半导体级高纯双氧水中痕量杂质元素的检测

用高分辨电感耦合等离子体质谱测定半导体级高纯双氧水中的痕量金属杂质,用直接稀释法,把高纯双氧水稀释10倍后,用标准加入法进行上机检测,前处理简单、快速,避免了在样品前处理时的污染问题。高分辨电感耦合等离子体质谱可以消除多分子离子干扰,降低检出限,提高定量准确性。方法的检出限为0.34~15.36 ng/L,加标法回收率为90.1%~102.5%。方法简单,结果可靠,适用于高纯双氧水中痕量元素的快速测定。     

半导体级高纯氨水中痕量杂质元素的检测

用高分辨电感耦合等离子体质谱测定半导体级高纯氨水中的痕量金属杂质,用直接稀释法,把高纯氨水稀释10倍后,用标准加入法进行上机检测,前处理简单、快速,避免了在样品前处理时的污染问题。高分辨电感耦合等离子体质谱可以消除多分子离子干扰,降低检出限,提高定量准确性。该方法的检出限为0.31~14.4 ng/L,加标法回收率为91.5%~108.6%。该方法简单,结果可靠,适用于高纯氨水中痕量元素的快速测定。     

膜去溶进样高分辨ICP-MS测定半导体级硝酸中杂质元素

利用高分辨电感耦合等离子体质谱测定半导体级高纯硝酸中的痕量金属杂质,用膜去溶进样系统直接进样,用标准加入法进行上机检测,无需前处理,快速,避免了在样品前处理时的污染问题。高分辨电感耦合等离子体质谱可以消除多分子离子干扰,降低检出限,提高定量准确性。方法的检出限为0.69～23.73ng/L,加标回收率为88.2%～106.0%,方法简单,结果可靠,适用于高纯硝酸中痕量元素的快速测定。     

太阳能级多晶硅用三氯氢硅中金属杂质的检测方法

在洁净室里,采用在氩气保护下进行高纯三氯氢硅的挥发,然后用高纯酸溶解,用高分辨电感耦合等离子体质谱仪检测痕量金属杂质,方法的检出限为0.45~14.6 ng/kg,加标法回收率为89.6%~108.2%。前处理简单、快速,避免了在样品前处理时的污染问题,检测结果准确可靠。     

高纯氨中金属颗粒杂质检测方法

通过蒸发捕集法与溶液吸收法两种前处理方法,利用高分辨电感耦合等离子体质谱对高纯氨中痕量金属杂质进行上机检测。实验表明,双聚焦磁质谱对稀氨水中金属杂质方法检出限低达10-12级,对高纯氨中金属杂质方法检测限低于1×10-9 m/m。方法便捷、准确,容易避免前处理污染,可以作为高纯氨中金属杂质检测的有效手段。     

电感耦合等离子体质谱在长寿命放射性核素分析中的应用

电感耦合等离子体质谱(Inductively Coupled Plasma Mass Spectrometer,ICP-MS)具有灵敏度高、检出限低、线性动态范围宽和可以进行多元素同时测定及同位素比测量等优点,是一种具有广阔前景的痕量(超痕量)无机多元素分析技术。ICP-MS检测半衰期大于几百年的放射性核素优于放射计数测量方法,用ICP-MS检测环境样品中痕量放射性核素,成为研究的热点。本文从长寿命放射性核素含量测定、同位素比测量及环境科学研究等方面对电感耦合等离子体质谱在放射性核素分析中的应用作了评述。     

微波消解-电感耦合等离子体-质谱(ICP-MS)测定木制食品接触材料中有害重金属

采用微波消解法处理木制食品接触材料,优化电感耦合等离子体质谱检测参数,建立木制食品接触材料中Sb、As、Cd、Cr金属元素的微波消解-电感耦合等离子体质谱的分析方法.对所测定元素,标准曲线相关系数为0.9999,方法的检出限为0.08～0.22μg/L,RSD＜5%,平均加样回收率84.9%～97.2%.方法准确可靠,可用于实际样品分析.     

