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用新型氢化物发生喇叭口Ⅱ型同心雾化器替代Meinhard同心雾化器,溶液雾化为气溶胶和氢化物发生反应生成氢化物气体就可以在雾化系统中同时进行,选用L-巯基丙氨酸(L-cysteine)和硫脲(thiourea)作为基体铜的掩蔽剂,无需分离基体铜,实现了电感耦合等离子体原子发射光谱(ICP-AES)同时测定纯铜样品中氢化物和非氢化物形成元素的目的。研究了酸度、NaBH4的浓度、载气流速及清洗时间对氢化物形成元素的影响,考察了铜基体对氢化物形成元素的化学干扰情况。用本方法测定了纯铜标准样品(NIST SRM400),结果令人满意。在1000mg/L纯铜样品溶液中,其氢化物形成元素As、Bi、Sb、Sn、Se和Te的检出限分别为0.08、0.15、0.10、0.17、0.21和0.23μg/L。 相似文献
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The precision of isotopic measurements of Pb by thermal ionization mass spectrometry (TIMS) is limited by the fact that this element does not possess an invariant isotope ratio that can be used for the correction of mass fractionation by internal normalization. Multiple-collector inductively coupled plasma mass spectrometry (MC-ICPMS) can overcome this limitation, because with plasma ionization, elements with overlapping mass ranges are thought to display identical mass discrimination. With respect to Pb, this can be exploited by the addition of Tl to the sample solutions; the mass discrimination factor obtained for Tl can then be used for the correction of the measured Pb isotope ratios. In this article we present the results of a detailed study that investigates the accuracy and precision of such an external correction technique for mass discrimination based upon the results of multiple analyses of a mixed standard solution of NIST SRM-981 Pb and SRM-997 Tl. Our data indicate that normalization of the Pb isotope ratios to the certified isotopic composition of SRM-997 Tl produces Pb isotopic results that are significantly lower than recently published reference values by TIMS. This systematic offset can be eliminated by renormalization of the Pb data to a different Tl isotopic composition to obtain an empirically determined mass discrimination factor for Pb that generates accurate results. It is furthermore shown that a linear law is least suited for the correction of mass discrimination, whereas a power or exponential law function provide significantly more accurate and precise results. In detail, it appears that a power law may provide the most appropriate correction procedure, because the corrected Pb isotope ratios display less residual correlations with mass discrimination compared to the exponentially corrected data. Using an exponential or power law correction our results, obtained over a period of over seven months, display a precision (2σ) of better than 60 parts per million (ppm) for 208Pb/206Pb and 207Pb/206Pb and of better than 350 ppm for 206Pb/204Pb, 207Pb/204Pb/204Pb, and 208Pb/204Pb. This represents a significant improvement compared to conventional TIMS techniques and demonstrates the potential of MC-ICPMS for routine, high-precision measurements of Pb isotopic compositions. 相似文献
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河口水体中痕量稀土元素的共沉淀预富集-电感耦合等离子体质谱法测定研究 总被引:3,自引:0,他引:3
建立了氢氧化铟共沉淀预富集 -电感耦合等离子体质谱法测定河口水体中痕量稀土元素的方法。实验结果表明 ,在80mg·L -1的In3 +和pH9.5的实验条件下 ,在1.0L水样中添加5.0~200.0ng的混合稀土标准溶液 ,均能定量回收 ,回收率在82.2 %~106.9 %之间。方法的分析流程空白为0.04(Tb)~10.17(La)ng·L -1,检出限在0.17(Yb)~1.46(La)ng·L-1之间 ,精密度 (RSD ,n=3)小于11.7 % ,可满足河口淡水和海水样品中的痕量稀土元素定量分析的要求 相似文献
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Himadri Paul Sumit Bhaduri Goutam Kumar Lahiri 《Journal of organometallic chemistry》2004,689(2):309-316
Fumed silica, silica gel, silica-alumina and cross-linked (5.5%) polystyrene have been functionalized with quaternary ammonium groups and the Chini cluster [Pt12(CO)24]2− has been anchored onto these functionalized materials by ion pairing. A catalyst has also been prepared by the adsorption of Na2[Pt12(CO)24] on unfunctionalized fumed silica. The catalytic activities of the resultant materials, and that of commercially purchased 5% platinum on alumina have been studied for the hydrogenation of a variety of unsaturated compounds. The substrates studied are: α-acetamidocinnamic acid, cyclohexanone, acetophenone, methyl pyruvate, ethyl acetoacetate, nitrobenzene and benzonitrile. Compared to the polystyrene supported catalyst, the inorganic oxide supported catalysts have higher surface areas and for most of the substrates have notably higher activities. The functionalized fumed silica-based catalyst gives higher conversions than functionalized silica gel and silica-alumina-based catalysts. In the hydrogenation of acetophenone and ethyl acetoacetate, the functionalized fumed silica-based catalyst show superior activity compared to the commercial platinum catalyst, and the catalyst made by conventional adsorption method. In benzonitrile hydrogenation with all the cluster-derived catalysts a hydrazine derivative is selectively formed, but when the commercial platinum catalyst is used benzyl amine is the main product. 相似文献