砷,硒价态的离子色谱法测定研究

砷、硒是常见的多价元素,不同价态的化合物具有不同的毒性和化学活泼性。因此,监测多种样品中不同价态砷、硒的含量是十分必要的。     

硒化合物对羟基自由基作用的研究

本文选用硒代蛋氨酸(Se-Met)和无机硒化合物,采用自旋捕集技术,在温和条件下进行硒化合物与羟基自由基作用的ESR研究。实验结果表明,硒化合物对羟基自由基具有清除作用。     

锗砷硒玻璃的一些物理性质

对作者研制的ＧｅＡｓＳｅ玻璃的一些物理性质进行了测试，密度，热膨胀系数与国外一致，吸收系数优于国外，可替代国外产品。     

微量元素硒在防护自由基损伤中的作用

微量元素硒通过与谷胱甘肽过氧化酶的结合而发挥作用,清除自由基,阻断自由基引起的脂质过氧化反应,分解过氧化物,保护细胞膜,维持细胞功能的完整性。     

ICP—AES法测定玩具材料中痕量砷,硒,锑

用电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ０测定了玩具材料中的痕量砷，硒和锑。方法简便快速，回收率为９７．５％－１０２．７％，相对标准偏差小于３％。     

石墨炉原子吸收法直接测定血清中硒,砷

选用Ｐｄ－Ｎｉ－Ｔｒｉｔｏｎ Ｘ－１００为基体改进剂，用石墨炉原子吸收法直接血清中砷、硒。该法具有操作简单、快速、灵敏度高的特点，为临床测定血清中砷、硒提供了一种新方法。     

用石墨炉原子吸收法测定水质中微量砷,硒的探讨

采用石墨炉原子吸收法测定水中微量砷，硒，经大量实验条件摸索，选择不同仪器分析工作条件，找出了最佳升温程序条件，特别是原子化时气流控制，使分析方法的检出限降低为：Ａｓ０．６μｇ／Ｌ，Ｓｅ０．５μｇ／Ｌ。线性范围；Ａｓ０．０００－０．１２０ｍｇ／Ｌ，Ｓｅ０．０００－０．０２４ｍｇ／Ｌ；精密度，相对标准偏差分别为：Ａｓ１．２６％，３．６７％，Ｓｅ２．５６％，４．５７％，回收率为：Ａｓ９８．０％－１１０．     

氢化物发生-原子荧光光谱法测定大蒜中砷和硒

采用氢化物发生-原子荧光光谱法测定大蒜中砷和硒。样品经硝酸和高氯酸消解,在盐酸(5+95)溶液中,加入溶于50g·L~(-1)氢氧化钠溶液的20g·L~(-1)硼氢化钾溶液,使其与溶液中砷及硒离子反应生成氢化物。分析中采用载气流量依次为800mL·min~(-1),600mL·min~(-1),屏蔽气的流量均为1000mL·min~(-1)。试样溶液中加入硫脲-抗坏血酸混合溶液作为还原剂。于仪器中引入试样溶液0.5mL,按选定的工作条件操作。砷及硒的质量浓度分别在0.04～0.40,1.00～10.0μg·L~(-1)范围内与其荧光强度呈线性关系,方法的检出限(3s/k)砷为0.017μg·L~(-1),硒为0.314μg·L~(-1)。分别加入两元素的标准溶液作回收试验,测得砷和硒的回收率分别在95.3%～104.4%和94.7%～105.2%之间。     

A Study of Two Atomic Absorption Methods for the Determination of Sub-Microgram Amounts of Arsenic and Selenium

Abstract

Two atomic absorption accessory units were studied for the determination of arsenic and selenium in waters. One involves a flame mode while the other a flameless mode. Each was analyzed for requirements in speed per analyses, sample sizes required, potential interferences, coefficients of variation, and in overall ease in use.

Although the flameless mode could determine lower levels of arsenic and selenium than the flame mode, it was hampered by some severe interferences. Advantages of these accessories in their use over conventional wet chemical methods included: speed per analysis, elimination of time-consuming concentration steps, and elimination of using fragile equipment and noxious solvents.     

