动态三磁场塞曼背景校正技术应用于石墨炉原子吸收光谱法测定血样中铅

在石墨炉原子吸收光谱法测定血样中铅时,采用动态三磁场塞曼背景校正技术,使血样中铅测定的线性范围由0～100μg.L-1扩增到0～800μg.L-1。动态模式下,质量浓度在80μg.L-1范围以内选择二磁场背景校正模式,特征量为29.4pg。在80～800μg.L-1范围内选择三磁场背景校正模式,特征量为10.7pg。应用此法测定高浓度铅的样品时无需稀释,同时解决了高浓度样品测定时出现塞曼反转,及吸收信号出现双峰的问题。     

三磁场塞曼背景校正技术用于石墨炉原子吸收光谱法测定水中铝

在石墨炉原子吸收光谱法测定水样中铝时,采用三磁场塞曼背景校正技术。铝的质量浓度在0.4mg.L-1以内与吸光度呈线性关系,方法的检出限(3s)为0.04μg。方法用于实验室能力验证标准溶液(NIL PT-0130)中铝的测定,测定结果与电感耦合等离子体质谱法测定值相符。取3个浓度水平的铝标准溶液进行精密度试验,平行测定6次,测定值的相对标准偏差在2.7%～4.3%之间。     

碱消解-火焰原子吸收光谱法测定土壤中六价铬

建立了碱消解-火焰原子吸收光谱法测定土壤中六价铬的方法.讨论了pH值对六价铬测定的影响.干扰实验的结果表明同等含量的三价铬对六价铬测定无干扰.实验对比了无背景校正、氘灯背景校正、塞曼背景校正三种工作方式,分别对低、中、高三个水平土壤六价铬标准物质进行了测定,结果表明,低含量的土壤样品用塞曼背景校正方式测定的结果更准确,...     

恒定横向磁场塞曼原子吸收吸光度的计算方法

提出了恒定横向磁场塞曼原子吸收光谱法中吸光度的计算方法，讨论了用该法指导塞曼原子吸收光谱仪器的技术改造，以改善其若干技术性能。     

等温平台石墨炉原子吸收法测定食用明矾中的铅

本文介绍了通过应用等温平台石墨炉,以(NH_4)_2HPO_4为基体改进剂,塞曼背景校正和积分吸收信号测定食用明矾中的Pb。本法有效地抑制了样品中基体干扰。重现性好,检测限为10pg,平均回收率为101.1%。     

原子吸收光谱中的三磁场塞曼背景校正技术

1　塞曼效应原子吸收光谱分析测量被分析元素基态原子对分析元素共振线的吸光度。但是除了被分析元素的共振吸收外 ,通常还有背景吸收 ,必须予以扣除或校正 ,才能获得准确的结果。塞曼原子吸收光谱仪利用塞曼效应作背景校正。当光源置于强磁场内时 ,光源辐射的谱线发生分裂 ,称为塞曼效应或塞曼分裂。分裂产生中心波长不变的π组分和对中心波长频移的σ +、σ -组分 ,该频移称为洛伦茨裂距。π组分和σ±组分有相互垂直的偏振方向。塞曼效应有正常塞曼效应和反常塞曼效应之分 :正常塞曼效应分裂出一条π组分和 2条σ组分(一条σ+和 -条σ -)…     

塞曼原子吸收光谱法应用技术

一、塞曼原子吸收光谱法的特点塞曼原子吸收光谱法的主要特点是背景校正能力强。本文从分析单色器光谱通带内谱线情况入手,将背景情况分类,进而讨论塞曼法对名类背景的校正能力。     

用塞曼GFAAS法和基体改进技术直接测定海水中痕量砷

用原子吸收光谱法测定砷有多种方法,各有其特点。本文将介绍采用塞曼背景校正技术和基体改进剂减轻或消除基体干扰,以标准加入法测定海水中痕量砷。方法灵敏度     

固体进样石墨炉原子吸收光谱法测定船用燃料油中硅、铝含量

建立了固体进样石墨炉原子吸收光谱法测定船用燃料油中微量硅、铝元素含量的快速检测方法。通过选择谱线和背景校正模式,优化了石墨炉条件;根据待测样品及元素特点优化了升温程序。硅、铝的测定波长分别为251.6,394.4 nm,采用塞曼背景校正,样品无需前处理,直接通过石墨舟进样检测。燃料油中硅、铝元素的检出限分别为0.165,0.126 ng;3个浓度水平下,硅元素平均回收率为88%~92%,铝元素平均回收率为93%~95%,测定结果的相对标准偏差为4.2%~10.7%(n=6)。采用本法对实际燃料油样品进行测定,硅、铝元素的测定结果与IP 501方法测定结果基本一致。该方法取样量少、操作简便、快速,检验结果准确度高、稳定性好,适用于船用燃料油中微量硅、铝元素含量的定量检测。     

