共查询到19条相似文献,搜索用时 156 毫秒
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《理化检验(化学分册)》2010,(6)
提出了辉光放电原子发射光谱法测定钢中痕量硼的方法。对样品制备、仪器分析参数、干扰元素等影响因素进行了研究。选择波长为208.959 nm和249.326 nm的谱线为硼和内标铁的分析线。硼标准与内标谱线强度的比值与硼的质量分数呈线性关系,其线性回归方程I=4.775 5w+0.001 843。检出限为4.5×10-5%,应用此法分析了11种低合金钢标准样品,相对标准偏差(n=11)在3.7%~9.9%之间。 相似文献
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辉光放电原子发射光谱法快速分析生铸铁 总被引:3,自引:0,他引:3
通过对辉光光源参数-放电电流、放电电压、预溅射时间和分析时间对生铸铁标样放电强度和稳定性影响的研究,优化光源参数,建立了辉光放电原子发射光谱法同时测定生铸铁中碳、硅、锰、磷、硫等12个元素的快速分析方法。分析生铸铁试样时发现了不同灰口铸铁在碳分析结果方面存在偏差,对碳的偏差进行了讨论并通过制样条件和光源参数的调整可以有效地减小偏差。通过对不同生铸铁样品进行准确度和精密度试验,结果表明:分析结果与标准值或化学法结果一致。分析一件试样的时间仅需2~5 min。 相似文献
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建立了基于低温等离子体(Low temperature plasma)剥蚀系统将固体样品直接引入电感耦合等离子体质谱(ICP-MS)并用于电路板镀层中Au,Ni和Cu的深度分析.此实验中采用介质阻挡放电(DBD)方式产生低温等离子体探针,逐层剥蚀样品表面,由ICPMS检测元素信号.对DBD所用放电气体种类、外加电场功率、放电气体流速和采样深度等实验条件进行优化.在优化条件下,应用LTP-ICPMS在30 s内完成电路板镀层(20 μm Au/10 μm Ni/Cu基底)的逐层剥蚀和深度分析,元素种类和分层顺序与X射线光电子能谱(XpS)相吻合,镀层的分辨率可拓展至微米水平,表明此技术可直接用于固体样品的深度分析. 相似文献
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低温等离子体原子荧光光谱法直接测定固体样品中的汞 总被引:1,自引:0,他引:1
建立了低温等离子体(LTP)与原子荧光光谱仪(AFS)联用直接检测ABS固体样品中Hg的方法.实验采用介质阻挡放电(DBD)方式产生低温等离子体,剥蚀固体样品后产生的元素蒸气引入到原子荧光光谱仪进行检测.优化的实验条件为:DBD外接电源的放电功率为16~18 W,放电气体流速为400 mL/min;采样距离为1~5 mm;原子荧光光谱仪的原子化器高度为10 mm.本系统测定Hg的检出限为0.91 mg/kg,线性范围为91.5~1096 mg/kg;精密度(RSD,n=7)为1.9%~2.3%,并对标准样品以及实际样品进行测定,测定结果与标准值与ICPMS及CVG-AFS一致,表明本方法可作为直接检测固体样品的新型元素分析技术. 相似文献
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建立电感耦合等离子体发射光谱法(ICP–AES)测定辐照后硼铝复合材料中元素的方法。用氢氧化钠将辐照后的硼铝复合材料溶解过滤,滤纸和滤渣采用碱熔法制样。采用基体匹配法消除基体干扰,仪器工作条件:RF发生器功率为1 150 W,雾化器压力为151.7 kPa,辅助气流量为0.5 L/min,硼元素的分析线为249.678 nm,积分时间为5 s。硼的质量浓度在15~28 mg/L范围内与光谱强度呈良好的线性关系,线性相关系数为0.999 7。方法的回收率为99.1%~100.8%,测定结果的相对标准偏差为0.76%(n=10)。该方法快速,准确度和精密度高,能够满足样品测量需要。 相似文献
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三步离子交换方法用于粘土沉积物酸溶相中硼同位素测定 总被引:1,自引:0,他引:1
在采用酸溶法进行粘土沉积物中硼同位素组成测定时,大量存在的Al、Fe、稀土等元素在较高pH溶液中会形成能强烈吸附硼的氢氧化物沉淀,对硼的提取和硼同位素的测定产生较大影响.有效去除这些干扰元素一直是测定粘土沉积物酸溶相中硼同位素组成的瓶颈.本实验采用三步离子交换法萃取和纯化粘土沉积物中的硼,以AG 50W×8阳离子树脂柱去除所有能生成水不溶性氢氧化物的Al、Fe、稀土等元素,再采用Amberlite IRA 743硼特效树脂柱提取硼,最后采用Ion-exchangerⅡ与AG 50W×8组成的阴阳离子混合树脂柱进一步纯化硼提取液.结果表明,采用以上三步离子交换法提取粘土沉积物中硼的回收率高于90%,未观察到明显的硼同位素分馏,可满足粘土沉积物酸溶相中硼同位素组成高精度测定的需要. 相似文献
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杜双会 《理化检验(化学分册)》2013,(3):284-286,289
提出了采用光电直读光谱法测定轧制态碳钢中碳、硅、锰、磷、硫、镍、铬、铜、钼、钒、铌、铝、硼、钙、钛、钨、铅、砷、锡、锑、锌等21种元素的含量。测定中选择氩气压力为0.7MPa,冲洗时间为5.0s,极距2.85mm。在优化的试验条件下,21种元素测定值的相对标准偏差(n=12)在0.3%~15%之间。方法用于线材和棒材实际样品分析,测定结果与化学分析方法的测定结果相一致。 相似文献
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S. N. V. M. S. Gupta A. K. Nayak U. B. Misra Balaji Rao Yarasi C. Phani Babu G. Kalyanakrishnan 《Journal of Radioanalytical and Nuclear Chemistry》2017,313(3):571-579
The present paper describes a new analytical method developed for direct determination of boron in steels using radio frequency glow discharge optical emission spectrometer. “Single parameter alternative method” technique has been used to optimize the various experimental conditions of glow discharge plasma such as forward power, gas pressure inside plasma chamber, pre-integration time, and integration time. Different emission lines for boron were studied and inter element interference effect is also discussed in the paper. A complete statistical analysis has been done to validate the developed method. A RSD of less than ±5% is achieved for boron in the range of 0.0010–0.020% in Steels using this method. 相似文献
