原子荧光光度计常见干扰因素与排除

介绍了原子荧光光度计使用中的干扰因素、排除方法及仪器使用的维护及注意事项.     

使用AFS1201型原子荧光光度计应注意的问题

原子荧光光谱分析是一种具有重要实用价值的痕量分析技术。酸化过的样品溶液中砷、铅、汞等元素与还原剂硼氢化钾反应,生成氢化物,过量氢气和气态氢化物与载气混合,进入原子化器,使待测元素的激发光源激发氩氢焰中待测元素原子,得到的荧光信号被日盲光电倍增管接收,然后经放大、解调、     

AFS-230E型原子荧光光度计测汞时盐酸引起的故障及故障排除

用AFS-230E型厦子荧光光度计测定汞时,使用相同规格但不同厂家生产的盐酸对测定结果影响较大。使用该仪器测汞时由于配制载流液时选用盐酸不当发生空白值过高的现象,影响汞的准确测定。在排除其它可能故障后,更换不同厂家生产的盐酸进行试验,选用汞空白值低的盐酸,故障排除。     

原子荧光光度计在砷测定过程中出现的一例故障及故障排除方法

介绍了原子荧光光度计中原子化器温度降低在砷测定过程的故障现象、故障诊断及故障排除方法。阐述了由于测定原理不同,原子化器温度降低对砷、硒、汞检测影响的差异。     

分光光度计与计算机联机

人工记录的方法进无法准确记录分光光度计所批示的消光值,特别是因浓度（１０＾－５－１０＾－４ｍｏｌ／Ｌ）改变,而导致精度和准确度不高,采用计算机的方式是可以克服此种弊端,精确度和准确度都很高并有良好线性关系,且自动绘图（即经耳定律的线性图）并输出。此装置具有快速、直观、图文并茂等特点。     

原子荧光光度计检定/校准的影响因素

摘要：主要介绍了原子荧光分光光度计检定/校准的过程中常见故障,如联机故障、载气故障、点火故障和自动主要介绍了原子荧光分光光度计检定/校准的过程中常见故障,如联机故障、载气故障、点火故障和自动进样器故障等,针对无信号强度、荧光强度偏低、空白强度较高、仪器不稳定和重复性较差、线性不好等常见问题进行剖析并提出相应解决方法,根据工作经验和仪器工作原理提出了原子荧光光度计检定/校准过程中仪器参数和溶液配制方法。     

AFS-9800型双道原子荧光光度计常见故障分析与处理

原子荧光光度计在日常测过程中,由一些因素导致仪器测量灵敏度、精密度及线性等技术指标和检测结果不理想.本文针对AFS一9800双道原子荧光光度计在测量过程中遇到的线性不好、灵敏度低、检测结果重现性差等问题的原因进行了分析,提出故障处理方法.     

751型分光光度计故障三例及其排除方法

介绍751型分光光度计在检定中常见、鲜见故障及其排除方法。     

原子荧光光度计检定中常见的问题及解决方法

介绍原子荧光光度计在检定中常见的问题及解决方法。     

非色散原子荧光光度计计量检定规程中相关问题的探讨

探讨了非色散原子荧光光度计检定中部分技术指标与检测方法对高灵敏度、智能化新型仪器的适应性,提出了相关修改补充建议。经实际计量检定证明行之有效,较好的解决了实际工作中遇到的无法实施或检定指标与具体检测要求不相适应的问题,保证了计量检定后仪器分析结果的准确程度与公正性。     

The Determination of Bismuth By Hydride Generation and Non-Dispersive Atomic Fluorescence Detection

Abstract

A sensitive determination of bismuth by hydride generation with non-dispersive atomic fluorescence spectrometric detection is proposed. A commercially available electrodeless discharge lamp was used as the light source. Studies on interference effects from foreign elements are reported and the determination of bismuth in copper metal was considered in detail.     

