溶膜预富集-石墨炉原子吸收法测定痕量钯

强酸性条件下 ,钯 (Ⅱ )与 5 [( 5 氯 2 吡啶 )偶氮 ] 2 ,4 二氨基甲苯 ( 5 Cl PADAT)生成紫红色螯合物 ,该螯合物可与十二烷基苯磺酸钠 (SDBS)生成离子缔合物 ,离子缔合物经 0 .3μm孔径的硝化纤维微孔滤膜富集后 ,于小体积 ( 0 .5mL)的浓硫酸中溶膜 ,用石墨炉原子吸收法 (GFAAS)测定 ,富集倍数可达 2 0 0倍 ,钯含量在 4.69× 1 0 - 1 2 ～ 7.0 9× 1 0 - 9mol/L范围内线性良好 ,检出限为 1 .78×1 0 - 1 2 mol/L。方法用于海水中痕量钯的测定。     

The ICP-MS approach to environmental studies

The certification of marine materials for trace metals is a process which challenges every technique involved, especially if a technique is as recent as inductively coupled plasma mass spectrometry (ICP-MS), Developmental work was required for several materials (natural waters, biological materials, marine sediments). It is reviewed here, in an attempt to show how one can take full advantage of ICP-MS. This includes a review of the digestion procedures developed for the multielement analysis of biological materials and marine sediments in order to minimize spectroscopic interferences. The multielement analysis of natural waters is also reviewed, in particular that of saline waters which requires a separation of the analytes from the alkali and alkaline earths elements and a preconcentration of the analytes on a column of silicaimmobilized 8-hydroxyquinoline. The potential of performing this separation/preconcentration procedure on-line is showed using both published and original results. Finally, the application of ICP-MS to speciation is illustrated by the determination of methylmercury in biological materials after extraction, and by the determination of arsenic species by high performance liquid chromatography coupled to ICP-MS.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, AustriaThe work described was carried out while the author was a Research Associate at the Analytical Chemistry Section, Chemistry Division, National Research Council of Canada, Ottawa, K1A OR9, Canada     

毛细管电泳中样品在线预富集方法

本文对高效毛细管电泳中样品在线预富集方法作了评述，包括瞬间等速电泳，反流速电泳，场放大进样，场放大排除基体和固相萃取等技术，引用文献81篇。     

环境和生物样品中铂族金属的分析研究进展

评述了近年来环境和生物样品中痕量铂族金属的分析研究进展，重点介绍了样品的预处理和分离富集技术以及检测手段等。     

Mesoporous titanium dioxide as a novel solid-phase extraction material for flow injection micro-column preconcentration on-line coupled with ICP-OES determination of trace metals in environmental samples

Mesoporous titanium dioxide as a novel solid-phase extraction material for flow injection micro-column preconcentration on-line coupled with ICP-OES determination of trace metals (Co, Cd, Cr, Cu, Mn, Ni, V, Ce, Dy, Eu, La and Yb) in environmental samples was described. Possessing a high adsorption capacity towards the metal ions, mesoporous titanium dioxide has found to be of great potential as an adsorbent for the preconcentration of trace metal ions in samples with complicated matrix. The experimental parameters including pH, sample flow rate, volume, elution and interfering ions on the recovery of the target analytes were investigated, and the optimal experimental conditions were established. Under the optimized operating conditions, a preconcentration time of 90 s and elution time of 18 s with enrichment factor of 10 and sampling frequency of 20 h⁻¹ were obtained. The detection limits of this method for the target elements were between 0.03 and 0.36 μg L⁻¹, and the relative standard deviations (R.S.D.s) were found to be less than 6.0% (n =7, c =5 ng mL⁻¹). The proposed method was validated using a certified reference material, and has been successfully applied for the determination of the afore mentioned trace metals in natural water samples and coal fly ash with satisfactory results.     

