钨丝电热蒸发-氩氢火焰原子荧光光谱分析法研究

以钨丝原子化器替换传统氢化物原子荧光分析仪石英炉原子化器及其氢化物发生气体进样系统,构建了一种新颖的集电热蒸发进样-氩氢火焰原子化为一体的原子荧光光谱分析系统;并用标准溶液研究了该系统的分析性能.在优化的仪器条件下,直接在钨丝表面进样,Pb、Ni和Au的检出限分别为:1.5、2.0和2.0μL.再结合电沉积预富集技术,...     

中国30多年来原子荧光光谱仪器的发展与应用

主要简述了原子荧光光谱仪器的发展历史,对我国30多年来原子荧光商品仪器在激发光源、石英管原子化器、蒸气发生反应系统等方面的发展作了详细论述,还就近年来新开发的原子荧光光谱仪器在多元素同时测定、多功能化、—机多用、形态分析等方面的技术发展和应用进行了全面阐述,并对原子荧光光谱分析领域的发展作出了展望。     

激光诱导荧光光谱分析进展

本文对激光诱导荧光光谱分析的研究现状和发展趋势进行了综述。着重介绍了激光诱导原子荧光光谱、激光诱导分子荧光光谱、激光低温光谱,时间分辨光谱和激光诱导荧光光谱与其它分析技术的联用研究。     

ICP-原子荧光光谱分析

一、前言高频感应耦合等离子体(以下简称ICP)作为优良的蒸发汽化源、原子化源(原子化器)、激发源及离子源而正在发射光谱分析(以下简称AES)中大量应用。然而,由于ICP产生的各种谱线非常多,对于ICP-AES分析,为使分析元素的光谱线分离,必须使用高分辨率的单色器,通常,由于光谱线的重叠或背景等产生的光谱干扰已成为重大的难题。原子荧光光谱分析(以下简称AFS)自1964年由Winefordner     

原子荧光光谱分析

一、前言原子荧光光谱分析(AFS)自1964年美国佛罗里达大学的Winefordner研究组提出以来,已经经历了20年,有了很大的发展,现在,已成为原子光谱分析的另一种力法。这期间由于Winefordner等及英国West等的大力研究,已发表许多关于原子荧光光谱分析的理沦研究、基础实验及各种应用的报告,确立了原子荧光光谱分析的基础。原子荧光光谱分析已被认为可与原子吸收光谱分析(AAS)和原子发射光谱分析(AES)相媲美的痕量金属元素的分析方法。但要像原子发射光谱分析那样成为常用的分析方法尚有待发展。在1970年Technicon公司试制并报导了能测定6种元素的原子荧光光谱分析装置.但是尚未达到普及的程度,暂时还没有市售的原子荧光光谱分析装置。另外,由于原子吸收光谱分析的兴盛,在相形之下显得衰落的原子发射光谱分析领域,开始了致力于新的等离子体光源的各种研究,以便代替原来所用的电弧、火花、火焰等激发电源。Fassel和Greenfield     

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、     

离子／原子荧光光谱分析

本文概述了离子／原子荧光光谱分析的实验装置，详细讨论了该技术中的激发源、离子化器和该技术的特点及应用；展望了离子／原子荧光光谱分析的发展趋势和研究方向。     

电热原子吸收光谱分析中的干扰及其消除和控制(一)

引言1.1 概述虽然化学火焰已广泛应用于原子光谱分析,但是仍然存在一些缺点。基本因素之一是其原子化效率较低。因此,研究了几种另外的基于辉光放电、稳定电弧、炉和丝的技术作为原子化的手段,其目的是在较小的体积中得到较高的原子浓度。用于原子吸收测量的在高温石墨炉中将试样电热原子化的方法已显示出最广阔的前景。它兼顾了非常高的原子化效率和适应固体试样或通常需要一些预处理的试样的能力。另外的好处是可以在受控的气氛中工作。然而,与火焰原子化法相比,在电热原子化器中     

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。     

地气样品元素含量分析

地气测量是一种有很好应用前景的找矿技术.然而,由于地气样品的元素含量非常低,这就使分析方法成为该找矿方法的关键所在.本文论述了原子吸收光谱法、中子活化分析、激光原子荧光光谱分析、等离子体质谱分析等在地气样品元素含量分析中的应用现状.建议对不同的地气样品采用不同的分析方法,用解脱剂解脱吸附在聚氨脂泡沫塑料上的地气物质和高效采集样品.     