石墨管阴极电化学氢化物发生原子荧光法测定锗

使用原子吸收法中的石墨管作为电解池中的阴极,设计了一种圆柱型电解池。通过电解产生锗的氢化物,并与原子荧光法联用,测定了标准样品中Ge的含量。对各种实验参数和干扰情况进行了详细研究。方法的检出限为0-67μg／L（36）;相对标准偏差（RSD）（200μg/L,n=11）为1．7％。     

Speciation of Organotin Compounds by Capillary Electrophoresis Coupled with Hydride Generation Atomic Fluorescence Spectrometry

Abstract

Capillary electrophoresis (CE) coupled with hydride generation atomic fluorescence spectrometry (HG‐AFS) was developed for the speciation analysis of organotin compounds. The four organotin cations of trimethyltin (TMT), monobutyltin (MBT), dibutyltin (DBT), and tributyltin (TBT) were completely separated by CE in a 50 cm×75 µm i.d. fused‐silica capillary at 15 kV and using a mixture of 50 mmol l^?1 H₃BO₃?50 mmol l^?1 Tris‐5% v/v methanol (pH 7.10) as electrolyte. 0.008 mmol l^?1 cetyltrimethylammonium bromide (CTAB) added to the electrolyte suppressed the adsorption of the organotin cations on the inner wall of capillary. The generated hydride species were detected on‐line with AFS. The precisions (RSD, n=5) were in the range of 1.7–3.1% for migration time and 3.8–4.7% for peak area response for the four organotin species. The detection limits ranged from 1–10 µmol l^?1 (as Sn).     

氢化物发生原子荧光法测定人发、玉米及辣椒中的砷

采用硝酸、高氯酸和硫酸湿法分解人发、玉米及辣椒,在盐酸介质中用硫脲-抗坏血酸将As(Ⅴ)还原为As(Ⅲ),氢化物发生原子荧光法测定,此法简便快速,相对标准偏差为2.4%。     

原子荧光光谱法测定食品硒的前处理方法研究

建立了湿法消解-原子荧光光谱法测定食品中硒。采取两种不同加热方式还原硒,实验发现:温热还原方式标准参考物的测定结果在认定值范围内,回收率为108%~114%,样品测定结果精密度良好;强热还原方式标准参考物的测定结果低于认定值,回收率偏高,样品测定结果精密度差。采用湿法消解-原子荧光法测定食品中硒,前处理过程中加入还原剂盐酸后应进行温热还原,加标回收率和精密度良好,结果准确。     

植物和人发样品中痕量铅的氢化物原子荧光测定

以双电极高强度空心阴极灯作激发光源，于铁氰化钾碱性体系内进行铅的氢化反应。实验表明，原子化过程中石英炉芯对铅烷存在吸附。在最佳测试条件下，溶液检出限为０．１７μｇ／Ｌ，分析了国家一级植物标样和头发标样中痕量铅，取得令人满意的结果。     

氢化物原子荧光法测定海水中硒的方法研究

用原子荧光法测定了海水中的硒，校准曲线的线性程度、检出限、精密度及准确度都能满足要求。     

氢化物原子荧光光谱法测定水中微量砷和硒

研究了氢化物发生-原子荧光光度法测定水中微量砷和硒的方法。结果表明,检出限:砷为0.0518μg/L,硒为0.0524μg/L;11次测定的相对标准偏差为0.36％～0.62％;标准回收率:砷为96.8％～100.9％;硒为95.9％～103.7％。方法简便、快速、灵敏,适于生活饮用水、地表水和水源水中微量砷、硒的同时测定。     

Hydride Generation Atomic Fluorescence Spectrometric Determination of Ultratrace Arsenic in High Purity Indium Oxide

A simple, sensitive, and interference free method was proposed for the determination of total arsenic in high purity indium oxide by hydride generation atomic fluorescence spectrometry (HG-AFS). Preconcentration was carried out by distillation of volatile arsenic trichloride. Hydrazine sulfate was used as a prereductant to reduce As (V) to As (III). The volatile arsenic trichloride generation was based on the reaction between As (III) and hydrochloric acid, and vapors were absorbed with water. The method provides a linear response range of 2 ng/mL–70 ng/mL, a detection limit of 0.1 ng/mL, a recovery of 96%–113%, and an average relative standard deviation of 2.42%. The method was validated by means of interlaboratory comparative analysis with the proposed method HG-AFS, and the comparison of data by using proposed method HG-AFS and reference methods of ICP-OES and spectrophotometry.     

Atomic Fluorescence Determination of Selenium Using Hydride Generation Technique

Abstract

Hydride generation followed by atomic fluorescence spectrometry, a simple and very sensitive technique, has been evaluated for selenium analysis in different environmental and biological samples. Research is focused on the interfering effects of several selected anions, cations, and acids on the selenium determination and the sample preparation procedures. Besides some transition metals such as Ni²⁺ Co²⁺ and Cu²⁺ HNO₃ acid, the digestion medium used for sample preparation, shows strong interference. In order to reduce this interfering effect, matrix match or standard addition is recommended. This technique is validated by analyzing a number of standard reference materials. Results for selenium analysis in some biological samples are also presented.