光纤用四氯化硅中金属杂质的检测方法

在洁净室里采用加热挥发的前处理方法制备光纤用四氯化硅样品,用高分辨电感耦合等离子体质谱仪(HR-ICP-MS)测试金属杂质含量,可以有效地提高各元素的分辨率,降低检出限,用加标回收的方式计算回收率在85.1-115.4之间。     

电感耦合等离子质谱法测定石英砂中十四种痕量杂质元素

文章根据不同石英砂的矿相、加工工艺,建立了密闭消解和微波消解等样品处理方法,利用电感耦合等离子体质谱仪（ICP-MS）对石英砂中痕量杂质元素进行检测。采用Sc为内标补偿基体效应和仪器漂移。检测结果表明,密闭酸溶法与微波消解法无显著性差异（P≥0.05）;ICP-MS检测石英砂中痕量杂质元素准确度和精确度高,检测线性范围宽,检出限低,分析快速。测定结果的相对标准偏差（RS D）0.2%～5.0%,检出限为0.009～0.093 ng/ml。     

ICP-MS测定有机肥中的氧化钾

本文讲述了ICP-MS测定有机肥中氧化钾含量,试验用电感耦合等离子体质谱(ICP-MS)法和火焰光度法比较测定有机肥中氧化钾的含量。其结果表明,ICP-MS法与原子吸收火焰光度法相比,本法灵敏度高,检出限低,用时少,效率高,数据准确可靠等优点,可满足检验分析要求。     

电感耦合等离子体原子发射光谱法同时测定生铁中硅锰磷砷锑锡

本文研究了电感耦合等离子体原子发射光谱法(ICP-OES)同时测定生铁中常量元素磷、锰、硅及痕量元素砷、锑、锡。用盐酸-硝酸混合酸溶解试样,选择了各元素的合适分析谱线,在最佳工作条件下,测得磷、锰、硅、砷、锑、锡的检出限分别为0.0042%、0.0003%、0.0009%、0.0024%、0.0033%、0.0021%,相对标准偏差(n=10):常量元素磷、锰、硅及痕量元素砷的RSD小于2%,痕量元素锑和锡的RSD小于10%。本方法用标准物质进行测定,测定结果与认定值吻合。     

Use of plasma atomic emission spectrometry for the quality control of grade lead

An inductively coupled plasma atomic emission spectroscopy method for speciation of Ag, Cu, Bi, Sb, As, Ni, Cd, Zn, Sn, and Fe in grade lead is described. The spectrometer was calibrated using water solutions with known concentrations of trace elements. The matrix effects were taken into account using an internal standard added to the reference-sample, calibrated-blank, reagent-blank, and tested-sample solutions. The metrological examination of the technique was accomplished. The repeatability rms error does not exceed 0.10. The systematic error is not statistically significant.     

海芒果树叶中氨基酸和微量元素的分析

采用高效液相色谱法和等离子发射光谱法,分析测定了红树植物海芒果Cerberamanghas树叶中氨基酸和微量元素成分。结果表明,叶子提取液中含有16种氨基酸,其中6种为必需氨基酸,2种为半必需氨基酸,其中必需氨基酸占总氨基酸的33.20%;15种微量元素,分别为Al、As、Ba、Ca、Cd、Cr、Cu、Fe、Mg、Mn、Ni、Pb、Sr、Ti、Zn。     

红树木榄胚轴基本化学组分研究

对红树植物木榄胚轴中的水分、灰分、灰分中的酸不溶物和硫化物、粗脂肪、粗蛋白及氨基酸和微量元素等一系列物质组分进行了系统的分析测定。结果显示:木榄胚轴中水分64.97%、灰分0.78%、灰分中酸不溶物0.0125%、灰分中硫化物化物0.2038%、粗脂肪0.9143%、粗蛋白3.43%;由木榄胚轴中测得了16种氨基酸,其总含量为25.005ug/g,其中人体必须氨基酸7种,占所含氨基酸总量约7.9%;在木榄胚轴中检测到了砷、钴、铬、铜、铁、镁、锰、镍、铅、硒、钛、钡、锶等13种元素,并测得了含量。     

交换柱富集-ICP等离子光谱法测定岩矿中痕量稀土元素

本文应用强酸阳离子树脂交换柱富集稀土元素,ICP等离子光谱法测定各稀土元素含量。文中对采用交换型选取,仪器工作条件,共存元素的干扰及消除等方面进行探讨。实验表明,该方法操作简便,RSD小于1%,样品测定回收率在90%～115%。     