Laser excited atomic fluorescence spectrometry — a review

This review focuses on the development of new instruments, and new applications of laser excited atomic fluorescence spectrometry, LEAFS, in recent years since the last published reviews. Such developments include solid-state tunable lasers, deep UV tunable lasers, the use of charge coupled detectors (CCDs), and the applications of LEAFS for trace metal determination in various samples. The advent of diode lasers with their now somewhat improved range of wavelengths and power output, provides opportunities for research and applications in LEAFS. The further development of the coupling of second and third harmonic crystals to pulsed diode lasers shows promise for compact and robust instrumentation. There have been no recent instrumental developments that might provide more isotopic selectivity beyond the elements like uranium where the spectral isotope splitting is greater than most elements, but laser diodes could provide this due to their potential to provide an output with very narrow spectral bandwidth. The advent of optical parametric oscillator-based lasers has enabled LEAFS to be much more practical then in the past when dye lasers were used. This should be the harbinger of more applications of LEAFS to complex real sample analyses that can not be done by other techniques for reasons of sensitivity or selectivity. Array detectors provide an additional degree of freedom by provision of more spectral information more rapidly, which should aid the study of complex samples that might produce complex background problems. The recent literature indicates that the sensitivity, selectivity and ease of method development of LEAFS is well-established, and that there are no substantial analytical disadvantages to the technique beyond the instrumental limitations associated with the single element at a time mode of operation and the complexity of the laser systems. Laser technology continues to develop rapidly, which heralds a bright future for LEAFS.     

LEAFS determination and concentration of metals in Great Lakes ecosystem

A Laser-Excited Atomic Fluorescence Spectrometric (LEAFS) method for Tl determination has been extended to investigate the direct determination (without preconcentration nor acid digestion) of total Pb, for which the method validation was successfully achieved by using a standard reference material as well as many spike recoveries of digested and undigested unfiltered water samples. The method was applied to study total and dissolved Pb in many water columns collected from different stations in Lake Ontario. Dissolved Pb was found to be about twice as much as dissolved Tl, and total Pb about seven times higher than total Tl. Seventy five percent of Pb is in particulate form versus 11% for Tl. Also, a simple cold dissolution procedure using HNO(3) and HF (not a hot acid digestion) is proposed to "liquefy" sediments in a form suitable for LEAFS analysis and was used to analyze a sediment core, where pore water samples were also collected. The interaction dynamics of Tl within the natural environment of a water/pore water/sediment system from Lake Erie was assessed. The calculations of fluxes suggest a strong similarity between Tl and Cd geochemical transport. The paper also presents for the first time a genuine sediment pore water profile of Tl concentration, which ranged from sub- to 40 ng/l and which was directly determined by LEAFS.     

Ultratrace determination of Bi in Greenland snow by laser excited atomic fluorescence spectrometry

The results of the first determination of Bi traces in snow samples from Greenland by laser excited atomic fluorescence spectrometry are presented. A limit of detection as low as 0.05 for one-color LEAFS technique is attained. Strong matrix interference in real snow samples was observed and some ways of reducing this are tested. The main source of background is molecular fluorescence of unidentified species. The measured Bi concentration in snow samples ranges within 0.07–0.6 .     

LEAFS determination and concentration of metals in Great Lakes ecosystem

A Laser-Excited Atomic Fluorescence Spectrometric (LEAFS) method for Tl determination has been extended to investigate the direct determination (without preconcentration nor acid digestion) of total Pb, for which the method validation was successfully achieved by using a standard reference material as well as many spike recoveries of digested and undigested unfiltered water samples. The method was applied to study total and dissolved Pb in many water columns collected from different stations in Lake Ontario. Dissolved Pb was found to be about twice as much as dissolved Tl, and total Pb about seven times higher than total Tl. Seventy five percent of Pb is in particulate form versus 11% for Tl. Also, a simple cold dissolution procedure using HNO₃ and HF (not a hot acid digestion) is proposed to liquefy sediments in a form suitable for LEAFS analysis and was used to analyze a sediment core, where pore water samples were also collected. The interaction dynamics of Tl within the natural environment of a water/pore water/sediment system from Lake Erie was assessed. The calculations of fluxes suggest a strong similarity between Tl and Cd geochemical transport. The paper also presents for the first time a genuine sediment pore water profile of Tl concentration, which ranged from sub- to 40 ng/l and which was directly determined by LEAFS.     

Analytical characterization of laser excited atomic fluorescence of bismuth

The possibilities of direct determination of Bi traces by laser excited atomic fluorescence spectrometry were investigated. Practically all one-color excitation-detection schemes were examined. For the resonance fluorescence at 306.8 nm, the main source of background was a molecular fluorescence of residual water vapors. The background characteristic OH rotational lines of O-O band of ²Σ - ²Π transition were registered in the excitation spectra. From the relative intensities of the rotational components, the gas temperature of the analytical volume above the open graphite cup of the atomizer was estimated as 680 ± 120°C. A detection limit (LOD) of about 1 pg/ml was achieved for the resonance scheme. For the excitation wavelength shorter than 230 nm, broadband fluorescence of unidentified species in the 300-400 nm spectral range was the main source of background. The best LOD of 0.05 pg/ml was realized for the 223.1/ 299.3 nm excitation-detection scheme. This LOD is the best one for the one-color LEAFS technique. Possible ways of further increasing the LEAFS sensitivity of Bi traces detection are briefly discussed.     

Tungsten coil devices in atomic spectrometry: absorption, fluorescence, and emission.

