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Development of Electrothermal Vaporization/ICP-MS for Microtrace Analysis

用于微量分析的电热汽化/ICP-MS 的开发

基本信息

批准号：
13650868
负责人：
TANAKA Tomokazu
金额：
$ 2.18万
依托单位：
Nagoya University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (C)
财政年份：
2001
资助国家：
日本
起止时间：
2001 至 2002
项目状态：
已结题

项目摘要

A detachable sample-injector with a coiled tungsten filament was constructed for the effective introduction of tiny amounts of sample into ICP-MS. A 5 μl volume of the sample was placed on a filament and an injector was inserted into a plasma torch. After desolvating the sample, the filament was electrically heated. The resulting vapor was transferred to the plasma for the determination of As and Se. The signal intensities increased by almost 100 times as compared with the values in a previous study, where a looped tungsten filament was heated outside the plasma torch. The absolute detection limits were 0.5 pg for As and 1.1 pg for Se.The proposed method was applied to the determination of As and Se in certified reference human hair (5 mg). The analytical results were 0.29±0.03 μg g^1 for As and 1.8±0.2 μg g^1 for Se, which are in good agreement with the certified values (As 0.31±0.02 μg/g, Se 2.0±0.08 μg/g). The analysis was tried with 0.50-mg weight of the sample. The sample was deco … More mposed with 10 μl of 14 mol/l HNO_3 and 2 μl of 30% H_2O_2 in a PTFE high-pressure decomposition vessel. The resulting solution was mixed with 25 μl of 1 μmol/l KMnO_4 solution and evaporated to dryness. The residue was dissolved in 500 μl of 1 mol/l HNO_3. The addition of KMnO_4 to the sample was essential for the prevention of serious losses (30〜50%) of analytes during evaporation. The results (0.30±0.01 μg/g for As and 2.0 ± 0.2 μg/g for Se) agreed closely with the certified values.The proposed method was also applied to the determination of Se in high-purity copper (99.9999%). After the acid decomposition of a sample (200 mg), a 5 μl portion of the resulting solution was directly placed on a filament and the signal intensities of ^<82>Se+ were measured. Copper matrix, however, significantly decreased the signals and immediately deteriorated filaments. Copper in the sample solution was effectively removed by coprecipitation with iron hydroxide, and consequently, μg/g level of Se in the sample was successfully determined. Less

为了有效地将微量样品引入ICP-MS，我们构造了一个带有螺旋钨丝的可拆卸进样器。将5 μl样品置于灯丝上，将进样器插入等离子体炬中。在使样品去溶剂化之后，电加热细丝。将产生的蒸气转移到等离子体中用于测定As和Se。与先前的研究中的值相比，信号强度增加了近100倍，其中环形钨丝在等离子体炬外部加热。绝对检出限分别为0.5 pg的砷和1.1 pg的硒。所提出的方法适用于测定认证的参考人发（5 mg）中的砷和硒。分析结果为As 0.29±0.03 μg g^1、Se 1.8±0.2 μg g^1，与认证值（As 0.31±0.02 μg/g、Se 2.0±0.08 μg/g）一致。用0.50 mg重量的样品进行分析。样品是deco ...更多信息在聚四氟乙烯高压分解器中，加入10 μ l14 mol/lHNO_3和2 μ l30%H_2O_2。将所得溶液与25 μl 1 μmol/lKMnO_4溶液混合并蒸干。残渣溶于500 μl 1 mol/l HNO_3中。在样品中加入KMnO_4可防止蒸发过程中分析物的严重损失（30 ~ 50%）。测定结果（As为0.30±0.01 μg/g，Se为2.0 ± 0.2 μg/g）与认定值基本一致，该方法也用于高纯铜（99.9999%）中Se的测定。在样品（200 mg）的酸分解后，将5 μl所得溶液直接置于细丝上，并测量13 Se+的信号强度<82>。然而，铜基质显著降低了信号，并立即恶化细丝。用氢氧化铁共沉淀法有效地去除了样品中的铜，从而成功地测定了样品中μg/g的硒。少