The Elimination of Chloride and Sulfate Interference on Germanium in Graphite Furnace Atomic Absorption Spectrometry

The advantage of determination of trace germanium (Ge) by graphite furnace atomic absorption spectrometry is that only a few microliter of sample is used. But the matrix interference,especially chloride ion and sulfate ion are very serious.     

涂钨石墨管石墨炉原子吸收光谱法测定人参中锗

石墨炉原子吸收法测定锗的问题主要是样品原子化前会形成易挥发的GeO,影响分析灵敏度。有关测锗的报道见文献。本工作应用CCl_4萃取和水反萃取,涂钨石墨管石墨炉原子吸收测定人参中锗,获得满意的结果。     

氢化物发生——原子荧光光谱法的干扰及其消除

归纳总结了在氢化物发生-原子荧光分析中液相干扰和气相干扰产生的机理及消除办法,特别是对复杂样品根据不同的分析对象采用不同的办法消除干扰,对在日常的分析中的各种干扰将会得到更好的解决办法.引用文献38篇.     

Factorial and Doehlert Design Used as Optimization Procedures for the Direct Determination of Lead in Whole Blood Samples by Graphite Furnace Atomic Absorption Spectrometry

In this work, the direct determination of lead in whole blood samples by graphite furnace atomic absorption spectrometry is proposed. The samples were diluted 1:9 with HNO₃ and Triton® X-100, both 0.2% v/v. Multivariate optimization was made to evaluate the pyrolysis and atomization temperatures and the use of a chemical modifier. The method allowed lead determination with a curve ranging from 0 to 6.0 μg dL^?1. Recovery studies presented results from 88 to 109%. The LOD and the characteristic mass were 0.21 μg dL^?1 and 7.4 pg, respectively. Intra- and inter-assay studies showed respective coefficients of variation of 4.2 and 8.9%.     

消除原子吸收光谱分析中干扰效应的正交多项式回归设计

应用正交多项式回归设计的方法,对原子吸收光谱分析中的干扰效应进行计算消除的研究。通过实验建立了针对高纯 Eu2O3中钙含量测定时消除干扰的最优回归方程,回归方程精度为 1.32× 10－ 2,对高纯 Eu2O3中钙含量测定,计算结果与实际含量基本一致,相对误差为 1％～ 4％。     

石墨炉原子吸收法测定人体血浆和尿中锗

研究了口服有机锗（Ｇｅ－１３２）后人体血浆及尿中锗的测定方法。以５％三氯乙酸溶液沉淀血蛋白，离心分离后，取上清液测定。以钯和硝酸镍混合溶液做基体改进剂，提高灰化温度至１４００℃，消除了样品中大量基体对测定锗的干扰。方法特征量为３１ｐｇ，检出限为２８ｐｇ（３σ），样品加标准回收率为：血浆９１．４％～９７．０％，尿９７．２％～１０５％。     

原子荧光光谱法测定锌电解液中的痕量锗

主要研究了锌电解生产过程中新液、电解液中痕量锗的准确稳定分析方法。结果表明:在20%的磷酸溶液中,用标准加入法,原子荧光光谱仪测定新液、锌电解液中的锗,对同一样品进行8次测定,其相对标准偏差为5.3%,锗的加标回收率为95.6%~102.0%,结果稳定可靠,能满足生产要求。     

氢化物发生-原子荧光光谱法测定铀矿石中的锗元素

建立了氢化物发生-原子荧光光谱法测定铀矿石中锗元素的方法,使用HNO_3-HF-H_2SO_4-H_3PO_4混酸体系消解样品,对铀矿石中的微量Ge元素进行分析,方法检出限为0.024μg/g,样品相对标准偏差（RSD）为3.4%。通过与标准值比对,结果准确度令人满意,未知样品加标回收率在98.4%-103%。可以作为实验室日常分析含铀矿石中微量Ge元素的参考方法。     

镧涂层塞曼效应石墨炉原子吸收法测定铜基合金中微量锡

本文采用塞曼石墨炉原子吸收法结合石墨管涂镧技术测定了铜基合金中微量锡。文章对比了涂镧管与非涂镧管测定锡时的原子化曲线对于镧涂层对实验结果的影响及酒石酸的作用进行了讨论，提出了镧化合物可能在管内起到催化作用的观点。实际样品测定相对标准偏差为４．４％，加标回收率１０１％。     

Determination of Germanium and Tin and Inorganic Tin Species by Hydride Generation in Situ Trapping Flame Atomic Absorption Spectrometry

The analytical performances of a coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system were evaluated for determination of Ge and Sn and inorganic tin species in environmental samples. Germanium and tin hydrides were atomized in air-acetylene flame-heated IAT. A new design of HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube) permitting construction of an “integrated trap” was investigated. For the estimation of Sn(II) and Sn(IV) concentrations in samples, the difference between the analytical sensitivities of the absorbance singnals obtained for tin hydride without and with previous treatment of samples with L-cysteine could be used. The concentration of Sn(IV) was calculated by the difference between total Sn(tot) and Sn(II). An improvement in limit of detection was achieved compared with that obtained using any of the aforementioned atom trapping techniques separately. The concentration limits of detection were 25 and 8 ng mL^?1 for Ge and Sn, respectively. For a 2 min in situ preconcentration time, sensitivity enhancement, compared to FAAS, were 10 and 14 folds for Ge and Sn, respectively, using hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The relative standard deviations (RSDs) are of the order of 5–10% for this hyphenated technique. The designs studied include slotted tube, single silica tube, and integrated atom trap water-cooled atom traps. The accuracy of this method was tested by analyses of BCS-CRM No.346 (Alloy), GBW 07302 (Stream Sediment), PACS-1 (Marine Sediment), NBS SRM 1633a (Coal Fly Ash), and NIST SRM 1643e (Trace Element in Water) certified reference materials. Agreement between analytical results and certified values for the test elements Ge and Sn (in the range of 1.7–91.0 µg g^?1) were in agreement with recommended values. The measured Ge and Sn contents in five referenced materials were in satisfactory agreement with the certified values. The hyphenated technique was applied for germanium and tin determination in coal fly ash, soil, sediment, garlic, sewage, and river water.     

