微波消解-氢化物发生原子荧光光谱法和质谱法测定高有机质无烟煤中汞砷的可行性研究   总被引：2，自引：2，他引：0  

杨常青  张双双  吴楠  侯艳娜  徐彩春  徐志彬 《岩矿测试》2016,35(5):481-487

微波消解技术适用于处理大部分煤炭样品,但对于高有机质含量的无烟煤样品,因其煤化程度高,含有多种复杂的高分子有机化合物,应用现有的消解技术不能将其完全消解。本文对微波消解的实验条件包括消解试剂、消解温度及消解时间进行优化,确定了适合处理高有机质无烟煤的消解体系,评价了采用HG-AFS和ICP-MS测定其中总汞和总砷含量的可行性。结果表明,以硝酸-硫酸-氢氟酸(6∶4∶0.5)作为微波消解试剂,消解温度达205℃,保持30 min可将高有机质含量的无烟煤彻底分解,其中硫酸对无烟煤的消解起到了关键作用;ICP-MS与HG-AFS对汞的检测结果一致,回收率都达到98%以上,但由于砷的化学形态复杂,有机态砷不能全部转化无机态砷使得HG-AFS对砷的检测结果偏低。因此,对于有机质含量特别高(81%~90%)的煤炭样品,微波消解可将其彻底转化为溶液,用ICP-MS可以准确定量其中的汞和砷,而HG-AFS不能作为检测砷的有效手段。  相似文献   

Stress and pore pressure histories in complex tectonic settings predicted with coupled geomechanical-fluid flow models     

《Marine and Petroleum Geology》2016

Most of the methods currently used for pore pressure prediction in sedimentary basins assume one-dimensional compaction based on relationships between vertical effective stress and porosity. These methods may be inaccurate in complex tectonic regimes where stress tensors are variable. Modelling approaches for compaction adopted within the geotechnical field account for both the full three-dimensional stress tensor and the stress history. In this paper a coupled geomechanical-fluid flow model is used, along with an advanced version of the Cam-Clay constitutive model, to investigate stress, pore pressure and porosity in a Gulf of Mexico style mini-basin bounded by salt subjected to lateral deformation. The modelled structure consists of two depocentres separated by a salt diapir. 20% of horizontal shortening synchronous to basin sedimentation is imposed. An additional model accounting solely for the overpressure generated due to 1D disequilibrium compaction is also defined. The predicted deformation regime in the two depocentres of the mini-basin is one of tectonic lateral compression, in which the horizontal effective stress is higher than the vertical effective stress. In contrast, sediments above the central salt diapir show lateral extension and tectonic vertical compaction due to the rise of the diapir. Compared to the 1D model, the horizontal shortening in the mini-basin increases the predicted present-day overpressure by 50%, from 20 MPa to 30 MPa. The porosities predicted by the mini-basin models are used to perform 1D, porosity-based pore pressure predictions. The 1D method underestimated overpressure by up to 6 MPa at 3400 m depth (26% of the total overpressure) in the well located at the basin depocentre and up to 3 MPa at 1900 m depth (34% of the total overpressure) in the well located above the salt diapir. The results show how 2D/3D methods are required to accurately predict overpressure in regions in which tectonic stresses are important.  相似文献   

MRI-CGCM模式对东亚夏季风的模拟评估及订正     

罗连升  段春锋  杨玮  徐敏  程智  丁小俊 《大气科学》2016,40(6):1320-1332

本文利用CMAP月降水资料、NCEP再分析资料、NOAA的ERSST资料和日本气象厅海气耦合模式（MRI-CGCM）的输出结果,从东亚夏季风气候态、主模态和年际变率等方面分析了MRI-CGCM模式对东亚夏季风的预测性能,并且利用观测的东亚夏季风指数（EASMI）与模拟PC（principal component）的关系建立多元线性回归方程来订正EASMI（简称PC订正法）。结果表明:MRI-CGCM模式能够较好再现东亚夏季风降水和低层风场的气候态,但模拟的西北太平洋反气旋偏弱、偏东,使得模拟的副热带地区降水量偏小。模式较好地模拟出东亚夏季风降水第一模态（EOF1）及相应的低层风场,能够较好再现出EOF1对应El Ni?o衰减位相;模拟降水的EOF1与观测之间的空间相关系数（ACC）为0.72,且能较好地再现其对应的年际变率,其时间系数PC1与观测之间的相关系数为0.41,能模拟出观测EOF1的2 a和5 a主导周期;但模拟的我国以东梅雨锋区雨带位置偏南,这与模拟的西北太平洋反气旋位置偏南有关。模式对降水第二模态EOF2的模拟能力比EOF1明显下降,模拟EOF2与观测之间的ACC降到0.36;虽然模式能较好地再现出EOF2对应El Ni?o发展位相,但模拟的西太平洋反气旋位置偏南,使得雨带位置偏南,模拟的我国梅雨锋区雨带位于江南,与观测场上江南少雨相反。模式较好地模拟出我国东部夏季降水和气温空间异常分布和年际变化,模拟与观测夏季降水和气温的多年平均ACC分别为0.74和0.68。模式模拟我国东部、江淮流域和华南地区夏季降水多年平均PS评分分别为69、70和68分,略高于我国夏季降水业务预测多年平均评分（65分）。模拟的我国东部夏季气温与观测多年平均PS评分为74分。PC订正后EASMI与实况的相关系数由0.51提高到0.65、符号一致率由84%升到91%、标准差由0.75增大到1.4、大于1个标准差年数由6年变为12年,订正后在模拟变幅偏小和梅雨锋区雨带偏南等方面均有一定的改善,对应西太平洋反气旋位置和梅雨锋区雨带位置与实况较为吻合。  相似文献   

