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蒸气收集脉冲进样流动注射氢化物发生—原子荧光法测定痕量梯 总被引：3，自引：0，他引：3
研究了流动注射氢化物发生－原子荧光测定矿石中Ｓｂ的方法，提出用蒸气收集脉冲进样技术，较大地提高了氢化物发生法的灵敏度和检测能力，标准参考样品的分析结果与推荐植吻合，精密度和检出限分别为５．１％（８ｍｇ／ｍｌ，ｎ＝９）和０．１９ｎｇ／ｍｌ，测定速度为１２０样／ｈ。 相似文献
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文章介绍石英缝管原子捕集技术在氢化物－火焰原子吸收光谱法测定Ｂｉ中的应用。采用自制的无载气氢化物发生装置，对实验条件进行了最佳化。实验结果表明，原子捕集技术的应用使氢化物－火焰原子吸收法的灵敏度提高２．２倍；方法检出限达２．５ｎｇ；２０ｎｇ／ｍｌＢｉ的标准溶液１０次测定的ＲＳＤ为２．９％。方法用于地质标样中微量Ｂｉ的测定，结果与推荐值符合。 相似文献
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锆—槲皮素—EDTA三元混配络合荧光体系的研究及其应用 总被引：6，自引：0，他引：6
在弱碱性条件下，ＥＤＴＡ与Ｚｒ（Ⅳ），槲皮素发生三元混配络合反应，形成组成比为２：１：３的锆－槲皮素－ＥＤＴＡ混配荧光络合物，由此建立了锆的选择性较好，灵敏度较高的荧光测定方法。该法测定Ｚｒ（Ⅳ）的线性范围为０．１８－３．６５μｇ／ｍｌ，方法检测限达３．５ｎｇ／ｍｌ。将此法用于直接测定合金样中的锆，结果令人满意。 相似文献
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探讨在十二烷基磺酸钠（ＳＬＳ）存在下，铟（Ⅱ）与桑色素的荧光反应。在ＰＨ为１．７１的ＨＣｌ－ＮａＡｃ缓冲溶液中，ＳＬＳ对铟（Ⅱ）－桑色素荧光反应有很强的增敏作用。铟的检测限可达６．９ｎｇ／ｍｌ，铟在（０－０．８）μｇ／ｍｌ范围内符合比耳定律，用适当的分离方法消除干扰离子后，可用于纯锡和纯锌中微量铟的测定。 相似文献
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探讨了各种类型的表面活性剂对Ｓｃ－铜铁试剂体系的增敏效应；观察到在ｐＨ９．０的ＮＨ＿４ＯＨ－ＮＨ＿４Ｃｌ缓冲介质中，溴化十四烷基三甲铵使该体系催化波灵敏度提高了２５倍。峰电位在－１．５０Ｖ（ｕｓ．Ａｇ／ＡｇＣｌ），峰高与Ｓｃ浓度在２～４０ｎｇ／ｍｌ呈线性关系，检出限１ｎｇ／ｍｌ；用拟定的方法测定了岩石样品中的痕量Ｓｃ；并对其极谱性质和表面活性剂增敏机理进行了探讨。 相似文献
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在０．００２％溴化十四烷基三甲铵（ＴＴＭＡＢ）－２０％ＨＣＩ体系中，Ｓｎ有一灵敏的吸附波，峰电位在－０．４７Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ），线性范围２～１０００ｎｇ／ｍｌ。体系可用于岩石、土壤样品中微量Ｓｎ测定；机理研究表明，溴化一四烷基三甲铵通过诱导吸附ＳｎＣｌ提高测定的灵敏度。 相似文献
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邻硝基苯基萤光酮－溴化十六烷基三甲铵二阶导数光度法同时测定微量钨和钼 总被引：1，自引：0，他引：1
研究了邻硝基苯基萤光酮（ｏ－ＮＰＦ）－溴化十六烷基三甲铵（ＣＴＭＡＢ）与Ｗ（Ⅵ）和Ｍｏ（Ⅵ）共同显色条件及其吸收光谱和导数光谱行为。选择二阶导数光谱用基线相交法同时测定Ｗ和Ｍｏ，对１：１０或１０：１的Ｗ和Ｍｏ互不干扰，回收完全。测定范围为４～１６０ｎｇ／ｍｌ的Ｗ，４～１２０ｎｇ／ｍｌ的Ｍｏ。对１０￣（－６）水平的Ｗ和Ｍｏ测定的ＲＳＤ（ｎ＝８）均小于１０％，对国家一级地质标样测定结果符合要求。 相似文献
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在０．００２％溴化十四烷基三甲胺（ＴＴＭＡＢ）－２０％ＨＣｌ体系中，Ｓｎ有一灵敏的吸附波，峰电位在－０、４７Ｖ（ｖｓ．Ａｇ／ＡｇＣｌ），线性范围２～１０００ｎｇ／ｍｌ。体系可用于岩石、土壤样品中微量Ｓｎ测定；机理研究表明，溴化十四烷基三甲铵通过诱导吸附ＳｎＣｌ＾２－４提高测定的灵敏度。 相似文献
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油菜籽品质及重金属污染程度直接关系到人类健康,对油菜籽中As、Sb、Cd和Tl等有毒元素含量进行监测有助于对食用油生产原材料的提前监控。避开强酸消解前处理的繁琐,为了实现快速测定菜籽中As、Sb、Cd和Tl等易挥发有毒元素的准确含量,以及解决粮油食品脂肪含量高对前处理的挑战,本文采用一种悬浮-乳化协同制样技术,详细考察了影响悬浮-乳化的诸多条件,制得均匀稳定的悬浮-乳化试液(Slurry-Emulsion Solution, SES)体系。在进样效率高的电热蒸发器(ETV)中,优化程序升温参数和改进剂硝酸钯的用量,SES直接进样,采用电感耦合等离子体质谱(ICP-MS)测定了油菜籽中As、Sb、Cd和Tl。该方法对As、Sb、Cd和Tl的相对标准偏差(RSD)分别为10.1%、8.8%、8.9%、6.4%[c=0.5%(m/V),n=5]。在最佳实验条件下,As、Sb、Cd和Tl检出限(3σ)分别为40.0ng/L、20.0ng/L、50.0ng/L和10.0ng/L,对应原始固体样品的检出限(3σ)分别为8.0ng/g、4.0ng/g、10.0ng/g和2.0ng/g。菜籽样品中As... 相似文献
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采用Luminol－H。O。Air（巨）化学发光反应体系作为分析检测方法，建立了一个测定地质样品中痕量锑的化学发光分析法。方法的原理是用AgNO。吸收由样品发生的氢化锑气体，使吸收液中生成Sb（巨）与过量的K。Cr。O，反应生成Cr（1），方法的检出限为0．6us／mlSb，工作曲线的线性范围是2～1000ng／mlSb，测定的相对标准偏差小于5％。本方法已用于地质样品中痕量佛的测定。 相似文献