Evaluation of the emission characteristics of trace metals from coal and fuel oil fired power plants and their fate during combustion

Coal as well as fuel oil combustion generates emissions of potentially toxic trace pollutants including organic and inorganic chemical compounds besides major pollutants. A study on As, Cd, Co, Cr, Cu, Hg, Fe, Mn, Ni, Pb, Se, and Zn emissions from a 220 MW coal-fired power plant equipped with a electrostatic precipitators (ESPs) and 6 MW oil fired-power plant was carried out, using stack monitoring kit, Envirotech APM 620, which is similar to EPA Method 29. Simultaneous sampling of coal, fuel oil, oil waste, bottom ash, fly ash, flue gases, and particles associated with the gas phase has been performed. This sampling method was used for trace metal sampling. The content of all these metals in coal, oil, oil waste, bottom ash, fly ash have been determined by XRF, whereas their contents in the flue gases, and particles associated with the gas phase has been analyzed with ICP-AES. The mass balances obtained for trace elements were satisfactory in case of fuel oil based power plant, whereas in case of coal fired power plant, the mass balance for all the trace elements were below 50% except for the As, Se, and Hg. The enrichment factors for all trace metals was <1 in both cases. The above sampling method is moderately adequate method for trace element sampling in coal as well as oil fired power plants except for Hg. The results indicate that trace metals emissions were higher in coal-based power plant than the fuel oil-fired power plant.     

ICP-AES法测定锂离子电池电解液中金属杂质元素

采用电感耦合等离子体发射光谱仪(ICP-AES)同时测定六氟磷酸锂电解液中钠、钾、钙、铁、铜、铬等多种元素,回收率在97.3%～104.1%之间,线性相关系数大于0.999,相对标准偏差在0.02%～0.66%。该方法分析速度快,灵敏度高,重现性好,适合六氟磷酸锂电解液中杂质元素的检测。     

ICP-AES analysis of silicon,germanium, and their oxides

The techniques of atomic emission spectrometry with inductively coupled plasma (ICP-AES) for quantitative determination impurities in silicon, germanium, and their dioxides are developed. Analytical lines for silicon-matrix (29 trace elements) and germanium-matrix (42 trace elements) are selected. Matrix interferences caused by the presence of silicon and germanium in the solutions are studied. The optimal concentrations of matrix are determined. LODs for trace elements are in the range from n × 10^–7 to n × 10^–5 wt %; RSD < 20%. The accuracy of the results is confirmed by the method of “introduced–found.” The developed techniques are express, simple, and can determine a broad range of trace elements.     

Multiple stirred-flow chamber assembly for simultaneous automatic fractionation of trace elements in fly ash samples using a multisyringe-based flow system

There is a current trend in automation of leaching tests for trace elements in solid matrixes by use of flow injection based column approaches. However, as a result of the downscaled dimensions of the analytical manifold and execution of a single extraction at a time, miniaturized flow-through column approaches have merely found applications for periodic investigations of trace element mobility in highly homogeneous environmental solids. A novel flow-based configuration capitalized on stirred-flow cell extraction is proposed in this work for simultaneous fractionation of trace elements in three solid wastes with no limitation of sample amount up to 1.0 g. A two-step sequential extraction scheme involving water and acetic acid (or acetic acid/acetate buffer) is utilized for accurate assessment of readily mobilizable fractions of trace elements in fly ash samples. The fully automated extraction system features high tolerance to flow rates (< or = 6 mL min(-1)) and, as opposed to operationally defined batchwise methods, the solid to liquid ratio is not a critical parameter for determination of overall readily leachable trace elements provided that exhaustive extraction is ensured. Analytical performance of the dynamic extractor is evaluated for fractionation analysis of a real coal fly ash and BCR-176R fly ash certified reference material. No significant differences were found at the 0.05 significance level between summation of leached concentrations in each fraction plus residue and concentration values of BCR-176R, thus revealing the accuracy of the automated method. Overall extractable pools of trace metals in three samples are separated in less than 115 min, even for highly contaminated ashes, versus 18-24 h per fraction in equilibrium leaching tests. The multiple stirred-flow cell assembly is thus suitable for routine risk assessment studies of industrial solid byproduct.