四酸敞口溶解-电感耦合等离子体发射光谱法测定土壤中的硫   总被引：2，自引：2，他引：0  

姜云军  李星  姜海伦  张宁  韩雪  朱永晓 《岩矿测试》2018,37(2):152-158

当前土壤中硫元素的测定方法主要是X射线荧光光谱法和燃烧法,上述两种方法分析速度慢,对高、低含量样品的分析精度较差,难以满足大批量样品快速、准确分析的要求。为提高分析速度和结果的准确度,本文建立了用盐酸-硝酸-氢氟酸-高氯酸(四酸)溶解土壤样品,电感耦合离子体发射光谱法测定硫的方法。通过考察王水消解、王水水浴消解和四酸消解的溶样效果,测定结果表明采用四酸能更好地溶解土壤样品中的硫。方法检出限为10μg/g,测量范围为33.3~50000μg/g,相对标准偏差为0.47%~4.05%。本方法简单快速,准确度高,已经过数千件实际样品验证,在不增加分析成本的情况下,一份溶液还可以同时测定钾钠钙镁铁锰铍锂镧铈钪钒钴镍钛等元素,适合在地质行业推广应用。  相似文献   

应用ICP-MS研究川西南龙马溪组泥页岩稀土元素特征及沉积环境   总被引：2，自引：2，他引：0  

张茜  余谦  王剑  肖渊甫  程锦翔  赵安坤  张彬 《岩矿测试》2018,37(2):217-224

为深入研究盐源盆地龙马溪组黑色岩系的沉积环境、构造背景及物源属性,指导区域页岩气勘探及相关研究,本文利用电感耦合等离子体质谱技术研究了盐源盆地南缘龙马溪组黑色页岩的稀土元素地球化学特征和沉积环境。结果表明:该区稀土总量偏低,轻稀土富集重稀土亏损,轻重稀土分异较大;δCe_N均值为0.87,显示弱的负异常,δEu_N值为0.66~1.43,变化范围较大,说明源岩成分复杂;La_S/Yb_S均值为1.31,说明研究区构造背景主要为被动大陆边缘,源岩为古老沉积岩、花岗岩及中基性岩的混合物,推测康滇古陆为其提供了主要物源。δCe_S为负异常,δEu_S为正异常,La/Ce1等特征均指示沉积期水体为还原环境,推测为深水陆棚沉积,且受到一定程度热水沉积影响。深海热液带来丰富的营养元素有利于有机质形成,还原水体环境有利于有机质保存,使得研究区龙马溪组泥岩页富含有机质,且富有机质页岩段厚度较大,由此初步认为龙马溪组泥页岩为优质烃源岩储层。  相似文献   

铌钽元素分析技术新进展   总被引：2，自引：2，他引：0  

李刚  姚玉玲  李婧祎  赵朝辉  罗涛  李崇瑛 《岩矿测试》2018,37(1):1-14

铌钽是发展新兴产业所需的功能性和结构性材料,铌钽矿产是国家重点支持的战略新兴矿产资源,开展相关物料中铌钽的分析技术研究具有重要意义。由于铌和钽的物理化学性质十分相似,彼此难以分离,且易水解,加之地质样品分解困难,因此铌和钽的分析测试一直困扰着分析工作者。本文重点对铌钽元素分析中的样品前处理技术和现代分析测试技术进行综述。样品前处理是铌钽分析的关键环节,结合分析方法和样品特性,选择合理的样品分解和分离富集方法是准确测定铌钽的前提。仪器分析是现代分析测试技术的主流,电感耦合等离子体发射光谱/质谱法(ICP-OES/MS)是目前测定铌钽应用最多的方法,需要解决共存组分的干扰、基体效应和盐类影响等问题。激光剥蚀(LA)技术、X射线荧光光谱法(XRF)和中子活化分析法(NAA)采用固体进样,避免了前期样品处理的繁琐步骤和杂质的引入,是铌钽元素分析发展的方向。  相似文献   

