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.     

Analytical perspective on trace element species of interest in exploration

Analysis of soil and sediment samples, using selective extraction methods to distinguish different phases, is of particular interest in exploration geochemistry to locate deeply buried mineral deposits. There are various mechanisms of binding labile elements in the secondary environment, including physical and chemical sorption, precipitation, chelation and complexation. Phases present in soils and sediments which are likely to scavenge ‘free' elements include amorphous Mn and Fe oxides, the humic and fulvic components of humus, and clays. This paper reviews these forms of trace elements and the methods in current use to quantify them. Examples of precision data, both for control and survey samples, are given with respect to trace elements dissolved from the ‘soluble organic' component of humus, Mn oxides and amorphous Fe oxides. The high sensitivity of inductively coupled plasma mass spectrometry (ICP–MS) is required to measure accurately and precisely a large suite of trace elements, especially where only small fractions of elements are dissolved by such leaches as the commercially available Enzyme and MMI (Mobile Metal Ion) extractions. The relative standard deviations (RSD) obtained for 33 elements (e.g. Ag, Cd, In, I) in the standard reference sample (SRM), TILL-2, are in the range 0.5–8% for the hydroxylamine hydrochloride (NH₂OH·HCl) leach designed to extract hydrous Fe and Mn oxides. The corresponding RSDs for elements in the reactive Mn oxide phase extracted by the Enzyme leach are in the range 3–19% except for some trace elements at levels close to detection limit (e.g. Cd, Bi). The RSDs obtained for field duplicates are inferior to those for analytical replicates (i.e. sample splits), probably a reflection of different concentrations of the host phase. In one soil survey, the Fe extracted by a 0.25 M NH₂OH·HCl leach ranged conservatively from 0.2 to 1.7% whereas the Mn extracted by the Enzyme leach varied extensively, from 0.3 to >999 ppm. In contrast, precision, at 1–7% RSD, for field duplicates was found to be comparable with that for both analytical duplicates and the SRM, LKSD-4, for elements associated with the humic and fulvic component of humus samples sieved to <177 μm.     

2014年2月12日于田7.3级大震对青藏东北缘地震活动的影响分析

First of all,using the GPS velocity field from campaign GPS measurements implemented by CMONC( C hina Crustal Movement Observation) a nd TEONC( C hina Tectonic Environment Observation Networks) u p to 2013, w e analyzed the background of regional crustal horizontal movement and deformation before the M S7. 3 Yutian,Xinjiang earthquake on February 12,2014. Then,by comparing this to the vertical movement from leveling measurements,we studied the crustal movement deformation and the state of strain accumulation on the northeastern edge of Qinghai-Tibetan block.Finally,we investigated the possible effects on the earthquake activity of the northeastern edge of Tibet from the M S7. 3 Yutian earthquake. The result indicates that,the M S7. 3Yutian earthquake occurred against the background of strong tectonic movement and intensive intracontinental crustal differential movement on the edges of tectonic blocks in western China,and also that it happened in the period of the strong tectonic stress field in Qinghai-Tibetan block and its edges. The sinistral strike-slip and stress transfer of the Yutian M S7. 3 earthquake may accelerate the rupture of fault segments with high strain accumulation at the northeastern edge of Qinghai-Tibetan block( especially in Qilian Mountain fault zone,and border area of Gansu,Qinghai and Sichuan provinces on the south of western Qinling).     

