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生物样品中微量元素硒的分析检测,经典方法是湿法消解-氢化物发生原子荧光光谱法(HGAFS)。湿法消解处理生物样品需使用大量试剂,并且消解时间长,样品背景值高;HG-AFS的分辨率较低,已经不能满足微量硒的分析需求。解决生物样品的消解过程缓慢、试剂用量大的问题是提高样品中微量元素硒的检出限和分辨率的前提。本文采用湿法消解和微波消解两种消解体系处理样品,对两种方法制备的溶液分别采用HG-AFS和电感耦合等离子体质谱法(ICP-MS)进行测定,通过对比试验确定了微波消解ICP-MS方法可以实现生物样品中微量硒的准确测定。对比试验表明:采用高压密闭微波消解前处理样品技术可以大大缩短消解时间,减少试剂用量,降低了样品背景值;利用ICP-MS直接进行测定,方法检出限为0.01μg/g,精密度(RSD,n=12)小于4%,低于HG-AFS的检出限(0.03μg/g)和精密度(10%)。微波消解ICP-MS方法操作简单快捷,降低了方法检出限,提高了样品分析的准确度和精密度。 相似文献
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研究建立了增压-微波消解电感耦合等离子体质谱法测定含难溶矿物(含铌钽铀矿物、锆石等)岩石样品中微量元素的测试方法。该技术有效地解决了传统湿法消解方法不能完全消解含难溶矿物(含铌钽铀矿物、锆石等)岩石样品的难题。根据超高压-微波消解原理,自行设计加工了电加热增压消解装置一台。该装置的技术创新在于对含难溶矿物岩石样品采用了在同一消解罐中先微波消解再增压消解的方式,解决了微波消解到增压消解的转换问题,实现了对含难溶矿物岩石样品的无交叉污染、低本底、快速地增压-微波消解。通过一系列研究获得了含难溶矿物(含铌钽铀矿物、锆石等)岩石样品的微波-增压消解条件参数,然后采用电感耦合等离子体质谱(ICP-MS)法测定含难溶矿物岩石样品中微量元素含量。经标准物质测试验证,分析方法的定量限为0.004~0.084μg/g,精密度小于5%,测量相对误差小于10%,该方法能满足行业分析测试质量的控制要求。 相似文献
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样品用王水微波消解浸提,氢化物发生-原子荧光光谱法测定茶园土壤中痕量铅的含量。对样品浸取方法、实验条件、增感剂和共存元素进行了条件实验。结果表明,王水微波消解浸取,铅浸出量最大,减少了试剂用量和环境污染;铁氰化钾-盐酸羟胺体系有显著的增感作用,铁氰化钾在配制溶液时用米糠除去试剂中可能存在的铅,降低了空白;钴、锌、砷、镉等共存离子不干扰铅的测定,通过加入邻菲啰啉-硫氰酸钠消除铁和铜的干扰,提高了铅的回收率。方法检出限为0.65 μg/L,精密度(RSD,n=10)为1.89%,回收率在86.8%~110.4%之间。用土壤标准物质验证,测定值与标准值相符,方法快速准确,适合于大批量样品的分析检测。 相似文献
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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
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
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稀土元素因其用途广泛,已经得到了越来越多的关注,被应用于各个行业。研究表明,稀土元素对作物的光合作用、产量、抗逆、品质、发育和养分吸收等具有重要作用。作物中的稀土元素主要来自对土壤中稀土元素的吸收,因此,有效分解并快速测定土壤中的稀土元素,可以合理指导稀土元素的施用,对作物的生长和土壤的营养状况具有重要作用。本文比较了敞口酸溶、密闭消解、微波消解和碱熔等4种消解样品前处理方法,最终确定采用微波消解-电感耦合等离子体质谱法(ICP-MS)快速测定土壤中的稀土元素,并通过优化微波消解的条件,选择合适的试剂用量、消解温度、消解时间,对方法的检出限、精密度、准确度、回收率进行了实验,结果显示其测定均值与标准值基本吻合,相对误差(RE)绝对值为0.16%~3.39%,精密度为0.27%~5.09%,均小于10%,加标回收率为93.1%~106.0%。该方法准确度高、稳定性好,可以有效地应用于土壤中稀土元素的分析测定。 相似文献
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Gilles Serge Odin 《Comptes Rendus Geoscience》2002,334(6):409-414
Lithostratigraphy, physicochemical stratigraphy, biostratigraphy, and geochronology of the 77–70 Ma old series bracketing the Campanian–Maastrichtian boundary have been investigated by 70 experts. For the first time, direct relationships between macro- and microfossils have been established, as well as direct and indirect relationships between chemo-physical and biostratigraphical tools. A combination of criteria for selecting the boundary level, duration estimates, uncertainties on durations and on the location of biohorizons have been considered; new chronostratigraphic units are proposed. The geological site at Tercis is accepted by the Commission on Stratigraphy as the international reference for the stratigraphy of the studied interval. To cite this article: G.S. Odin, C. R. Geoscience 334 (2002) 409–414. 相似文献
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正1 Introduction Geological studies established on several sections in Lanping-Simao basin have shown that the salt-bearing strata of Mengyejing formation(Yunlong Fm.in Lanping basin)are constituted by an alternation of salt layers and interbedded facies.The latter consists mainly of mudstones,and mudstone-rich conglomerate.The mineralogy and geochemistry of salt-bearing beds and 相似文献
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正On 22nd April 2014,with the approach of the 45th World Earth Day,China’s Ministry of Land and resources issued the status of China’s mineral resources in 2013.The first task of the prospecting breakthrough strategy action implemented in the last five years has been completed,and China’s security capacity for mineral resources has been significantly improved.In the 相似文献
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正There are more than 700 salt lakes with area of more than 1km2 on the Qinghai-Tibet Plateau of China.In recent years,an oilfield brine was also found in the Nanyishan Section of Qaidam Basin in the Qinghai-Tibet 相似文献
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正1 Introduction Physical and numerical models are constructed to investigate the evolution and mechanism of salt migration driven by tectonic processes.In recent years,we have designed and ran series of models to simulate salt 相似文献
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YUAN Qin LI Jianguo QIN Zhanjie WEI Haicheng SHENG Shurong SHAN Fashou 《《地质学报》英文版》2014,88(Z1):276-276
正The study of Cretaceous-Palaeogene salt-bearing strata of the Khorat Basin Laos and the Lanping-Simao Basin in Yunnan,China has an great significance not only in explaining the basin evolution and the genesis of potash 相似文献
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正Potash is one of the long-term scare deposits in China,and potash prospecting has long been listed as a key brainstorm project for our nation and geological prospecting units.There have been considerable studies in search for potash deposits in the Kuqa depression of the Tarim basin(Jackson et al.,1991;Gemmer et al.,2004;Vendeville,2005;Vendeville and Jackson,1992a,1992b), 相似文献
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正1 Introduction Qaidam Basin in Qinghai,including 43 salt lakes with multiple dominant mineral such as potassium,magnesium,lithium etc.,is the most intensive distribution of Saline 相似文献