A Device for Precise Temperature Control of Electrodeless Discharge Lamps

Electrodeless discharge lamps, (EDL) operated with an “A” antenna are shown to be extremely temperature sensitive. Changes of up to 10³ × in spectral radiant output may be produced by a 130 °K change in operating temperature. A simple device for controlling EDL temperature is described. Lamp stability and reproducibility for Hg, Cd, T1, Zn, Cu and Fe EDL are found to be greatly improved by temperature control, and lamp operation is greatly simplified.     

Atomic Emission Spectrometry of Microsamples in a Glow Discharge

A glow discharge system for atomic emission spectrometry is evaluated for physical and analytical characteristics. Lead (as the nitrate) is the model element used for these studies. The sputtering characteristics of several electrode designs are studied with the best system tried resulting in total sample vaporization in less than 1 s. Discharge currents up to 200 mA at a discharge voltage of 1200 V and a pressure of 2 torr are found to give the best results. The detection limit for lead is 0.9 ng and the linear dynamic range of response is greater than 2 orders of magnitude. Sodium chloride at a 100-fold excess amount causes a 50% decrease in the signal level.     

微波等离子体炬离子/原子荧光光谱研究 --稀土元素铕的离子/原子荧光光谱

文中用微波等离子体炬作离子／原子化器,强短脉冲供电空心阴极灯作激发源,进行了稀土元素的离子／原子荧光检测。详细研究了系统对Ｅｕ检测时的最佳工作条件,对微波等离子体功率,空心阴极灯电流,观测高度等因素对Ｅｕ离子／原子荧光信号的影响进行了讨论,测量了离子荧光和原子荧光谱的检测限。     

空心阴极灯激发的微波等离子体炬原子/离子荧光光谱研究--钙的原子/离子荧光光谱

用强短脉冲供电技术的空心阴极灯作激发源、微波等离子体炬作原子／离子化器，建立了原子／离子荧光光谱实验装置。详细研究了微波等离子体功率、观察高度、空心阴极灯电流等因素对原子／离子荧光信号强度的影响，测量了系统对Ca的原子／离子荧光光谱的检出限。     

Application of Preconcentration and Separation Techniques in Atomic Fluorescence Spectrometry

Abstract

With 135 references, this review presents the recent application of various preconcentration and separation techniques in atomic fluorescence spectrometry for the sensitive determination and speciation of various elements and their species. It focuses on sample pretreatment, separation, and enrichment-related techniques, including liquid–liquid extraction, solid-phase (micro)extraction, microwave/ultrasound-assisted extraction, pressurized liquid extraction, as well as chemical vapor generation. In this review, the historical development and overview of these preconcentration and separation methodologies are briefly discussed, together with a comprehensive collection of application of these methods in combination with atomic fluorescence spectrometry for determination of ultratrace amounts of elements and their species in various sample matrices (liquids and solids).     

原子荧光光谱法测定杜仲中的砷

采用双通道原子荧光光谱法测定杜仲中砷的含量。确定了仪器的最佳工作条件,考察了酸度、还原剂、预还原剂的影响以及共存元素的干扰情况。方法快速、简便、准确且灵敏度高,为中药材中砷的含量测定提供了较好的方法。     

原子荧光光谱法测定土壤中的硒

应用原子荧光光度计测定土壤中的硒,用1 1王水消解样品,对消解方式、仪器条件和共存元素的干扰及消除进行了探讨,确定最优检测条件,得到检出限0.13μg/L,相对标准偏差5.46%,测定标准样品与推荐值接近,该法简单,有较好的精密度和准确度.     

原子荧光光谱法测定黄铁矿中碲的含量

采用氢化物发生-原子荧光光谱法,考察了原子化器高度、负高压、灯电流、载气流速、屏蔽气流速、介质酸度、载流酸度和硼氢化钾浓度对测定的影响,优化了测定条件。用硫脲-抗坏血酸做干扰抑制剂消除大量基体元素及常见元素对碲元素测定的干扰,确定了黄铁矿中痕量碲的分析方法。     

Evaluation of a Continuous Flow Furnance Atomizer for Laser Excited Atomic Fluorescence Spectrometry

A system for continuous sample introduction into a ceramic atomization furnace for laser excited atomic fluorescence spectrometry (LEAFS) was developed. The system was evaluated using two different excitation sources, a nitrogen laser-pumped dye laser and a copper vapor laser-pumped dye laser. Pure aqueous Pb solutions were used for system optimization and analytical calibration curves. These curves were linear over at least three     

原子荧光光谱法测定水中砷的定量限

计算定量限的方法有很多,但是目前仍然没有一个普遍接受的方法。2006年美国环境保护署(USEPA)研发了一个计算定量限的新方法,在该方法中,定量限被称为最小浓度最低报出限(The Lowest Concentration Minimum Reporting Level,LCMRL)。这个计算方法操作简单,数据可靠而且具有很好的适用性。文中通过使用原子荧光光谱仪测定纯净水和矿泉水中的砷(As)的定量限,来对该EPA方法进行了验证。本文用EPA方法得到纯净水和矿泉水中As的定量限均为0.12μg/L,与常用的计算定量限方法10S0(S0为空白标准偏差)的计算结果相比较。EPA方法无论是从定义还是计算方法中都体现了定量限对准确度和精密度的要求,该方法在理论上较为严谨。     