原子吸收背景校正的新技术——史密斯-希夫叶法

背景校正在原子吸收光谱分析中是非常重要的,尤其对于石墨炉原子吸收分析。1965年氘弧背景校正器问世,1968年开始商品化,自那以后,大多数原子吸收光谱仪都配备了它。70年代后期,利用塞曼(Zeeman)效应的背景校正器被用于原子吸收光谱仪,但目前仅用在为数不多的仪器上。在1982年的第三十三届匹兹堡分析化学和应用光谱会议上,史密斯—希夫叶(Smith-Hieftje)背景校正法第一次公诸于世,在1983年于阿姆斯特丹举行的第二十三届国际光谱讨论会和第十届原子光谱会议上,H.L.Kahn又再次对其进行描述。本文将介绍这一看起     

An application of the Zeeman effect to atomic absorption spectrometry: a new method for background correction

A new Zeeman method for background correction in atomic absorption spectrometry was studied. The light source was operated in a steady magnetic field,     

Theory of Zeeman atomic absorption spectrometry

A theoretical analysis is presented of the signals observed with different systems that employ the Zeeman effect for background correction in analytical atomic absorption spectrometry.Magnetic modulation of the primary source of radiation offers basically the same possibilities as the deuterium background correction system. Correction for wavelength dependent background absorption is possible only when the magnetic field is applied to the absorbing vapour. Similar expressions are obtained for constant or variable magnetic fields directed either perpendicular or parallel to the optical axis. However, mere magnetic modulation of either the source or the atomizer cannot correct for non-absorbed lines.It is demonstrated that simultaneous correction for non-absorbed lines and background absorption can be attained with a variable magnetic field applied to the atomizer, by taking measurements at three discrete, different field strengths.     

Laser-excited atomic-fluorescence spectrometry in an electrothermal atomizer with Zeeman background correction

A pulsed excimer-pumped dye laser was used to excite atomic flourescence in graphite tube electrothermal atomizer. A 60-Hz ac magnitude field was applied around the atomizer and parallel to the excitation beam, for Zeeman background correction. The correction system was found to degrade the detection limits for silver, cobalt, indium, manganese, lead, and thallium by a factor of between 1 and 10. An increase in magnetic field strength, or a decrease in laser linewidth, should improve the detection limits, but was not possible here. For copper, the application of Zeeman background correction was unsuccessfull because the instrumentation was unable to resolve the sigma components from the laser emission profile sufficiently during the background correction measurement. For elements that exhibit sufficient Zeeman splitting, the linear dynamic range was the same with or without background correction Zeeman background correction was used to correct for scatter, in the resonance flourescence determination of manganese in a zinc chloride matrix and in mouse brain tissue.     

Background overcorrection problems for lead in the presence of phosphate with various metals in Zeeman graphite furnace atomic absorption spectrometry

Phosphate in various chemical forms has been widely used as a chemical modifier for the determination of Pb by graphite furnace AAS. When Pb was determined in bone digestate, with NH₄H₂PO₄ modifier and a transversely-heated furnace and a longitudinal Zeeman background correction system, low recoveries of Pb were found. This was found to be caused by a background overcorrection problem associated with the matrix of phosphate plus Ca and/or Mg. The overcorrection problem caused erroneously low Pb concentrations to be predicted when using aqueous Pb standards for calibration. The overcorrection problem was not reproduced with a transverse Zeeman correction system. While the magnitude and shape of the background signal changed with different phosphate compounds, the important features remained constant. We suggest that the background overcorrection problem was caused by molecular absorption of PO formed during atomization in the presence of any of several metals, most specifically the alkaline earth elements, since the PO molecular absorption bands appear to be subject to Zeeman-effect splitting.     