树脂交换分离-电感耦合等离子体质谱法测定铅锌矿中钨钼锡锗硒碲   总被引：3，自引：3，他引：0  

张洁  阳国运 《岩矿测试》2018,37(6):657-663

铅锌矿常与硫化矿共生形成复合多金属矿床,其中伴生有益元素的含量对矿床的综合利用评估有重要的参考意义。在目前常用方法中,钨钼锡锗硒碲主要采用分组或单独熔矿和测试的方法,操作强度大、分析效率低,且高含量铜、铅和含量高于1μg/g的硒分别干扰钨钼和碲的测定。本文采用过氧化钠碱熔,提取后加入0. 8%柠檬酸溶液络合钨、钼、锡形成金属复合物,以8～9 g阳离子树脂交换分离高含量钠盐和铜、铅、锌、铁等主量元素,采用动能歧视模式以铼、硼为内标用电感耦合等离子体质谱仪同时测定钨钼锡锗硒碲的含量。经树脂处理后,铜铅锌铁的去除率均高于96%,在测定介质中实际浓度为0. 192 ng/mL～1. 28μg/mL,基本消除了主量元素的干扰。各待测元素工作曲线相关系数为0. 9994～0. 9999,优于阳离子树脂处理前的0. 9923～0. 9992。经标准物质验证,各元素测定相对误差为-8. 33%～7. 00%,加标回收率为94. 9%～107. 5%,相对标准偏差(RSD,n=8)小于8%。该方法在样品前处理环节将主量干扰元素从溶液体系中分离,优化了测定介质,实现了铅锌矿中多元素的准确快速测定。  相似文献   

乙醇介质制备载炭泡塑及其在地质样品金测定中的应用   总被引：2，自引：2，他引：0  

马怡飞  汪广恒  张尼  高文旭  权斌 《岩矿测试》2018,37(5):533-540

载炭泡塑相较于无负载泡塑,可有效提高泡塑对金的吸附能力,但现有制备载炭泡塑的方法制备效率不高。为了缩短制备载炭泡塑的时间,提高制备效率,本文采用活性炭-乙醇溶液制备载炭泡塑,通过优化制备条件,包括负载介质的种类、试剂浓度、浸泡时间,使得制备100个载炭泡塑的时间可以控制在30 min之内,并结合ICP-OES建立了测定地质样品中金的方法。实验结果表明:该方法的振荡时间可以缩短至20 min。金的质量浓度在0～100. 00μg/mL范围内与光谱强度呈良好的线性关系,相关系数为0. 9997,方法检出限(3σ)为0. 0066μg/g,测定结果相对标准偏差为0. 81%～2. 11%(n=10)。该方法经4个国家标准物质验证,准确度与精密度良好,能够满足地质样品中金的分析测试要求。  相似文献   

Nonlinear dynamics and recurrence analysis of extreme precipitation for observed and general circulation model generated climates          下载免费PDF全文

Dionysia Panagoulia  Eleni I. Vlahogianni 《水文研究》2014,28(4):2281-2292

A statistical framework based on nonlinear dynamics theory and recurrence quantification analysis of dynamical systems is proposed to quantitatively identify the temporal characteristics of extreme (maximum) daily precipitation series. The methodology focuses on both observed and general circulation model (GCM) generated climates for present (1961–2000) and future (2061–2100) periods which correspond to 1xCO₂ and 2xCO₂ simulations. The daily precipitation has been modelled as a stochastic process coupled with atmospheric circulation. An automated and objective classification of daily circulation patterns (CPs) based on optimized fuzzy rules was used to classify both observed CPs and ECHAM4 GCM‐generated CPs for 1xCO₂ and 2xCO₂ climate simulations (scenarios). The coupled model ‘CP‐precipitation’ was suitable for precipitation downscaling. The overall methodology was applied to the medium‐sized mountainous Mesochora catchment in Central‐Western Greece. Results reveal substantial differences between the observed maximum daily precipitation statistical patterns and those produced by the two climate scenarios. A variable nonlinear deterministic behaviour characterizes all climate scenarios examined. Transitions’ patterns differ in terms of duration and intensity. The 2xCO₂ scenario contains the strongest transitions highlighting an unusual shift between floods and droughts. The implications of the results to the predictability of the phenomenon are also discussed. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

Estimating liquefaction-induced settlement of shallow foundations by numerical approach     

Hadi Shahir  Ali Pak 《Computers and Geotechnics》2010

Occurrence of liquefaction in saturated sand deposits underlying foundation of structure can cause a wide range of structural damages starting from minor settlement, and ending to general failure due to loss of bearing capacity. If the bearing capacity failure is not the problem, reliable estimation of the liquefaction-induced settlement will be of prime importance in assessment of the overall performance of the structure. Currently, there are few procedures with limited application in practice for estimation of settlement of foundations on liquefied ground. Therefore, development of a general relationship is important from the practical viewpoint. In this paper, the dynamic response of shallow foundations on liquefied soils is studied using a 3D fully coupled dynamic analysis. For verification of the numerical model, simulation of a centrifuge experiment is carried out and the analysis results are compared with the experimental measurements. The results of centrifuge experiment are taken from the literature for the purpose of comparison and the experiment has not been performed by the authors. After verification of the numerical model, a practical relationship for estimation of liquefaction-induced settlement of rigid footings on homogeneous loose to medium fine sand is proposed based on the results of a comprehensive parametric study. In the interpretation process, the soil layer thickness in which the liquefaction takes place is found to be a key parameter, since by normalization with respect to this parameter, effects of a number of other parameters can be eliminated.  相似文献