原子荧光光谱法测定土壤和沉积物中铋

建立了王水沸水浴消解-原子荧光光度法测定土壤和沉积物中铋。优化了仪器参数、载流及还原剂浓度,比较了水浴消解、微波消解和电热板消解三种前处理方式处理土壤/沉积物中铋的优劣。实验表明,最佳的消解方式为水浴消解,该方法操作简单方便,结果准确,可靠。采用王水沸水浴消解土壤或沉积物试样,方法的检出限为0.01 mg·kg-1(取样量为0.500 0 g,定容体积为50 mL),检出下限为0.04 mg·kg-1。该方法测定土壤标准样品,测定值都在标准值范围之内,相对误差为-4.7%～-2.0%。该方法用于测定土壤和沉积物实际样品的相对标准偏差分别为2.5%～3.4%和3.1%～3.4%,加标回收率分别为97.6%～102%和99.5%～104%。     

原子荧光光谱法测定饮用水中的砷

研究了两种载流溶液浓度和还原剂溶液浓度条件下,原子荧光光谱法测定饮用水中砷的过程中仪器荧光强度值和光谱峰的变化,对仪器测量条件进行了优化.研究了不同检测条件下,待测水样中砷元素检出量的变化.结果表明,载流溶液浓度影响仪器荧光强度值的大小,还原剂溶液浓度影响光谱峰的出峰位置.盐酸和硫脲-抗坏血酸的加入影响待测水样中砷含量的测定结果.     

原子荧光光谱法测定灵芝中汞

用双道原子荧光分光光度计,断续流动程序和消解体系,测定灵芝中的汞,试验回收率在89.2%-106.3%之间.     

原子荧光光谱法测定动物肝中微量砷

建立了测定动物肝中微量砷的原子荧光光谱方法 ,方法灵敏度高 ,准确度好。在选定的试验条件下 ,荧光强度与砷浓度在 0～ 16 0ng·mL- 1 范围内成线性关系 ,相关系数r =0 9996 ,检出限 0 4ng·mL- 1 ,回收率 94 2 %～ 98 5 % ,相对标准偏差不超过 4 6 %。     

原子荧光光谱法测定海水中的镉

原子荧光光谱法测定海水中镉,研究了酸度、KBH4浓度、载气流量、灯电流以及原子化器高度等因素对测定的影响,优化了测量条件,并进行了海水样品以及准确度的测定,此方法具有操作简单、基体干扰少、灵敏度高等优点,结果可靠,适用于海水中镉元素的测定。     

原子荧光光谱法测定饲料添加剂中的汞

建立了原子荧光光谱法测定硫酸盐型饲料添加剂中汞的方法,讨论了共存离子的干扰情况。在最佳实验条件下.方法的检出限达到了0.0096ng/mL,加标回收率在97.2%—109.7%之间,相对标准偏差为1.03%,被分析的硫酸盐型饲料添加剂中的共存离子对汞的测定基本无干扰。方法可用于硫酸盐型饲料添加剂中的汞的测定。     

利用氢化物原子荧光光谱法快速测定枸杞中硒的含量

在20%(V/V)盐酸溶液介质中将试样中Se(Ⅵ)充分还原成Se(Ⅳ),氢化物原子荧光光谱法测定枸杞中微量元素硒,优化最佳测试条件.检出限为0.032ng/mL,回收率在95.0%-101.0%之间.方法具有简单快捷、灵敏度高、稳定性好等优点.     

原子荧光光谱法测定土壤、水系沉积物中的碲

对土壤、水系沉积物等地球化学样品中碲的原子荧光光谱测定方法进行了一些改进.方法检出限为0.0081μg/L.对实际样品进行连续12次测定,方法精密度(RSD)为3.55%.     

The Application of Photon Counting as a Detection System in Atomic Fluorescence and Emission Spectrometry

Despite the profusion of literature associated with analytical atomic spectrometric techniques, very little has been reported concerning the development of detector systems. This is particularly surprising in view of the current trend in atomic spectrometry towards the use of non-flame atom reservoirs. These devices frequently produce weak transient signals and dc level detector systems designed for steady state measurements are in consequence often unsatisfactory. High speed recorders may be used with success providing the total response time of the various electronic components is comparable with or preferably less than that of the signal duration and only in such instances will precise measurement of the signal be achieved (1,2). The use of absolute integration techniques are obvious for this type of measurement, although their application has not been particularly forthcoming to date. Photon counting would seem to have many advantages for such purposes, although with the exception of the more general studies of Morton (3) and Malmstadt and co-workers (4) it has received so far little consideration. Indeed its use as a detection system in analytical atomic fluorescence and emission spectrometry has yet to be reported.