锗的分析概况

本文是关于锗分析方法的综述，共分锗的分析和分离方法，锗的定量法和有机锗Ｇｅ－１３２产量质量控制法研究现状三大部分。锗的分析和分离方法中，介绍了锗的分析方法及分类，锗样品前处理、分离与预浓集的原理和方法，并便 出了有参考价值的图表，锗的定量法中介绍了重量法、容量法、分光光度法、荧光法和发光分析法原子吸收分光光度法、原子发射光法、电化学分析法。每一分析法中又介绍了测定法研究及应用实例。在测定法研究及应     

天然药物及制剂中微量元素硒的测定方法概况

硒是人体必需的微量元素，具有抗肿瘤、防衰老、防辐射和增强机体免疫力等多种功能。本文就国内近年来对天然药物及其制剂中微量元素硒的分析方法概况作一综述，包括：原子吸收分光光度法、荧光分光光度法、电感耦合等离了光谱法、催化分光光度法、分光光度法、化学发光淬灭法、极谱法、中子活化分析法和色谱法等。     

痕量硒的分析概况

本文介绍了痕量硒的分析概况及近几年的进展,包括试样的消化、分离富集、测定方法和形态分析四个方面。在测定方法方面,着重综述了分光光度法、荧光分析法、气相色谱法、电化学分析法及原子吸收分光光度法。认为探索灵敏度更高、选择性更好的测定方法,特别是形态分析仍是今后的重要研究课题。文献118篇。     

食物中微量元素硒的分析方法研究进展

就国内近年来对食物中微量元素硒的分析方法研究进展作一综述。包括：分光光度法，荧光光光度法、原子吸收分光光度法，电感耦合等离子体发射光谱法、极谱法、色谱法和中子活化法。     

生物样品中硒的测定方法研究进展

硒是生物体必需的微量元素,硒的毒性和营养功能与其总量有关,硒的测定具有重要意义。综述了生物样品中硒的测定分析方法研究进展,包括：样品预处理方法,荧光法,原子吸收光谱法,原子荧光光谱法,电感耦合等离子体发射光谱法,吸光光度法,化学发光法,电分析法,中子活化分析法,色谱法等。     

微量元素铬的分析方法研究进展

就国内外近年来对食品，药物，环境等样品中铬元素的分析方法研究进展进行了综述。主要有分光光度法，原子吸收分光光度法，荧光分析法，化学发光法，电化学分析法，电感耦合等离子体发射光谱法，色谱法，质子诱发X－射线分析法和共振瑞利散射法。     

光度分析法测定痕量硒的研究与应用

就目前研究较多的测定痕量硒的光度分析法进行了综述,着重介绍了分光光度法、荧光光度法、散射光谱法、原子吸收光谱法、电感耦合等离子体发射光谱等方法.     

微量元素锰的分析方法研究进展

就国内近年来对食品,环境样品和生物样品中微量元素锰的分析方法研究进展作一综述。包括分光光度法,荧光分析法,原子吸收分光光度法,电感耦合等离子体发射光谱法,催化光度法,极谱法,高效液相色谱法,化学发光法和滴定法。     

稀有分散元素分析方法的研究进展

综述了1990年以来国内外关于镓、铟、铊、锗、硒和碲等稀有分散元素的样品分解方法、分离富集方法以及主要的检测方法,检测方法包括分光光度法、分子荧光光谱法、原子荧光光谱法、原子吸收光谱法、电化学分析法、电感耦合等离子体原子发射光谱法、电感耦合等离子体质谱法、中子活化分析法和化学发光法等,指出了各分析方法的特点和不足,并展望了这些方法在稀有分散元素分析中的应用前景(引用文献90篇)。     

钢铁中硫的测定方法研究进展

综述了从1979-2009年间测定钢铁中硫元素分析方法的研究进展。钢铁材料中硫元素的主要分析方法包括红外吸收光谱法、原子发射光谱法、离子色谱法、质谱法、电化学方法、分光光度法、滴定分析法、重量法和原子荧光光谱法;并对钢铁中硫元素的分析方法进行了展望(引用文献54篇)。     

Ag_2Se纳米材料的制备方法

对纳米Ag2Se的化学制备方法进行了概述,着重介绍了模板法、声化学法、水(溶剂)热法、光照合成法、微乳状液法等;展示了新近得到的不同形貌和性质的As2Se纳米晶体;并对其发展趋势和应用前景进行了展望.     