Kalman滤波法校正火焰原子吸收光谱干扰

本文将Ｋａｌｍａｎ滤波法应用于原子吸收光谱中，对光谱严重叠加的锰和镓进行了校正，讨论了波长测量点的选取技术对实际结果的影响。１６个合成样品的测定结果表明该法简单，有效。     

石墨炉原子吸收光谱法测定黑花生中痕量锗

建立了高压密闭消解-石墨炉原子吸收法测定黑花生中痕量锗的分析方法。优化了石墨炉原子吸收法的测定条件。该法以Pd(NO3)2+Ni(NO3)2为基体改进剂,样品的灰化温度和原子化温度分别为1100℃和2300℃,锗的检出限为3.27μg/L;回收率为92.7%～105.0%;相对标准偏差为1.74%～4.65%。研究结果表明:花生仁及其包衣中均含有痕量锗,且黑花生中锗含量高于同一产地出产的另外两个品种。     

石墨炉原子吸收光谱法测定人血及人发中的锗

研究了人体血液及人发中锗的测试方法，其中人发样品在密封罐中消化分解，血液用Ｔｒｉｏｎ Ｘ－１００以１：８稀释，以硝酸钯和硝酸铵混合溶液作为基体改进剂，用石墨炉原子吸收光谱法进行测定，在很大程度上提高了方法的灵敏度和抗干扰能力。方法特征值为２０ｐｇ，标准检出限为０．４５μｇ／Ｌ。样品加标回收率，血液１００．９％￣１０３．２％，发样９３．７％￣９７．２％，ＲＳＤ＝５．１％。     

Gas-Screen Slotted Quartz Tube Atomic Absorption Spectrometry: A Remedy for Reducing Interference Effects of Calcium and Chromium

A simple device for the reduction of nonspectral interferences in flame atomic absorption spectrometry is proposed. It has been reported that the use of a gas screen (GS) system together with a slotted quartz tube (SQT) enhances the residence time of analyte atoms in measurement zone even more than the SQT alone. This combination causes enhancement of sensitivity and improves the reproducibility of absorbance measurements. In addition, it protects the optical windows of the atomic absorption spectrometer. The operational mechanism of gas screen is simply applying two argon gas walls at both ends of SQT to provide an environment that is partly protected from air. This action enhances the sensitivity of measurement.

In this study, interference effects of excess amounts of calcium and chromium on the measurements of Cd, Co, Cu, Pb, Mn, Ni, Se, and Zn were studied using flame AAS. The presence of both Ca and Cr cause higher absorbance values; it is suggested that this is due to formation of oxide species of Ca and Cr and as a result analyte oxide production is suppressed. Therefore, analyte free atom population and sensitivity are enhanced. This enhancement results in a positive error in measurements. For instance, presence of solely 8.0 mg L^?1 of Cr or Ca for Pb as the analyte enhances the signals by 75% and 56%, respectively. When SQT or GS-SQT is used, this effect is significantly reduced.     

电感耦合等离子体发射光谱法(ICP-OES)测定钴白合金中的锗

建立了一种电感耦合等离子体原子发射光谱法(ICP-OES)测定钴白合金中锗含量的分析方法,确定了溶样方法和分析谱线,进行了基体元素的干扰等实验,对方法精密度和准确度进行了考察,结果表明,方法的检出限为0.043 μg/mL,对钴白合金中锗的测定结果与其它标准分析方法分析结果基本一致,方法的相对标准偏差RSD在1.1%~1.9%(n=7),样品的加标回收率在98.5 %~102.1 %。所建立的方法准确、快速,适用于钴白合金中锗的测定。     

氯化物发生-电感耦合等离子体发射光谱法测定含锗保健品中无机锗

基于电感耦合等离子体发射光谱(ICP-OES)法研究了无机锗和有机锗在HCl介质中的氯化物发生情况.结果表明,有机锗(Ge-132)不形成氯化物,而无机锗在以浓 HCl为载流,载气压力0.14 MPa,样品溶液中HCl浓度为6 mol/L时能实现最佳的氯化物发生效率,由此建立了含锗保健品提取液中无机锗的选择性测定新方法...     

空气-乙炔火焰原子吸收测定铬时与浓度有关的化学干扰的研究——Ⅰ、铁、钴对铬的干扰

本文较详细地研究了在Fe、Co基体中测定铬时出现的与浓度有关的化学干扰,铬的价态对干扰的影响,并讨论了干扰的机理及克服干扰的办法。     

多波长线性回归法校正火焰原子吸收光谱干扰

用多波长线性回归法校正了火焰原子吸收分析中Ｇａ４０３．２９８ｎｍ对Ｍｎ４０３．３０７ｎｍ的吸收线重叠干扰，对合成样中Ｍｎ和Ｇａ含量的测定，结果令人满意。     

微波消解石墨炉原子吸收光谱法测定钛白粉中铅

采用微波消解系统消解钛白粉样品，研究了各种酸的用量与不同消解程序对消解效果的影响，选择了微波消解的最佳工作条件。用平台石墨炉原子吸收光谱法测定样品中的铅，与常压酸消解法的结果作比较，结果基本一致。