灰化法与微波消解法处理地电化学泡塑样品的分析效果对比研究   总被引：1，自引：1，他引：0  

严洪泽  孙彬彬  徐进力  周国华  贺灵  刘银飞  王腾云 《岩矿测试》2016,35(3):276-283

当前普遍使用灰化法对地电化学泡塑样品进行预处理,但可能存在高温下某些元素(如Hg、As)挥发损失的缺点。本文选择了内蒙古洛恪顿热液型铅锌多金属矿床一条地电化学勘查剖面,开展灰化法及微波消解法处理地电化学泡塑样品的勘查效果对比研究,采用原子荧光光谱和高分辨电感耦合等离子体质谱测定其中的主要元素。结果表明:①对于Zn、Cu、Fe、La等十余种元素,两种处理方法取得的异常模式基本一致,可根据实际工作需求任选一种方法进行样品预处理;②对于Au、Pb等元素,微波消解法因为取样量小,可能存在较严重的样品均匀性、代表性及分析检出限等问题,应采用灰化法;③对于Hg,灰化法存在显著的元素损失,更适合采用微波消解法;④对于As,两种方法均存在较大问题,建议参考植物样品尝试使用硝酸及高氯酸直接溶解等方法进行预处理。  相似文献   

Combination of single and sequential chemical extractions to study the mobility and host phases of potentially toxic elements in airborne particulate matter     

《Chemie der Erde / Geochemistry》2016,76(4):481-489

Risk assessment of metals associated to airborne particulate matter (PM) has usually been based on the analysis of their total concentrations, which is a poor indicator of metal mobility. Chemical fractionation processes may provide an additional level of information, however, chemical complexity and small sample sizes do not allow to combine several extraction methods. Additionally, analysing the metal concentrations during the extractions exceptionally provides restricted information about metals’ speciation. To overcome these limitations we collected total suspended particulate matter (TSP) samples from the air filters placed in the air supply channel of methane-heated turbines of thermal power stations which allows collecting large amounts of TSP materials. Additionally, we combined single and sequential chemical extractions in which not only the concentrations of potentially toxic elements (PTE) (Cd, Cr, Cu, Ni, Pb, Zn) but also that of the major chemical components (Al, Ca, Fe, K, Mg, Mn, Na, P, S, Ti) were analysed. Our aims were to study these metals’ mobility and speciation through the study of their association to major chemical components.Accumulation of the studied PTEs in the TSP material suggests moderate contamination for Ni, Cd and Cr whereas a heavy one for Cu, Zn and Pb. Three groups of these PTEs could be distinguished based on their mobility. The highly mobile Zn and Cd (large ratios of water and weak acid soluble fractions) can be considered as especially harmful elements to environment. The moderately mobile Pb and Cu (large ratios of reducible and oxidizable fractions, respectively) may potentially have a negative effect on the environment, whereas the immobile Cr and Ni cannot be expected to pose a serious risk. Based on the statistical evaluation of extraction data, the potential phases for Zn and Cu are presented by metal-sulphates, -nitrates, -chlorides, -carbonates and -hydroxides, as well as sorbed forms. Lead primarily hosted by metal-carbonates and sorbed forms, as well as by -hydroxides, whereas Cu by organic matter. Finally, Cr and Ni are mostly incorporated into very resistant phases, most probably by magnetite or other resistant metal-oxides.Combination of single and sequential extractions, as well as that of the analysis of not only the target elements but also the major chemical components were found to be a very effective tool to study the host phases of PTEs in the TSP material. The necessity for relatively large sample amounts for such analyses could be fulfilled using special sampling methodology; however, obvious disadvantages of this kind of sampling must be taken into account when resulted data are evaluated.  相似文献   

Quantification of Cl,Br and I in Geological Materials by NH4F Digestion: Comparison with Rapid Acid Digestion     

Tao He  Mufei Li  Zhaochu Hu  Wen Zhang  Haihong Chen  Zaicong Wang  Yongsheng Liu 《Geostandards and Geoanalytical Research》2023,47(1):155-168

The lack of analytical techniques for halogens in geological materials is mainly due to the loss of analytes during sample preparation. This study describes a rapid bulk rock digestion method (NH₄F digestion) for determination of the abundances of Cl, Br and I in geological materials by SF-ICP-MS. During high temperature (200–240 °C) digestion, NH₃ released from the decomposition of molten NH₄F can effectively prevent the loss of halogens released from geological samples. Chlorine, Br and I were not lost during NH₄F digestion at 220 °C for 0.25–6 h. The limits of quantitation for NH₄F digestion were 2.8, 0.018 and 0.003 μg g^-1 Cl, Br and I, respectively. Most results for halogens in geological reference materials by NH₄F digestion were in agreement with their certified values, confirming that the high-performance rapid bulk rock NH₄F digestion has sufficient digestion capability to extract Cl, Br and I from rocks, sediments and soils. In comparison, results obtained following acid digestion showed that HNO₃ + HF digestion could effectively extract Br and I from soil and sediment samples, and that HNO₃ acid digestion is only suitable to use for the determination of Br and I in soil samples.  相似文献   

