硅藻土吸附在线柱富集-火焰原子吸收光谱法测定环境水样中痕量铜

提出了硅藻土吸附在线柱富集-火焰原子吸收光谱法测定环境水样中痕量铜的方法。利用硅藻土对环境水样中痕量铜在线预富集,浓集因子达到27.6,使火焰原子吸收光谱法的检测能力达到测定环境水样中痕量铜的要求。方法检出限为0.32μg.L-1,RSD(20μg.L-1)为3.52%,加标回收率为97.0%~105.0%。     

流动注射在线富集-FAAS测定合金钢中微量镍

提出了流动注射在线离子交换富集-火焰原子吸收光谱法测定合金钢中微量镍的分析方法.在线离子交换采用双柱正向富集和反向洗脱流路方式,使用80目732强酸型阳离子交换树脂在酸度为0.10mol/L HCl中富集样品中的Ni2+,并用2.0mol/L HCl洗脱.设计了流动注射在线离子交换富集双柱流路的操作程序,优化了各项仪器...     

原子吸收光谱法测定环境及食品样品中痕量元素的样品前处理方法的研究进展

综述了原子吸收光谱法测定环境及食品样品中痕量元素的样品前处理方法的研究进展,主要涉及原子吸收光谱法分析中常用的样品前处理方法(包括干法、湿法和微波消解等),原子吸收光谱法测定环境样品中痕量元素的样品前处理新方法(包括固相萃取、在线富集和超声波辅助技术等)和原子吸收光谱法测定食品中痕量元素的前处理新方法(包括浊点萃取法、悬浮液进样法和紫外光解法等)。     

流动注射在线萃取-火焰原子吸收法测定化探样品中痕量铊

１引言原子吸收光谱法是测定生物、地质和环境样品中铊的重要方法，但多以电热原子吸收光谱法为主。常规的火焰原子吸收光谱法由于测定灵敏度低则往往难以满足分析要求。溶剂萃取预处理直接进行原子吸收光谱测定痕量元素，可起到分离富集的作用并能提高灵敏度和选择性，而流动注射在线萃取技术与原子吸收光谱法相结合却更具有简便、安全、不污染环境等优点。本文研究了在线萃取流程中各项最佳参数，用盐酸－甲基异丁基酮（ＭＩＢＫ）将铂萃取到有机相后，将有机相直接注入火焰中进行原子吸收测定。本法检出限为５μｇ／Ｌ；相对标准偏差为１…     

微量Cu2+的乳化液膜法富集分离及原子吸收光谱测定

微量Cu2+的乳化液膜法富集分离及原子吸收光谱测定;Cu2+; 乳状液膜; 分离; 富集; 原子吸收光谱     

流动注射在线分离富集-石墨炉原子吸收光谱法测定氧化铅中痕量金

采用流动流射在线分离富集－石墨炉原子吸收光谱法测定了氧化铅中痕量金。使用本文研究的取样杯,实现了流动注射装置与石墨炉原子吸收联机测定。通过在线分离富集,提高了分析速度,消除了基体干扰,使金的测定灵敏度提高３０倍,金特征量为０．０６ｐｇ,检出限为０．０３８ｐｇ。分析了含金量为０．２＊１０＾－６％的试样,相对标准偏差。为２．６％。     

流动注射-在线富集火焰原子吸收分光光度法测定痕量铅

本文报道在流动注射分析体系中用装有黄原脂棉的微型柱对溶液中Pb2 进行在线富集后,用3.0 mol/L盐酸洗脱柱上富集的Pb2 ,然后采用火焰原子吸收光谱法在线测定痕量Pb2 ,方法的线性范围为0.5～100μg/L。与未富集前相比,测定的灵敏度可提高65倍。方法用于环境水样中痕量Pb2 的测定,回收率在97.0%～102%之间,相对标准偏差小于4.0%,分析结果满意。     

流动注射在线螯合树脂预富集火焰原子吸收光谱法测定痕量铜

研究了以国产D412螫合树脂作柱材料的流动注射在线微柱预富集火焰原子吸收光谱法测定铜的方法。选择了最佳的富集条件,在富集时间60s时,富集46倍,检出限为0.4ng·ml-1,(3σ),RSD为1.6％(20ng·ml-1Cu,n=11),分析速度为30次·h-1。井用此法进行水中痕量铜的测定。     

