一次消解测定蔬菜中多种重金属的简捷方法

针对一般实验室检测人员少,检测任务重的问题,研究了蔬菜通过一次湿化消解后,消解液可以测定多种重金属元素的方法,大大提高了效率,减轻了工作量.     

Measurement uncertainty of selenium determination in the reference material Seronorm Trace Elements Serum by hydride generation atomic fluorescence spectrometry

 An analytical result is not considered to be complete without a statement of the measurement uncertainty associated with it. Evaluation of measurement uncertainty is therefore an essential part of every determination. In the present study the measurement uncertainty of the result of determination of selenium in the reference material Seronorm Trace Elements Serum was studied. The combination of a digestion procedure using sulfuric acid, V₂O₅ in H₂SO₄ and hydrogen peroxide and the continuous flow approach of hydride generation atomic fluorescence spectrometry (HG-AFS) detection was used for selenium determination. The total uncertainty budget was calculated with the help of the GUM Workbench program, in which computations follow the rules of the ’ISO guide to the expression of uncertainty in measurement’. The major sources of uncertainty were found to be due to the recovery of the procedure, measurement of peak heights and the purity of Na₂SeO₃. A selenium mass fraction of 77.1±4.8 ng/g (with a coverage factor of 2.1, 95% probability) was determined, which is comparable with the recommended value of 80 ng/g. Received: 13 September 2002 Accepted: 23 December 2002 Acknowledgements We would like to thank Tinkara Buˇcar, B.Sc. for useful discussions and the IAEA Vienna, for financial support of the project 11553/RO. Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to V. Stibilj     

Synthesis of O-unprotected glycosyl selenoureas. A new access to bicyclic sugar isoureas

β-d-Gluco and mannopyranosyl selenoureas have been prepared by coupling of the corresponding glycosylamines with phenyl isoselenocyanate in aqueous pyridine. Alkyl and aryl isoselenocyanates, and 1,4-phenylene diisoselenocyanate have been obtained from the corresponding formamides with an excess of triphosgene, black selenium and triethylamine. Treatment of the O-unprotected β-d-glucopyranosyl selenourea with aqueous oxygen peroxide afforded a 1,2-trans-fused bicyclic isourea.     

Fabrication of isotype (p-p) selenium-polyaniline heterojunction diode by electrochemical method

In the present work, for the first time, heterojunction has been fabricated using electrochemically deposited isotype p-selenium-p-polyaniline from a single solution bath. The structural characterization of selenium and polyaniline thin film was carried out using XRD technique. Polyaniline exhibited amorphous structure while selenium offered monoclinic (β) phase. The junction was formed by electrodepositing polyaniline over selenium film and heating at 423 K. The current density versus voltage (J-V) plot showed the formation of a junction with ideality factor of 1.16. From J-V characteristics at different temperatures, static resistance (R_s), dynamic resistance (R_d), and rectification ratio of diodes were determined. Heat treatment above 448 K caused junction breakdown.     

54例白血病患者血清硒含量分析

以催化极谱法测定了５４例白血病患者血清硒含量。结果表明，急淋、急粒患者血清硒含量均低于正常对照组，慢粒及急、慢粒经治疗缓解者血清硒含量与正常对照组间均无显著性差异，提示低硒状态只存在于急性患者，且随病情缓解后血硒水平趋于正常，慢粒与血硒含量没有明显的相关关系。     

石墨炉原子吸收光谱法直接测定血样中硒

用石墨炉原子吸收光谱法，以硝酸铜和硝酸铵为基体改进剂，塞曼效应扣背景，采用标准加入法可直接测定血样中硒，回收率为95％～105％，相对标准偏差为5．8％，检出限为96pg，测定结果准确可靠。     

血清硒浓度与口腔鳞癌相关性研究

分析了１９９４￣１９９５年在浙江医科大学附属第一医院门诊的口腔鳞癌患者的血清的硒浓度，结果表明口腔鳞癌患者血清硒浓度极显著低于正常人群，而手术后患者血清硒浓度又极显著高于手术前患者。     

长光路光度法测定中药材中痕量硒

本文研究了用长光路光度法测定痕量硒。在酸性溶液中，Ｓｅ（Ⅳ）催化ＫＣｌＯ３氧化苯肼成偶氮离子，继而与变色酸生成红色偶氮化合物。硒含量在１．０×１０－９～２．０×１０－７ｇ／ｍＬ范围内遵守比尔定律。巯基棉分离后，测定中药材中总硒，获得满意结果。     

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.     

Solid-phase microextraction–capillary gas chromatography combined with microwave-induced plasma atomic-emission spectrometry for selenite determination

The use of solid-phase microextraction (SPME) with gas chromatography coupled to microwave-induced plasma atomic-emission detection (GC–MIP-AED) is described for selenite [Se(IV)] speciation. Aqueous standards were derivatised with sodium tetraethyl- or tetrapropylborate and extracted by SPME. Headspace extraction of the ethyl and propyl derivatives was studied. Relevant experimental conditions were optimised, including conditions for derivatisation and extraction and those of gas chromatographic analysis. The limits of detection achieved for headspace sampling of derivatised Se(IV) were in the low ng mL^–1 range for both ethylation and propylation. When the method was applied to analysis of selenite in selenised yeast reference material results were in good agreement with the indicated values.