成点线状、似层状、充填状、网络状分布，可能有利于煤成油气的运移和聚集。     

新疆罗布泊盐湖卤水资源综合开发研究

罗布泊盐湖赋存有丰富的含钾硫酸镁亚型卤水,现已探明仅罗北凹地区段孔隙度储量2.67×109 t(折合KCl),属特大型钾盐卤水矿藏,是生产硫酸钾的理想原料;此外,卤水中含有丰富的钠、镁、锂、硼等资源,综合回收利用价值较大.本文针对罗布泊盐湖卤水资源,在有效利用盐湖钾资源同时,加快其他共生资源的综合开发进程,将新疆罗布泊盐湖资源开发建设推向持续、合理、有效、高值的循环经济发展的道路,为国家西部经济开发做出贡献.     

超深地下连续墙施工中若干问题探讨

随着地下空间工程的不断发展,超深地下连续墙的应用越来越多,施工的风险也越来越高。结合工程实践,对超深地下连续墙施工方法及施工中存在的若干问题进行探讨、分析,并提出相对应的解决措施。通过采用先进合理的解决措施,超深地下连续墙的施工是完全能达到设计要求的。