山楂中硒的测定

用荧光法测定了山楂中硒的含量，结果表明，山楂中含有痕量硒。     

测定硒过程中湿法分解样品时防止硒损失的研究

通过对湿法分解样品常用的几种混合酸体系进行研究,发现硒有不同程度的挥发损失。本文提出在分解样品的混合酸中加入铜催化稳定剂,可防止硒损失;探讨了反应机理,提高了测定硒的准确度。用荧光法测定硒回收率达97.0～106.0%。首次应用于测定配合饲料中的硒并取得满意的效果。     

77Se solid-state NMR investigations on As(x)Se(1-x) glasses using CPMG acquisition under MAS

⁷⁷Se (I=1/2) solid-state NMR is a very sensitive probe of the local structure of selenide glasses, which themselves are promising for optical applications. In this work, we show that although ⁷⁷Se has a low natural abundance (7.58%) and a wide spectral range, the sensitivity can be dramatically increased using Carr–Purcell–Meiboom–Gill (CPMG) trains of rotor-synchronized π pulses during the detection of ⁷⁷Se magnetization but may be affected by chemical shift anisotropy when the Magic Angle Spinning rate is not fast enough and by offset effects. The indirect dimension of the T₂^CPMG-resolved spectrum shows a strong influence of the J-couplings between naturally occurring ⁷⁷Se pairs. The resulting spectra show that the structural model known as “chains crossing model” is not entirely suitable to describe the glassy network of the Se-rich compositions.     

荧光探针辅助研究硒(Ⅲ)、土霉素与DNA的相互作用

采用偶氮胭脂红(G)荧光探针作为辅助手段,利用紫外-可见及荧光光谱技术分别测定了土霉素、硒(Se2+)与DNA的相互作用的光谱,得到了土霉素-硒离子与DNA的作用方式为嵌插作用,土霉素-硒离子与DNA的相互作用的固有结合常数K为1.03×104L/mol。     

ICP-MS测定食用菌中硒的方法研究

采用石英高压消化罐在较低温度下缓慢消化食用菌样品,减少了硒的损失,以ICP-MS测定食用菌中微量硒,并对分析方法进行了研究。实验表明样品浓度、积分时间与响应值呈正相关。当样品中硒的浓度大于50 μg·L-1时,采用0.1 s的积分时间;硒的浓度小于5 μg·L-1时,采用高于2.0 s的积分时间。标准曲线在1.0～500 μg·L-1完成(r=1.000 0)。回收率为99.96%～102.7%。该法具有简便、快速、灵敏、稳定、准确等优点,用于食用菌中痕量硒的分析测定,结果令人满意。     

石墨炉原子吸收法测定麦芽粉中的锗和硒

本文叙述了平台石墨炉原子吸收法测定麦芽粉中的锗和硒，采用Ｐｄ＋Ｎｉ和Ｐｄ基体改进剂，使锗和硒的灰化温度分别提高到１４００和１２００℃，有效地消除了基体干扰。方法特征量为３１ｐｇ（Ｇｅ）和２３ｐｇ（Ｓｅ），检出限为２８ｐｇＧｅ和６２ｐｇＳｅ（３σ）。对含２２￣１１０μｇ／ｇＧｅ和１８￣３５μｇ／ｇＳｅ的样品测定，相对标准偏差为Ｇｅ３．７￣５．６％（ｎ＝９），Ｓｅ４．３￣６．５％（ｎ＝９），回收率在９     

Simultaneous Determination of Se and Te in Ores by HG-AFS After Online Preconcentration with Nano-TiO2 Immobilized on Silica GelSCIEI北大核心CSCD

A simple, sensitive and interference-free method was established for simultaneous determination of trace selenium and tellurium in ore samples by HG-AFS, by using nano-TiO2-immobilized on a silica gel packed microcolumn for online preconcentration. Selenium and tellurium were selectively adsorbed to the microcolumn in acidic condition and then completely eluted with 2% (m/v) NaOH solution. The experimental conditions for hydride generation, adsorption, elution and potential interference were investigated in detail. Under the optimum conditions, the detection limits of selenium and tellurium by the proposed method with 180 s sampling time were 4.0 and 3.6 ng.L-1, with sensitivity enhancement of 20- and 13-fold compared to conventional hydride generation method, respectively. The relative standard deviation (RSD, n=5) of this method for 1 mu g.L-1 Se(IV) and Te(IV) were 0.7% and 2.3, respectively. This method was applied to determination of selenium and tellurium in several ore samples.     

硒对钝顶螺旋藻氧化损伤的拮抗作用的光谱学特性及机制

研究了亚硒酸钠预处理对H2O2氧化胁迫下钝顶螺旋藻(Spirulina platensis)的生长、藻丝体形态、谱学特性以及细胞内活性氧(ROS)水平的影响,探究硒拮抗氧化胁迫保护螺旋藻的机制。结果显示,H2O2氧化胁迫明显抑制螺旋藻的生长,藻丝体严重受损,可见光吸收440nm峰增强,620和680nm峰降低;荧光发射和激发光谱特征峰强度明显降低,藻胆蛋白特征发射峰由660nm蓝移至650nm;红外光谱透射峰没有发生位移,蛋白质和多肽的特征谱带酰胺Ⅰ带和酰胺Ⅱ带相对强度降低;细胞内ROS相对含量显著性升高。硒预处理24h呈剂量效应地减轻由H2O2胁迫引起的氧化损伤,有效地抑制胞内ROS的过度累积,提高螺旋藻的抗氧化能力,缓解了氧化胁迫对光能捕获和传递等重要生理功能的影响。     

流动注射氢化物发生原子吸收法测定血液中硒

采用流动注射分析与氢化物发生原子吸收相结合的方法测定了血液中痕量硒。采用ＨＮＯ３－ＨＣｌＯ４体系溶解样品，取样量少，样品处理简单，快速。本法检出限为０．０６μｇ／Ｌ＾－１（３σ），进样频率为１２０－１５０样次／小时。讨论了砷对硒测定时的干扰及其排除方法，用该法测定了３００个正常人全血和７５个血清样品，其硒含量范围分别为０．０５６－０．１１８μｇｍ１＾－１和０．０４０－０．０７６μｇｍ１＾－１，回收     

Retention mechanism of calcium ferrite and compositions of ash on selenium during chemical looping gasification

Selenium pollution by coal utilization is of increasing concern. Calcium-iron (Ca–Fe) oxygen carriers (OCs) and alkali metal ions have strong inhibitory effects on selenium, which can reduce the emissions of selenium vapor. The retention mechanisms of selenium by Fe₂O₃, CaFe₂O₄, Ca₂Fe₂O₅ and bottom ash are investigated during chemical looping gasification (CLG). Iron-based OC can oxidize H₂Se(g) to SeO₂(g); furthermore, lattice oxygen is released by Fe₂O₃, contributing to the formation of an Fe–O–Se structure to retain selenium and form selenite. Because calcium ferrite is poorly oxidizing, it cannot oxidize H₂Se(g), but the CaO produced when OCs are reduced can react with H₂Se(g) to form CaSe(s), and this process can be promoted by H₂S(g). The best retention rates reached 32.301% when Ca₂Fe₂O₅ was used. In the cyclic experiment, the selenium retention of the bottom ash gradually increases. Alkali metal ions in bottom ash are the main factor in retaining selenium. Ca²⁺ and Mg²⁺ do not easily vaporize due to their high melting points; therefore, their selenium retention is significantly better than that of K⁺ and Na⁺. This research provided a new idea for the removal of selenium by using OCs and bottom ash particles during CLG.