流动注射在线共沉淀预富集火焰原子吸收法测定痕量铜

研究了以Ｎｉ＾２＋－ＤＤＴＣ为共沉淀载体，流动注射在线共沉淀预富集－火焰原子吸收光谱法测定痕量铜的体系，在０．３ｍｏｌ．Ｌ＾－１的硝酸介质中，铜离子在编织反应器中与Ｎｉ＾２＋－ＤＤＴＣ（产生共沉淀，并被收集在编织器内壁上，用甲基异丁基酮（ＭＩＢＫ）在线洗脱沉积物并引入火争原子化器中测定。当富集时间为４０ｓ时，４０μｇ．Ｌ＾－１的铜１０次测定的相对标准偏差为３．０％，灵敏度提高６０倍，检出限（３σ）     

Selective Determination of Trace Mercury (II) after Preconcentration with 4-(2-Pyridylazo)-Resorcinol-Modified Nanometer-Sized SiO2 Particles from Sample Solutions

A rapid, selective method that utilize 4-(2-Pyridylazo)-resorcinol (PAR)-modified nanometer SiO₂ (nanometer SiO₂–PAR) as a new solid-phase extractant for preconcentration of trace mercury (II) has been developed. The adsorption property of nanometer SiO₂–PAR for metal ions was studied by selectively extracting different metal ions from aqueous solutions. The results revealed an excellent affinity of the nanometer SiO₂–PAR for mercury (II) in presence of interfering metal ions at pH 4. The main parameters of solid-phase extraction such as shaking time, elution and sample dilution effect were studied. The extractant shows rapid kinetic sorption, and the adsorption equilibrium of mercury (II) on nanometer SiO₂–PAR was achieved in less than 2 min. The adsorbed mercury (II) was easily eluted by 4 mL of 6 mol L⁻¹ HCl. The maximum preconcentration factor was 50. The maximum static adsorption capacity was 276 μmol g⁻¹ at pH 4. The detection limit (3σ) was 0.43 μg L⁻¹ for cold vapor atomic absorption spectrometry (CVAAS), and the relative standard deviation of the eight replicate determinations was 2.4% for the determination of 2.0 μg of Hg(II) in 100 mL water sample. The method was applied to the determination of trace mercury (II) in sample solutions with satisfactory results.     

A new apparatus for the extraction of organic compounds from aqueous solutions

A new apparatus for the extraction of organic compounds from sea water is described. With this apparatus it is possible to extract 54 standard compounds with high recovery percentages from 9 1 of sea water with 3 ml ofn-hexane. The analysis time (about 1 h) is appreciably lower than those of the extraction methods based on RP-18 and Carbopack-B adsorption (about 15 h). Furthermore, it is possible to analyze samples without filtration. An application of this method to the analysis of Tirreno sea water is reported.     

On-line enrichment system for manganese determination in water samples using FAAS

An on-line preconcentration procedure for the determination of manganese using flow-injection approach with flame atomic absorption spectrometry as a detection method is described. The proposed method is based on the complexation between Mn(II) and 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin (TCPP). Two approaches were investigated for enrichment of manganese; the formation of Mn-TCPP complex in a solution followed by its retention on a sorbent and the sorption of manganese ions onto the TCPP-modified resin. The best results was obtained for the first approach when 10⁻⁵ M reagent was on-line mixed with an aqueous sample solution and passed through the microcolumn packed with anion-exchange resin Amberlite IRA-904 for 5 min. The sorbed complexes were then eluted with 0.5 ml of 2 M HNO₃. A good precision (2.2-3.1% R.S.D. for 50 μg l⁻¹ manganese) and the enrichment factor of 30 were obtained with the detection limit of 12 μg l⁻¹ for 5 min loading time. The interference of anions and cations has been studied to optimize the conditions and the method was applied for determination of manganese in natural water samples. The results obtained by FI-FAAS and ETAAS (as a reference method) were not statistically different for a significance level of 0.05.