Speciation analysis of selenium in rice samples by using capillary electrophoresis-inductively coupled plasma mass spectrometry

An enzyme-assisted extraction used to extract all species of selenium in rice sample and a sensitive analytical method for the determination of ultratrace Se(VI), Se(IV), SeCys₂ (selenocystine) and SeMet (selenomethionine) with capillary electrophoresis-inductively coupled plasma mass spectrometry were firstly described in this study. The extraction method is simple, effective and can be used to extract trace selenium compounds in rice with high extraction efficiency and no altering its species. The analytical method has a detection limit of 0.1-0.9 ng Se/mL, and can be used to determine trace Se(VI), Se(IV), SeCys₂ and SeMet in rice directly without any derivatization and pre-concentration. With the help of above methods, we have successfully determined Se(VI), Se(IV), SeCys₂ and SeMet in selenium-enriched rice within 18 min with a recovery of 90-103% and a RSD (relative standard deviation, n = 6) of 3-7%. Our results indicated that selenium-enriched rice contained only one species of selenium, SeMet, and its concentration is in range of 0.136-0.143 μg Se/g dried weight. The proposed method providing a realistic approach for the nutritional and toxical evaluation of different selenium compounds in nutritional supplements.     

Comparison of sample preparation methods based on proteolytic enzymatic processes for Se-speciation of edible mushroom (Agaricus bisporus) samples

A sequential sample preparation process was developed for the speciation analysis for Se-enriched edible mushroom, Agaricus bisporus containing 110.2 mug of total Se/g sample. Five different sample extraction methods were compared and the most efficient method (a three-step process involving the use of water extraction and two proteolytic enzymes - pepsin and trypsin) proved to be the most suitable for extracting selenium, with an extraction efficiency of 75%. As the analogues of these enzymes play an important role in human digestion the bioavailability of the selenium present in the sample was estimated. Selenocystine (SeCys(2)) and Se(IV) were detected in considerable amounts (27.7 mug Se/g sample and 46.4 mug Se/g sample, respectively). For the quality control of peak identification a spiking procedure was developed, using a low selenium mushroom containing 4.3 mug of total Se/g sample. During the analysis with HPLC-HHPN (Hydraulic High Pressure Nebuliser)-AFS complicated background effects and matrix problems were observed: stable and reproducible signals generated by the low selenium mushroom and the compounds used in sample preparation were detected. The three-step sample preparation method connected with the HPLC-HHPN-AFS system proved to be applicable for the speciation analysis of the Se-enriched Agaricus bisporus.     

Selenomethionine contents of NIST wheat reference materials

Values of the total selenium and selenomethionine (Semet) content of four wheat-based reference materials have been obtained by gas chromatography-stable isotope dilution mass spectrometry methods. The total Se method is an established one, and the results obtained with it are consistent with previously-assigned values. The Semet method (previously reported by our laboratory) is based on reaction with CNBr. Our data indicate that the four wheat samples (wheat gluten, durum wheat, hard red spring wheat, and soft winter wheat), though having a 30-fold range in total Se content, all have about 45% of their total Se values in the form of selenomethionine. Investigation of the CNBr-based method suggests that additional experiments are needed to verify that all selenomethionine in the wheat samples is accounted for, but also indicates that the values obtained are within 15% of the true values. As the form in which Se occurs in foods and dietary supplements is important from a nutritional perspective, adding information about Se speciation to total Se values in appropriate reference materials makes these materials more valuable in relevant analytical work.     

Development of extraction methods for speciation analysis of selenium in aqueous extracts of medicinal plants

Advanced extraction methods have been developed for direct speciation of dissolved inorganic and organic selenium (Se) species in aqueous extracts of medicinal plants (MPs). The inorganic species of Se (SeIV and SeVI) were separated from organic forms by adsorbing inorganic Se on alumina, while the organic Se was not retained. The retained inorganic Se species was eluted with 10 mL 0.2 M HCl. The total inorganic Se species was determined after prereduction of SeVI into SeIV with concentrated HCl. The SeIV in the eluent and total inorganic Se species were then complexed with diethyldithiocarbamate. The resultant complexes were entrapped in the nonionic surfactant Triton X-114. The total Se, organic Se, total inorganic Se, and SeIV species were determined by electrothermal atomic absorption spectrometry with a modifier. The SeVI concentration was obtained by subtracting SeIV from total inorganic Se contents. The main factors affecting the methodologies were investigated in detail. Under the optimized experimental conditions, the LOD for SeIV was 50 microg/L. Among dissolved inorganic and organic Se species in aqueous extracts of MPs, organic Se species were present in the range of 74-84%, SeIV 3.62-7.47%, and SeVI 12.4-18.57% of total Se contents.     

Kinetic-spectrophotometric determination of selenium in natural water after preconcentration of elemental selenium on activated carbon

A simple, accurate, sensitive and selective method is described for rapid determination of ultra-trace quantities of selenium. Selenium (IV) was collected on activated carbon after reduction to elemental Se by l-ascorbic acid. The collected selenium was then determined based on its accelerating effect on the oxidation reaction of methyl orange with bromate in acidic media. Total amount of Se(IV) and Se(VI) were collected on AC after their reduction by hydrazine. Se(IV), Se(VI) and total selenium could be determined by the method. Selenium in the range 10-10 000 ng could be determined by the method. The method was used to the determination of Se(IV), Se(VI) and total selenium in natural water with satisfactory results.     