Analysis of standard reference materials after microwave-oven digestion in open vessels using graphite furnace atomic absorption spectrophotometry and Zeeman-effect background correction

Summary Heating-covered teflon digestion vials located inside a reheatable container in the presence of different acid mixtures with microwave oven dissolve the metals from biological and environmental certified reference materials. Pb, Cd, Cu, Mn and Fe from the dissolved samples are determined by graphite furnace atomic absorption spectrophotometry and Zeeman-effect background correction. The method allows the treatment of about 100 samples per operation.     

Determination of trace impurities in aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry

The trace impurities Cr, Cu, Fe, K, Mn, Sb and Zn were determined in powdered aluminum nitride by direct solid sampling graphite furnace atomic absorption spectrometry using a ZEEnit 60 atomic absorption spectrometer. This spectrometer features inverse Zeeman-effect background correction and a variable magnetic field enabling measurements in two sensitivity modes over a concentration range of three orders of magnitude. The measurement sensitivity can be adjusted to the analyte concentration in the sample. The use of chemical modifiers was not necessary. Calibration was carried out by means of calibration curves obtained with aqueous standard solutions. Accuracy was checked mainly by comparison of the results with those obtained by instrumental and radiochemical neutron activation analysis whereby, excluding the results for potassium, no significant differences were found by carrying out the t-test at the significance level 0.05. The limits of detection were between 0.05 ng g⁻¹ (Zn) and 80 ng g⁻¹ (Fe) and the relative standard deviations below 11 %. With the proposed method, up to ten measurement cycles can be carried out in one hour.     

Correction for background absorption and stray radiation in a.c. modulated Zeeman atomic absorption spectrometry

Analytical results are presented obtained with Zeeman atomic absorption (ZAA) using a modified sine wave magnetic field. The measurement at zero field strength is lengthened to 0.5 ms for a 50 Hz magnetic field of 10 kG.The a.c. Zeeman system is extended with an additional intensity measurement performed at an intermediate field strength. The three field Zeeman system (3FZAA) permits simultaneous correction for background absorption and stray radiation at the expense of halved analytical sensitivity. The background correction capabilities of ZAA and 3FZAA are the same. However, the 3FZAA signals show increased noise in comparison to ZAA.In the three field system the roll-over problem, inherent in existing Zeeman systems, is shifted to higher concentration and to higher absorbance. The height and the position of the maximum in ZAA and 3FZAA analytical curves do not depend on the amount of background absorption.A method for the extension of analytical curves in AA is presented. Utilizing an a.c. modulated magnetic field any sensitivity between zero and ordinary AA sensitivity can be obtained.     

A new type of Zeeman-effect atomic-absorption spectrophotometer

A new type of Zeeman-effect atomic-absorption spectrophotometer has been developed. It uses fast heating of a special atomizer made from a pyro-coated graphite tube lined with tungsten-tantalum alloy, for easier determination of refractory and rare-earth elements. A boxcar integrator is used, and the atomic absorption, background absorption and atomization temperature can be recorded. By means of the Zeeman effect, the instrument can correct for background absorbance up to 2.0.     

Determination of selenium in biological tissue samples rich in phosphorus using electrothermal atomization with Zeeman-effect background correction and (NH4)3RhCl6+citric acid as a mixed chemical modifier

Spectral interferences from phosphorus on the determination of selenium in biological tissue materials were not observed when a Zeeman-effect background correction was used with rhodium as a chemical modifier. A suppression effect on the selenium signal resulted when the concentration of phosphorus present was greater than 1.0 mg ml⁻¹. Rhodium was found to be more effective than palladium in overcoming the phosphate interference. Analytical procedures for the direct determination of trace selenium in standard reference materials by graphite furnace atomic absorption spectrometry following sample dissolution in nitric acid and hydrogen peroxide using a microwave oven has been described. The results obtained agreed favourably with the certified values.     

Semiclassical self-consistent field perturbation theory for the hydrogen atom in a magnetic field

A recently developed perturbation theory for solving self-consistent field equations is applied to the hydrogen atom in a strong magnetic field. This system has been extensively studied using other methods and is therefore a good test case for the new method. The perturbation theory yields summable large-order expansions. The accuracy of the self-consistent field approximation varies according to field strength and quantum state but is often higher than the accuracy from adiabatic approximations. A new derivation is presented for the asymptotic adiabatic approximation, the most useful of the adiabatic approaches. This derivation uses semiclassical perturbation theory without invoking an adiabatic hypothesis. © 1998 John Wiley & Sons, Inc. Int J Quant Chem 69: 183–192, 1998