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Improving boron isotope ratio measurement precision with quadrupole inductively coupled plasma-mass spectrometry 总被引:2,自引:0,他引:2
Assad Al-Ammar Eva Reitznerov Ramon M. Barnes 《Spectrochimica Acta Part B: Atomic Spectroscopy》2000,55(12):1861-1867
A method was developed to improve the precision of inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) for the determination of boron isotope ratios (11B/10B) in various environmental materials including seawater. This approach is based on the common analyte internal standardization (CAIS) chemometric algorithm. The sample solution obtained after digestion is spiked with lithium, and both 7Li/6Li and 11B/10B values are measured using long-counting periods (20 min). The CAIS algorithm corrects the measured 11B/10B values for (a) statistical fluctuations resulting from short-term noise; (b) drift in 11B-to-10B ratio as a result of long-term deviation in instrumental parameters likely to occur during long counting times; (c) change in 11B-to-10B ratio caused by variation in matrix elements concentrations; and (d) drift in mass bias correction factor. Comparing boron isotopic ratios in seawater measured by conventional and the new isotope ratio methods validates the procedure. A synthetic isotopic mixture of boron SRM 951 and enriched 10B SRM 952 also was examined. The CAIS method provided a measured boron isotopic ratio precision of 0.05% R.S.D. while eliminating 5.1% matrix concentration error and 0.25% instrumental drift error. 相似文献
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Alexei Plotnikov Jens Pfeifer Silke Richter Heinrich Kipphardt Volker Hoffmann 《Analytical and bioanalytical chemistry》2014,406(29):7463-7471
Fast flow glow discharge mass spectrometry with a Grimm-type ion source providing a high sputter rate was used for the determination of major nonmetallic impurities in magnesium. The analytical signal was found to be strongly influenced by the electrical discharge parameters. For calibration by standard addition, synthetic standard samples were produced in two different ways—namely, by pressing and by sintering doped metal powders. The observed sensitivity of the calibration curves was shown to depend on the particle size of the powder. For the magnesium powders, the mass fractions of oxygen, nitrogen, boron, and silicon were determined to be about 0.01 kg?kg-1 (relative standard deviation approximately 10–20 %), 2,700 mg?kg-1, 150 mg?kg-1, and 300 mg?kg-1, respectively. 相似文献
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电感耦合等离子体质谱法测定硼同位素丰度 总被引:1,自引:0,他引:1
以硼同位素标准物质NIST SRM 951配制标准溶液,在优化的仪器操作条件下对电感耦合等离子体质谱(ICP-MS)测定的硼同位素质量进行校正,求出校正因子,确定了样品的线性浓度范围,选定样品浓度为1.1 mg/L。在同样的仪器条件下首先测定了硼标准物质的硼同位素丰度比,测量误差为0.2%,然后测定了硼同位素浓缩过程中硼样品的硼同位素丰度比,测定结果的相对标准偏差为1.1%。此外考察了仪器的稳定性。实验结果表明本方法“记忆效应”小,结果可靠,测量精度高。 相似文献