汶川大地震(MS 8.0)同震变形作用及其与地质灾害的关系

2008年5月12日发生于四川盆地西部龙门山断裂带的汶川大地震（MS 8.0）波及半个亚洲,震撼整个中国。本文通过地震后的实地调查,对发育在龙门山断裂带上的同震地表破裂带的分布、产状、继承性复活与变形特征,以及同震变形与地震地质灾害的关系等进行了初步总结,分析表明这次汶川大地震(MS 8.0)沿北川-映秀逆冲断裂和安县-灌县逆冲断裂同时发生地表破裂,前者产生以高角度逆冲兼右旋走滑为特征的地表破裂带长约275 km,后者产生以缓倾角逆冲作用为特征的地表破裂带长约80 km。汶川大地震的同震地表破裂带分布具有分段性特征,并与地表破坏程度的分带性有着一定的内在联系,详细研究表明,同震地表破裂带的产状直接影响地表破坏程度和地震地质灾害的强度,汶川大地震（MS 8.0）沿呈高角度陡倾的北川-映秀逆冲断裂发育的同震地表变形所产生的地表破坏程度和地震地质灾害的强度比沿缓倾角的安县-灌县逆冲断裂要强。从各种类型的地震断裂来看,具有垂直运动的逆冲型地震断裂所造成的地表破坏程度和地质灾害强度比具水平运动的走滑型地震断裂要强。因此,汶川大地震发生的破裂过程和同震地表变形与地震地质灾害的关系值得深入研究。     

2021年3月19日西藏比如MS 6.1地震总结

2021年3月19日西藏比如MS 6.1地震发生在班戈—安多地区的安多盆地南缘断裂附近,震源机制解反演结果显示,本次地震为近东西走向断层产生正断兼走滑型错动的结果,与区域构造特征一致;截止至4月15日,地震序列跟踪发现,主震与余震震级差为1.4,主震释放能量占序列的98.96％,表明6.1级主震释放了此次地震序列的绝大...     

Detection of petroleum contamination in river sediments from Quebec City region using GC–IRMS

Isotopic analysis by compound specific gas chromatography–isotope ratio mass spectrometry (GC–IRMS) is used to detect and characterize petroleum pollution in surficial sediments along the St Lawrence River, near Quebec City. Unusually mature n-alkane distributions have been found in some recent intertidal sediments in the region. GC–IRMS results suggest that the n-alkanes are not derived from indigenous organic sources because they carry δ¹³C values between −30.0 and −27.0‰, as well as very small isotopic differences between odd and even numbered n-alkanes, which are both typically associated with petroleum products. Comparison of these sediments with bunker fuel, an oil used in the shipping industry, has shown a close isotopic correlation in some sites, which is further supported by biomarkers. Overall, the contamination has been dispersed along the river but is generally localized around the industrial region where hydrocarbon transfer from shore storage to ships takes place. This study illustrates how GC–IRMS can be used effectively in the detection and characterization of petroleum pollutants in sediments.     

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     

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.     

Effect of the Dry Ashing Method on Cadmium Isotope Measurements in Soil and Plant Samples

A dry ashing method is commonly used to remove organic material from samples prior to geochemical analysis. In the course of this study, the Cd isotope ratios of a series of soil and plant reference materials and samples were studied to evaluate the effect of the dry ashing method on measurement results of Cd isotope ratios. The samples were pre‐treated using the dry ashing method and high‐pressure bomb for comparison. The results show that the digestion using high‐pressure bombs did not lead to Cd loss, but using the dry ashing method would cause different proportions of Cd loss. The whole range of Cd isotope difference between two methods was from ?0.07‰ to 3.01‰. There was also an obvious difference in measured Cd isotope ratios from the same leaf sample pre‐treated independently by the dry ashing method, indicating that the amount of Cd loss and the effect on Cd isotope measurement during dry ashing is related to the properties of the samples. Therefore, dry ashing may not be appropriate for the removal of organic material in Cd isotope ratio measurement, especially for samples with high organic contents. The δ^114/110Cd values of reference materials NIST SRM 1573a and GSD‐30 are reported for the first time in this study.     

与澜沧大震可能相关的震磁效应——小波分析一例

用小波法分析了与1988年澜沧大震相关的通海台地磁Z分量资料。小波分析结果显示地震前“日变幅差”ΔTg(24)存在可能的异常变化;异常为正异常,异常幅度很大,异常结束后立即发生了地震。