电感耦合等离子体发射光谱技术测定多金属伴生矿中钨钼铋两种消解方法的对比     

党铭铭  杨萍  雷勇  温智敏  张碧兰 《岩矿测试》2021,(4):603-611

当前多金属伴生矿中钨钼铋元素的测定方法主要是传统的硫氰酸钾比色法和EDTA容量法,均为单元素分析,操作过程繁琐,分析效率低,检测周期长,难以满足大批量样品简便、快速的分析要求。本文改进了传统的单元素分析法,对比了盐酸-磷酸-高氯酸-硝酸四酸和盐酸-硝酸-高氯酸三酸两种消解体系,并结合电感耦合等离子体发射光谱法（ICP-OES）,建立了一种同时测定多金属伴生矿中钨、钼、铋的快速分析法。结果表明：合理引入磷酸的四酸消解法对样品的消解更为彻底,钨、钼、铋的测定结果准确度更高,各元素测定值和标准值的相对误差介于-5.36%~-1.39%,精密度较高（RSD ≤ 4.18%）,方法检出限介于0.0027%~0.0037%。本方法应用于分析湖南郴州某地区多金属伴生矿实际样品,各元素加标回收率介于95.0%~103.0%,各项技术指标均优于三酸消解法。本方法提高了分析效率,结果准确可靠,适用于多金属伴生矿样品中钨钼铋及其他主次量元素的批量检测。  相似文献   

国际河流公平合理利用原则:回顾、反思与消解   总被引：1，自引：0，他引：1  

曾彩琳 《世界地理研究》2012,(2):41-46

公平合理利用原则是国际水法的一项基本原则,它的适用对保护国际河流水资源及协调国际河流水资源利用冲突具有重要的意义。但伴随全球淡水资源日益匮乏,水资源利用冲突频发,公平合理利用原则的局限性也日益凸显。要摆脱公平合理利用原则难以具体运用于实践的困境,一方面需在国际法律文件中对"公平合理利用"进一步界定和完善,另一方面,需结合实际情况缔结国际河流水资源公平合理利用条约并设置相应的配套措施,以保障国际河流水资源公平合理利用原则得以真正实现。  相似文献   

微波消解-电感耦合等离子体质谱法测定植物样品中微量元素   总被引：17，自引：7，他引：10  

李刚  高明远  诸堃 《岩矿测试》2010,29(1):17-22

采用过氧化氢-硝酸作溶剂,微波消解样品,外标方法校准,电感耦合等离子体质谱法同时测定植物样品中硼、镉、铜、钴、铬、钼、锂、镍、铅、镧、锗11个微量元素。确定了微波消解仪和等离子体质谱仪的最佳工作参数,研究了有机残留物和共存离子的干扰和消除方法,选择了各元素的测定同位素,以45Sc和103Rh双内标补偿基体效应,建立了样品测定方法。方法检出限(10s)在5~150 ng/g,相对标准偏差(RSD,n=12)在1.27%~5.27%。对多种国家一级生物标准物质进行分析验证,测定值与标准值相符。方法适用于植物的果实、根、茎、叶等不同类型样品中多种微量元素的测定。  相似文献   

湿碱消解-等离子体发射光谱法测定海洋沉积物中的生物硅   总被引：2，自引：1，他引：1  

熊志方  路波  于心科  翟滨  李铁刚 《岩矿测试》2010,29(1):1-4

利用湿碱式化学提取技术和电感耦合等离子体发射光谱仪,优化样品碱式消解方法,确定仪器最佳工作条件,建立了测定海洋沉积物中不同含量级别生物硅的方法。结果表明,仪器检出限为0.724μmol/L,方法检出限为0.942μmol/L。用于测定硅酸盐-硅溶液成分分析国家一级标准物质(GBW08648和GBW 08649,标准值分别为50.0μmol/L和100.0μmol/L),测定值分别为(49.888±0.275)μmol/L、(99.578±0.651)μmol/L,相对标准偏差为0.443%、0.527%;对于不同生物硅含量级别海洋沉积物样品的平行、独立测量,其相对标准偏差8.9%。方法快速、简便、准确,可满足古海洋学不同时空尺度气候和环境分析的应用。  相似文献   

Determination of Total Sulfur in Thirty One Geochemical Reference Materials Using an Inductively Coupled Plasma-Atomic Emission Spectrometer Fitted with a Semiconductor Photodiode Detector   总被引：2，自引：0，他引：2  

Takashi Okai  Shigeru Terashima  Noboru Imai 《Geostandards and Geoanalytical Research》2001,25(1):133-136

The total sulfur contents of thirty one geochemical reference materials were determined using an inductively coupled plasma-atomic emission spectrometer fitted with a semiconductor photodiode detector. Most samples were decomposed using an HF-aqua regia digestion. However, a few were incompletely decomposed by simple acid digestion, and these were decomposed by a fusion method. The agreement between the analytical results from this work and published data is generally good.  相似文献   

消解炉消解-氧化还原滴定法测定土壤样品中有机质   总被引：1，自引：0，他引：1  

熊艳钟夏阳  陈金保 《岩矿测试》2006,25(2):191-192

沿用经典重铬酸钾氧化-外加热法的原理，建立了消解炉消解-氧化还原滴定法测定土壤样品中有机质的方法。实验选择消解温度为180—200℃，消解时间为10—15min。方法用于大批量区域多目标地球化学调查样品中有机质的分析，测试值与标准值相符。对国家土壤标准物质进行测定，方法精密度（RSD，n=8）为1．93％～7．96％。  相似文献   

镁铁-超镁铁岩铼-锇同位素体系分析方法   总被引：11，自引：5，他引：11  

孟庆 郑磊夏琼霞  靳永斌支霞臣 《岩矿测试》2004,23(2):92-96

通过试验建立了镁铁-超镁铁岩Re-Os同位素体系分析方法，包括Re-Os的化学分离纯化流程，Re同位素比值的电感耦合等离子体质谱测量方法和Os同位素比值的负离子热电离质谱测量方法。化学流程包括Carius管溶样，小型蒸馏分离Os，微蒸馏纯化Os，阴离子交换法分离、纯化Re。用该流程测定了汉诺坝幔源橄榄岩、辉石岩捕虏体和大别山饶拔寨超镁铁岩样品的Re、Os含量和Os同位素比值。  相似文献