In this work, tungsten coil (W-Coil) devices are used as atomizers for electrothermal atomization atomic absorption spectrometry (ETAAS), electrothermal atomization laser excited atomic fluorescence spectrometry (ETA-LEAFS), and electrothermal vaporization inductively coupled plasma atomic emission spectrometry (ETV-ICP-AES). For most cases in ETAAS and ETA-LEAFS, limits of detection (LODs) using the W-Coil are within a factor of ten of those observed with commercial graphite furnace systems. LOD for Cd by W-Coil AAS is 10 pg, while LODs for As, Se, Cr, Sb and Pb by W-Coil LEAFS are 950, 320, 1400, 330, and 160 fg, respectively. The compact W-Coil device makes it an ideal atomizer for portable atomic spectrometry instrumentation, especially when coupled with a miniature charge coupled device spectrometer. Alternatively, the atomizer can be used as an inexpensive, modular add-on to an existing commercial ICP-AES system; and the thermal separation of Pb with interference elements Al, Mn, and Fe is demonstrated.     

A Novel, Simple Method for Tuning Dye Lasers

A novel, simple and cost-effective method has been developed for tuning dye lasers used in laser-excited atomic fluorescence spectrometry. The method uses two common laboratory items-a pierced mirror and a commercial electrodeless discharge lamp (EDL). In contrast to the existing procedure using flame, there is no nebulizer-burner, hood, gas tanks, nor burner control unit involved. The EDL lamp method also facilitates the simultaneous monitoring of reference and analyte peaks. It allows the monitoring of laser stability during experiments. A practical minimum pulse energy required for tuning and LEAFS studies was found to be 200 nJ.     

Thallium and cadmium in recent snow and firn layers in the Canadian Arctic by atomic fluorescence and absorption spectrometries

Compared to the Antarctic and Greenland, the Canadian Arctic has seen extremely few trace metal studies on snow and ice. Surface, subsurface and depth samples of snow and firns were collected from the Agassiz Ice Cap, Ellesmere Island, Canada using clean room practices. Results for Tl (directly determined by LEAFS) and Cd (determined by GFAAS) are reported. To our knowledge, the thallium depth profile presented here is the first one so far reported for both polar systems, Greenland or other places. Tl concentrations peak in the winter-spring periods, when the Arctic atmosphere is loaded with foreign pollutants and suspended particulates which sometime severely reduce the visibility, creating a phenomenon commonly known as the Arctic haze. These results are in general accordance with the historical Arctic air pollution and acidity/conductivity data on ice cores. Surface concentrations of Tl range from 0.3 to 0.9 pg/g, which is a few times higher than those found in Antarctica. Cadmium shows seasonal characteristics similar to Tl although there is not a definite correlation between the two. However, there could be two predominant origins of metals which were deposited in the snow: Eurasian origin in January–April corresponding to high level metals (main deposition), and a less definite origin in May–December corresponding to low level metals.     

Laser-induced fluorescence determination of thallium in sediments

A simple dissolution procedure is decribed for sediments to be analyzed for thallium by Laser-Excited Atomic Fluorescence Spectrometry (LEAFS). It simply uses a nitric – hydrofluoric acid mixture at room temperature (a “cold dissolution” procedure as opposed to the hot acid digestion) followed by a dilution with water (as opposed to the tedious steps of separation and preconcentration). Excellent accuracy (91–106% recoveries) and precision (4–10% relative standard deviation) were demonstrated by the use of five sediment reference materials of diverse origins. The detection limit was estimated to be 0.5 ng/g of thallium. Additionally, a hot plate digestion procedure, using an in-house designed semi-enclosed Teflon beaker, was also investigated; its analytical results agreed with certified values and confirmed the adequacy of the cold dissolution technique. The method is being applied to study the sediment – water interactions in lake environments. Received: 30 December 1996 / Revised: 20 March 1997 / Accepted: 30 March 1997     

Laser excited atomic fluorescence for studies of enhancement effects in the direct current plasma

This paper reports a preliminary use of laser excited atomic fluorescence spectrometry (LEAFS) to study analyte population enhancement caused by easily ionized elements (EIEs) in the direct current plasma (DCP). Spatial atom density profiles in the DCP were obtained using resonance fluorescence at the calcium atom line at 422.7 nm, with and without the addition of an EIE. Variations in atom density caused by an EIE were found to be far too small to account for the marked enhancements of atomic emission signals which are caused by EIEs.Direct line fluorescence of the barium ion, excited at 614 nm and detected at 455 nm, was used to probe the effect of an EIE on excited state populations. Measurements in the analytical region of the plasma close to the core revealed that enhancements of fluorescence signals at low laser powers disappeared at laser powers which were sufficient to saturate the atomic transitions. While this result does not clarify any of the mechanisms of excitation in the DCP, it does lend support to two of the fundamental postulates of a recent model of the spectrochemical excitation processes in the DCP. These are first, that the analytical region of the DCP is not in local thermodynamic equilibrium (LTE) and second, that EIE enhancement proceeds by modulating the rates of power distribution among various plasma zones.In the outer zone of the analytical region of the DCP, depressive interferences occurred. These did not disappear upon saturation which indicates that they were not rate effects but effects that resulted from atom density changes.