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提出了一种氢化物发生—原子荧光光谱法测定地质样品(水系沉积物)中Sb(Ⅲ)和Sb(Ⅴ)的方法.选取4.8 mol/L HC1为提取剂,采用超声波辅助提取,以6 g/mL柠檬酸钠作为Sb(Ⅴ)的掩蔽剂,在0.24 mol/L的HC1介质中选择性测定Sb(Ⅲ),用差减法求得Sb(Ⅴ).Sb(Ⅲ)的方法检出限为0.075×10-6,Sb(Ⅴ)的方法检出限为0.097×10-6.对40 ng/mL的Sb(Ⅲ)和Sb(Ⅴ)分别连续测定11次,得到相对标准偏差分别为1.1％和0.64％.应用该方法对地质样品中的Sb(Ⅲ)和Sb(Ⅴ)进行分析测定,并与王水溶解值相比较,该方法测定的总Sb提取率在80％以上,Sb(Ⅲ)和Sb(Ⅴ)的加标回收率分别为83％ ～ 107％和98％ ～ 114％. 相似文献
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We have developed a rapid and accurate method for the determination of Mo, Sb and W in geological samples using isotope dilution inductively coupled plasma-mass spectrometry with a flow injection system (ID-FI-ICP-MS). The chemical procedure requires HF digestion of the sample with a Mo-Sb-W mixed spike, subsequent evaporation and dissolution of Mo, Sb and W from Mg and Ca fluorides with HF. Recovery yields of Mo, Sb and W in the extraction were > 94% for samples of peridotite, basalt and andesite composition, with the exception of W in samples of peridotite composition for which recovery was 81%. No matrix effects were observed in the determination of the isotope ratios of Mo, Sb and W in solutions prepared from peridotite, basalt and andesite samples down to a dilution factor of 100. Detection limits of Mo, Sb and W in silicate materials were at the several ng g−1 level. Analysis of the silicate reference materials PCC-1, DTS-1, BCR-1, BHVO-1, AGV-1 from the US Geological Survey and JP-1, JB-1, -2, -3, JA-1, -2, and -3 from the Geological Survey of Japan as well as the Smithsonian reference Allende powder yielded reliable Mo, Sb and W concentrations. The repeatability in the analysis of basalts and andesites was < 9%. This technique requires only 0.2 ml sample solution, and is therefore suitable for analyzing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. 相似文献
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本法采用改装后的日立HFS-2型氢化物发生器和两种自制T型石英管与原子吸收光谱仪主机配合。以积分方式进行测量,使操作简化,节约试剂,扩大了线性范围.用本法一次取样后,加入选定的混合还原抑制剂,可连续测定地质样品中痕量砷、锑、铋.其检出限分别为0.33,0.80,0.41ng/ml,相对标准偏差小于6％. 相似文献
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Benjamin M. Moreton Jean-Michel Fernandez Mathieu B.D. Dolbecq 《Geostandards and Geoanalytical Research》2009,33(2):205-218