氢氧化铝共沉淀分离-火焰原子吸收光谱法测定富镓渣中镓

稀有金属镓是生产半导体元件的重要材料,原料90%以上来自有色金属富镓渣。镓的分析方法除了经典的罗丹明B光度法外,还可采用火焰原子吸收光谱法测定。火焰原子吸收光谱法测定镓灵敏度不高,样品预处理通常采用萃取-反萃取分离富集镓。萃取-火焰原子吸收光谱法测定镓,虽然方法简单,但预处理操作流程长,萃取剂污染环境,危害人畜健康。近年也见有机沉淀分离富集镓的报道。方法     

流动注射在线预分离富集-火焰原子吸收光谱法测定中成药中的痕量镉

应用D-411鳌合树脂作在线分离预富集柱填料,流动注射与原子吸收光谱联用测定中成药中的痕量镉。采样频率28次/h,富集倍数达46倍,线性范围0～0.020mg/L,该方法的检出限(3S,n=10)0.0285μg/L,相对标准偏差5.2%。将该方法用于中成药样品中镉的测定,结果满意。     

原子吸收法测定水样中的Cu,Zn,Cd,Pb——离子交换树脂预浓缩法

原子吸收法测定水样中的Ｃｕ、Ｚｎ、Ｃｄ、Ｐｂ——离子交换树脂预浓缩法庞文生（平顶山环保学校河南平顶山４６７０００）韩富贵燕青枝（平顶山师范专科学校化学系）关键词原子吸收分光光度法离子交换树脂预浓缩Ｃｕ、Ｚｎ、Ｃｄ、Ｐｂ测定中图分类号Ｏ６５７．３９当水...     

悬浊液直接进样非火焰原子吸收法测定蔬菜样品中微量铬的研究

本文通过用直接悬浊液进样原子吸收法对新鲜蔬菜中铬的测定,研究了各种实验条件,并建立了实际测定新鲜蔬菜中微量元素的方法。该法将可用于食品。     

Flame AAS determination of thallium in soils

The anion-exchange enrichment of TlCl(-)(4) coupled to flame AAS is applied to the determination of the total, pseudo-total (not bound in the silicate matrix) and mobile (plant available) content of thallium in soils. Ascorbic acid is used as a new efficient eluent of thallium. The limit of detection of the method is 0.04,mug/g, the relative standard deviation at the 1 mug/g level is about 3%. The method is rapid and simple.     

Preconcentration of trace elements from natural water with palladium precipitation

Palladium salts can be used as a coprecipitation carrier for the preconcentration of trace elements from natural water prior to their measurement by atomic spectrometry (AAS). The palladium is subsequently reduced by the introduction of hydrogen gas into the sample solution. The procedure is applied to the determination of Cu, Pb and Cd in seawater (enrichment factor 50) and synthetic water samples. Operating conditions have been optimized for the analysis of real samples. With the technique established an enrichment factor (500 fold) is feasible in synthetic samples. The recoveries of Cu, Cd and Pb from seawater are 95, 103 and 100%, respectively. This simple and rapid method can be applied in a wide pH-range and with complex matrices.     

Preconcentration of trace elements from natural water with palladium precipitation

Palladium salts can be used as a coprecipitation carrier for the preconcentration of trace elements from natural water prior to their measurement by atomic spectrometry (AAS). The palladium is subsequently reduced by the introduction of hydrogen gas into the sample solution. The procedure is applied to the determination of Cu, Pb and Cd in seawater (enrichment factor 50) and synthetic water samples. Operating conditions have been optimized for the analysis of real samples. With the technique established an enrichment factor (500 fold) is feasible in synthetic samples. The recoveries of Cu, Cd and Pb from seawater are 95, 103 and 100%, respectively. This simple and rapid method can be applied in a wide pH-range and with complex matrices.     

Determination of Ultra-trace Amounts of Selenium by Hydride Generation- Gold Wire Collection-Atomic Spectrometry

It is well known that mercury is the only metal which can be pre-concentration by gas phase amalgamation on a suitable noble metal such as Au,Au-Pt alloy wire, and subsequently determination by AAS and AFS. By using this technique, which only required a simple accessory, the detection limit of an analytical method can be greatly improved simply by increasing the sampling volume. Unfortunately, this enrichment technique could only be applied to Hg so far.     