Comparison of ultrasound-assisted emulsification and dispersive liquid–liquid microextraction methods for the speciation of inorganic selenium in environmental water samples using low density extraction solvents

Herein, ultrasound-assisted emulsification microextraction (USAEME) and dispersive liquid–liquid microextraction (DLLME) methods based on applying low-density organic solvents have been critically compared for the speciation of inorganic selenium, Se(IV) (selenite) and Se(VI) (selenate) in environmental water samples by gas chromatography-flame ionization detection (GC-FID). At pH 2 and T = 75 °C for 7 min, only Se(IV) was able to form the piazselenol complex with 4-nitro-o-phenylenediamine. Piazselenol was extracted using an extraction solvent and was injected into a GC-FID instrument for the determination of Se(IV). Conveniently, Se(VI) remained in the aqueous phase. Total inorganic selenium was determined after the reduction of Se(VI) to Se(IV) and prior to the above procedures. The Se(VI) concentration was calculated as the difference between the measured total inorganic selenium and Se(IV) content. The effect of various experimental parameters on the efficiencies of the two methods and their optimum values were studied with the aid of response surface methodology and experimental design. Under the optimal conditions, the limit of detections (LODs) for Se(IV) obtained by USAEME-GC-FID and DLLME-GC-FID were 0.05 and 0.11 ng mL⁻¹, respectively. The relative standard deviations (RSDs, n = 6) for the measurement 10 ng mL⁻¹ of Se(IV) were 5.32% and 4.57% with the enrichment factors of 2491 and 1129 for USAEME-GC-FID and DLLME-GC-FID, respectively. Both methods were successfully applied to the analysis of inorganic selenium in different environmental water samples and certified reference material (NIST SRM 1643e).     

Surfactant/oil/water system for the determination of selenium in eggs by graphite furnace atomic absorption spectrometry

An oil-in-water formulation has been optimized to determine trace levels of selenium in whole hen eggs by graphite furnace atomic absorption spectrometry. This method is simpler and requires fewer reagents when compared with other sample pre-treatment procedures. Graphite furnace atomic absorption spectrometric (GF AAS) measurement was carried out using standard addition calibration and Pd as a modifier. The precision, expressed as relative standard deviation, was better than 5% and the limit of detection was 1 µg L^− 1. The validation of the method was performed against a standard reference material Whole Egg Powder (RM 8415), and the measured Se corresponded to 95.2% of the certified value. The method was used for the determination of the Se level in eggs from hens treated with Se dietary supplements. Inorganic and organic Se sources were added to hen feed. The Se content of eggs was higher when hens were fed with organic Se compared to the other treatments. The proposed method, including sample emulsification for subsequent Se determination by GF AAS has proved to be sensitive, reproducible, simple and economical.     

玩具、铅笔中可溶性砷、锑、硒的形态分析

对玩具、铅笔中可溶性砷、锑、硒的形态分析方法进行了研究,对原子荧光光谱法测定不同价态砷、锑、硒的方法进行了优化,建立了砷、锑、硒的原子荧光光谱形态分析方法。该方法样品加标回收率为82.0%~110.0%,测定结果的相对标准偏差为1.35%~2.22%(n=10)。     

Revisitation of mineralization modes for arsenic and selenium determinations in environmental samples

Mineralization procedures for arsenic and selenium analysis are usually limited to wet digestion methods owing to high volatility of these analytes. On the other hand, variable amounts of silicon in some types of samples imply elaborated mineralization procedures to liberate analytes which may be retained in an insoluble residue. Consequently, methods for such material generally include an hydrofluoric step followed by an evaporation to dryness. This type of mineralization is most easily accomplished using a dry ashing procedure. For plant analysis, a well validated and readily applicable dry ashing method is used for a long time in several laboratories but up today one could suppose that As and Se determinations cannot be performed after such a type of mineralization. Surprisingly, it has been observed that for plant samples these analytes are detected even after a calcination at 450 degrees C. The general usefulness of a dry ashing method for analysis of all other analytes (main, minor and trace elements) incitates us to also verify As and Se recoveries. Results obtained in this work indicate clearly that plants of terrestrial origin may be mineralized using dry ashing procedure without As and Se losses. This statement was confirmed by analyses of several reference terrestrial plant samples (RMs) and laboratory control samples. Another confirmation was given by the direct graphite furnace analysis of the same plant samples but in slurried form (SS-ETAAS). As a direct consequence, As and Se analysis in terrestrial plants no more necessitates a separate preparation methodology. On the other hand, significant losses of As and Se were observed for aquatic plants, e.g. algaes. For the analysis of this type of samples, a separate wet digestion procedure remains unavoidable if the determination of As and Se has to be considered. Also some preparation procedures were tested for As and Se-analysis of soil and sediment reference samples. In these cases the wet digestion with a mixture of nitric, perchloric and hydrofluoric acids seems to remain the best alternative.