An iminodiacetate chelating resin was optimised for the rapid determination of Co, Cu, Fe, Mn and Ni in seawater. Using inexpensive, high-capacity, reusable cartridges allowed high flow rates of up to 25 ml min−1 . High preconcentration factors, of up to 500, were obtained in order to analyse samples using an ICP-OES. The requirement for a buffer was eliminated due to the high tolerance of the ICP-OES to interfering matrix elements, thereby further reducing the potential for contamination. Quantification limits in seawater were: Co = 6 ng l−1 , Cu = 8 ng l−1 , Fe = 6 ng l−1 , Mn = 5 ng l−1 and Ni = 6 ng l−1 . The method was verified by the analysis of near shore seawater (CASS-4) and open ocean seawater (NASS-5) reference materials. In order to satisfy the high sampling demands using the iminodiacetate cartridges, a portable off-line preconcentration unit was developed for routine analysis. The multi-channel preconcentration unit, was capable of treating up to eight samples simultaneously with concentrating times as little as 30 minutes. The technique was also used to determine dissolved metals in fresh and interstitial waters. The technique has been successfully used in a number of environmental studies and impact assessments to evaluate the effects of mining on the New Caledonian lagoon. 相似文献
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A method for the determination of Ge, As, Se and Te in silicate samples using isotope dilution-internal standardisation (ID-IS) octopole reaction cell (ORC) ICP-QMS by normal sample nebulisation was developed. The method does not involve either hydride generation or ion exchange. Germanium, Se and Te were determined by isotope dilution (ID), and As was determined by ID-IS. A silicate sample with an added Ge-Se-Te spike was digested with an HF-HNO3 -HBr mixture, dried, re-dissolved with HF and the supernatant liquid was directly aspirated into an ORC-ICP-QMS instrument with He or H2 gas. No matrix effects were observed down to a dilution factor (DF) of ∼ 70 for Ge, Se and Te and DF of ∼ 1000 for As, which resulted in 3s detection limits in silicates of 2, 1, 0.1 and 4 ng g−1 , respectively. Advantages of the method are the simple sample introduction as well as a capability of determining S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by ID-IS-ICP-QMS/SFMS from the same solution. Furthermore, the total sample solution consumption was only 0.253 ml with DF = 2000. Therefore, only a 0.13 mg test portion was required. To demonstrate the applicability of this technique, Ge, As, Se and Te in eight silicate reference materials were determined, as well as S, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta in four carbonaceous chondrites. 相似文献
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氢化物发生-原子荧光光谱法测定土壤中水溶态和可交换态锑(Ⅲ)和锑(Ⅴ) 总被引：2，自引：2，他引：0
在0.10 mol/L酒石酸介质中,采用氢化物发生-原子荧光光谱法测定土壤中水溶态和可交换态Sb(Ⅲ)和Sb(Ⅴ)。以氢气发生器为氩-氢火焰提供氢气,明显降低了硼氢化钾浓度,改善了测定检出限。考察了酒石酸掩蔽Sb(Ⅴ)的量及共存干扰元素的允许量。方法检出限Sb(Ⅲ)为0.026 ng/L,总Sb为0.019 ng/L。加标回收试验表明,方法准确、可靠。 相似文献