Atomic-absorption spectrophotometric determination of antimony, arsenic, bismuth, tellurium, thallium and vanadium in sewage sludge

Electrothermal atomic-absorption spectrophotometry (AAS), by use of a graphite furnace, in conjunction with sample pretreatment by homogenization, was evaluated as a rapid method for the determination of bismuth, thallium and vanadium in sewage sludge. This method was compared with use of flame, electrothermal and hydride-generation (for bismuth) AAS in conjunction with conventional acid digestion and dry-ashing pretreatments and was found to be applicable to this type of sample. Comparisons were also made between flame and hydride-generation AAS in conjunction with an acid digestion pretreatment for the determination of antimony, arsenic and tellurium in sewage sludge. The hydride-generation technique was considered the better for waste-water samples because of its greater sensitivity.     

Selective preconcentration of ultra trace copper(II) using octadecyl silica membrane disks modified by a recently synthesized glyoxime derivative

A new simple and reliable method has been developed to selectively separate and concentrate ultra trace amounts of copper ion in aqueous samples for subsequent measurement by atomic absorption spectrometry (AAS). The Cu²⁺ ions are adsorbed selectively and quantitatively during passage of aqueous solutions through octadecyl silica membrane disks modified with bis(2-hydroxyphenylamino) glyoxime. The retained copper ions then stripped from the disk with a minimal amount of 0.2 M nitric acid solution as eluent, and determined by AAS. The proposed method permitted large enrichment factors of about 100 or higher.The limit of detection of the proposed method is 0.004 ng ml⁻¹. The maximum capacity of the membrane disks modified with 25 mg of ligand was found to be 280±32 μg of copper(II). The effects of various cationic interferences on the percent recovery of copper in binary mixtures were studied.The method was successfully applied to the recovery and determination of copper in several water samples.     

On-line preconcentration and determination of cobalt by chelating microcolumns and flow injection atomic spectrometry

A simple and sensitive flow injection analysis-atomic absorption spectrometric procedure is described for the determination of cobalt. The method is based upon on-line preconcentration of cobalt on a microcolumn of 2-nitroso-1-naphthol immobilized on surfactant coated alumina. The trapped cobalt is then eluted with ethanol (250 μl) and determined by flame atomic absorption spectrometry. The analytical figures of merit for the determination of cobalt are as follows: detection limit (3 S), 0.02 ng ml⁻¹; precision (RSD), 2.8% for 20 ng ml⁻¹ and 1.7% for 70 ng ml⁻¹ of cobalt; enrichment factor, 125 (using 25 ml of sample). The method has been applied to the determination of cobalt in water samples, vitamin B₁₂ and B-complex ampoules and accuracy was assessed through recovery experiment and independent analysis by furnace AAS.     

Bestimmung von Gold im ppm- bis ppb-Bereich in Selen und Erzen mittels AAS nach Anreicherung durch Extraktion und Adsorption

Zusammenfassung In einem einfachen Verbundverfahren werden ppm- und ppb-Gehalte von Gold entweder nach Extraktion mit Methacrylsäuremethylester (MME) direkt im ppm-Bereich mittels Flammen-AAS oder im ppb-Bereich nach Absorption an selenorganische Verbindungen in der Graphitküvette bestimmt. Die Nachweisgrenze in der Flammen-AAS ist 0,2 g Au/ml MME; in der Graphitküvette können noch 0.25 ng nachgewiesen werden. Die relative Standardabweichungen für die Goldbestimmungen sind bei Gehalten von 0,064 ppm in Selen 23%, bei 14 ppm 3,5%; in Bleikonzentraten bei 0,41 ppm 10,2%. Das angegebene Verfahren ist auf Erze und andere Metallkonzentrate übertragbar.

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AAS Determination of gold in the ppm to ppb range in selenium after enrichment by extraction and adsorption

Summary With a simple method ppm and ppb amounts of gold were determined either after extraction with methyl methacrylate (MME) directly by flame AAS in ppm amounts or after absorption on organoselenium compounds in ppb amounts with flameless AAS. The determination limit by flame AAS is 0.2 g Au/ml MME, by flameless AAS 0.25 ng. The relative standard deviations for the determination of gold are 23% for the determination in selenium in the range of 0.064 ppm, in the range of 14 ppm 3.5%. For lead concentrates with 0.41 ppm the relative standard deviation is 10.2%. This method may be used, too, for the analysis of other metal concentrates and ores.

Für die Gewährung eines Stipendiums (L.F.) danken wir der Alexander von Humboldt-Stiftung.