Separation and Detection of Arsenic and Selenium Species in Environmental Samples by HPLC-ICP-MS

A method is presented for arsenic speciation analysis of an oyster sample using ion chromatography coupled with an inductively coupled plasma mass spectrometry (ICP-MS) instrument. A strong anion exchange resin was employed with a step gradient elution of 0.1 mM/0.1 M K 2 SO 4 at pH 10.2. Arsenobetaine and dimethylarsinic acid were determined following extraction based on trypsin enzymolysis with 95-100% extraction efficiency. Limits of detection in the range 0.1-0.3 mg kg m 1 of arsenic were obtained for organic arsenic species. No inorganic arsenic was detected. Validation was performed using TORT-2 as a certified reference material. Although high performance liquid chromatography (HPLC) coupled to ICP-MS is an effective method for speciation analysis it is not always necessary to obtain such a detailed picture. A simple liquid chromatographic separation technique based upon mini-column technology is presented. It was developed to obtain a fast, efficient and reliable separation of inorganic from organic, i.e. assumed toxic from non-toxic, arsenic and selenium species suitable for use as an initial screening method for environmental analysis. Two types of strong anion exchange resin were tested. Excellent separation was obtained for both min-column resins and analysis times were within 7 min. Limits of detection obtained for inorganic arsenic, organic arsenic, selenomethionine, Se IV and Se VI were 1.6, 1.8, 66, 32 and 22 µg kg m 1 , respectively.     

硒与消化系统癌关系的探讨

据不同地貌、地质条件在30个县市按剖面、同步、随机取土壤样品372份．测定硒等微量元素含量．作等级相关分析显示。土壤硒含量与消化系统癌呈负相关关系．作相对危险度、剂量-效应及多因素分析,认为此负相关关系并非偶然现象．     

金膜电极—微分电位溶出法测定谷物中的微量砷

研究用金膜电极－微分电位溶出法测定谷物中的微量砷,讨论了测定的最佳条件。     

一次消解土壤样品测定汞、砷和硒

建立了测定土壤中3种挥发性元素(汞、砷、硒)的一次消解方法,确定以程序控温石墨自动消解仪+王水-氢氟酸-硼酸络合敞开体系为最佳消解体系,采用氢化物发生-原子荧光光谱法(HG-AFS)分别测定同一消解液中汞、砷、硒的含量.采用国家标物中心有证标准物质土壤环境样品GSS-1~GSS-8进行了方法验证,结果均符合标准偏差的允许范围.此消解方法相比于现行标准方法,避免了针对各元素的分次处理,简化了消解步骤,节省了前处理时间,减少了试剂消耗,提高了实验效率,适用性广、灵敏度高、检出限低,尤其适合批量样品的微量/痕量元素分析,可作为一种大规模土壤样品中重金属污染监测和治理的快捷方法.     

硒的抗突变性作用与机体免疫功能的研究

研究了在三氯甲烷致突变性试验中加入硒的影响。结果显示硒能减少Ａｍｅｓ试验中三氯甲烷诱变的回变菌落数，能使小鼠骨髓嗜多染红细胞微核率和鳙鱼外周血有核红细胞微核率明显下降。并研究了硒在细胞免疫试验中的作用，结果显示硒能使正常鼠和荷瘤鼠的肺和脾的ＮＫ细胞活性提高，能促进其脾Ｔ淋巴细胞的增殖反应，还能增加外周血Ｔ淋巴细胞数。     

Determination of Trace Arsenic and Selenium in Water Samples by Inductively-Coupled-Plasma Mass Spectrometry

Utilisation of a miniature anion-exchanger preconcentration column of Dowex 1-X8 to increase the sensitivity for As and Se determinations by inductively-coupled-plasma mass spectrometry (ICP-MS) is described. The ion signal was enhanced were 15 fold for As and 20 fold for Se. The multielement detection limits were 2 ppt (ng/L) and 33 ppt for As and Se, respectively. This flow injection ICP-MS method was applied to the determination of trace levels of arsenic and selenium in riverine reference material SLRS-2 and spring water samples.