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Masanori Kurosawa Simon E. Jackson Shigeho Sueno 《Geostandards and Geoanalytical Research》2002,26(1):75-84
Fifty elements in NIST SRM 614 and 616 glass reference materials were determined by laser ablation microprobe-inductively coupled plasma-mass spectrometry (LAM-ICP-MS). The values determined for NIST SRM 614 agreed well with the NIST-certified and information values (mean relative difference ± 3.6%), except for B, Sc and Sb. The values determined for NIST SRM 616 agreed with the NIST-certified and information values within a mean relative difference of ± 1.5%, except for B, Sc and Ga. In addition, at an 80 μm sampling scale, NIST SRM 614 and 616 glass discs were homogeneous for trace elements within the observed precisions of 5 and 15% (mean), respectively. Detection limits were in the range 0.01 - 0.3 μg g−1 for elements of lower mass numbers (amu < 80) and 1 - 10 ng g−1 for heavy elements (amu > 80). Detection at the sub ng g−1 level is possible for most of the heavy elements by using an ablation pit size larger than 10 0 μm. 相似文献
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Zongshou Yu Philip Robinson Ashley T. Townsend Carsten Mnker Anthony J. Crawford 《Geostandards and Geoanalytical Research》2000,24(1):39-50
Six low abundance rock reference materials (basalt BIR-1, dunite DTS-1, dolerite DNC-1, peridotite PCC-1, serpentine UB-N and basalt TAFAHI) have been analysed for high field strength elements (Zr, Nb, Hf, Ta, Th and U), Rb, Sr, Mo, Sb, Cs, Tl and Bi at ng g−1 levels (in rock) by magnetic sector inductively coupled plasma-mass spectrometry after HF/HClO4 high pressure decomposition. The adopted method uses only indium as an internal standard. Detection limits were found to be in the range of 0.08 to 16.2 pg ml−1 in solution (equivalent to 0.08 to 16.2 ng g−1 in rock). Our data for high field strength elements, Rb, Sr, Mo, Sb, Cs, Tl and Bi for the six selected low abundance geological reference materials show general agreement with previously published data. Our Ta values in DTS-1 and PCC-1 (1.3 and 0.5 ng g−1 ) are lower than in previously published studies, providing smooth primitive mantle distribution patterns. Lower values were also found for Tl in BIR-1, DTS-1 and PCC-1 (2, 0.4 and 0.8 ng g−1 ). Compared with quadrupole ICP-MS studies, the proposed magnetic sector ICP-MS method can generally provide better detection limits, so that the measurement of high field strength elements, Rb, Sr, Mo, Sb, Cs, Tl and Bi at ng g−1 levels can be achieved without pre-concentration, ion exchange separation or other specialised techniques. 相似文献