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Marisa Di Sabatino Anne L. Dons Joachim Hinrichs Lars Arnberg 《Spectrochimica Acta Part B: Atomic Spectroscopy》2011,66(2):144-148
A commercially available Element GD, the latest generation of glow discharge mass spectrometry (GDMS), has been used for quantitative analysis of impurities in silicon for photovoltaic applications (PV silicon). In order to be able to accurately measure impurities in silicon, relative sensitivity factors (RSFs) need to be determined. These factors are, currently, given only for steel matrices. In this study, standard silicon materials with known levels of impurities have been produced and independent analytical methods have been used for determining the RSFs for silicon matrices. It has been found that the tuning parameters of the Element GD, mainly the discharge gas flow rate, influence the RSF values. In addition, it has been found that RSF values are matrix specific; RSFs for a silicon matrix differ significantly from those for metallic conductor matrices even under identical instrumental parameters. A study of the relative reproducibility in the quantitative analysis of impurities in solar cells silicon has shown variations between 5% and 12%. 相似文献
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建立了双孔石墨管原子吸收法测定化探样品中痕量金的方法。以王水溶解样品,泡沫塑料吸附,10 g/L的硫脲溶液解脱,2%抗坏血酸作为基体改进剂,用双孔石墨管原子吸收法测定化探样品中的痕量金。该方法仪器分析时间由65 s缩短到32 s,提高了工作效率,方法标准曲线线性相关系数为0.999 8,检出限为0.045 ng/g,测定结果的相对标准偏差为4.1%~6.9%(n=7),标准样品测定值与推荐值的相对偏差小于3.24%。该法适合批量化探样品中金的测定。 相似文献
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The breakdown voltage has been found to be dependent on the gap width between the electrodes and on the melting point of the sample elements in spark-source mass-spectrometry (SSMS). The number of discharges per pulse train and the time required to reach the first discharge depend only on the chosen breakdown voltage. The spark gap is proportional to the "radius" of the volume sampled (for a given element) and this radius is linearly related to the reciprocal of the melting point of the elements (23 different elements, metals or semiconductors), when fixed spark-parameters are used. The effect of electrode temperature on material consumption can be qualitatively explained by a fictive increase or decrease in melting point of the element. Knowledge of the relations between the different spark and instrumental parameters and the volume or weight of sample consumed can be applied to the study of the homogeneity of samples, to in-depth analysis by SSMS and to the analysis of microsamples. 相似文献
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Differential pulse anodic stripping voltammetry with a hanging mercury drop electrode is used for the direct and simultaneous determination of Zn, Cd, Pb, Cu, Sb and Bi at their natural levels in sea water after adjustment to pH 1 and to a 2 M chloride concentration. The optimal instrumental parameters are described. With a plating time of 60 min, the detection limits are about 0.1 ppb for Zn and Cu, 0.01 ppb for Cd and Pb, and 0.05 ppb for Sb and Bi. Relative standard deviations are about 10—15%. Simultaneous determinations of the six metals take about 2 h. 相似文献