境外农药产品中禁限用的助剂及相关杂质名单(二)——西班牙和德国禁限用物质

介绍了西班牙和德国农药产品中禁限用助剂及相关杂质名单。     

Adsorption Equilibrium Parameters of Trace Impurities

Abstract

Atmospheric air contains various trace impurities which include oxides of nitrogen, carbon, sulphur, and light hydrocarbons. Prior to cryogenic distillation of air to produce oxygen, nitrogen, and argon, these trace impurities have to be removed since many of these compounds constitute a safety hazard in the plant. In this study, adsorption has been considered for their removal and adsorption behavior of ethylene, acetylene, nitrous oxide, acetonitrile, methyl tert-butyl ether, methyl sulfoxide, dimethyl sulfoxide, and methanol have been studied in the Henry's Law low concentration region with several different adsorbents. Adsorption equilibrium parameters have been determined with samples of Alcan pure alumina, Alcan alumina/13X composites Actiguard 600/650PC, CABSORB Chabazite, Ceca13X, and Clinoptilolite by using the concentration pulse chromatographic technique. Heat of adsorption values and van't Hoff plots have been presented.     

低浓度煤层气流态化燃烧技术的研究进展

低浓度煤层气由于热值低、流量变化大,利用较困难,大部分都未经处理就直接被排放,不仅浪费资源,而且还污染环境,引起了国内外的密切关注。较之常规的煤层气利用技术,以惰性颗粒和催化颗粒为床料的流态化燃烧技术具有热容量大、燃料适应性广的特点,在低浓度煤层气燃烧利用方面表现出巨大的潜力。为此,综述了该技术的研究现状,分析了惰性颗粒和催化颗粒作用下,床层温度、进气浓度、流化风速及气固两相流对其燃烧特性的影响,介绍了在流化床中催化燃烧反应的模型及其动力学特性,探讨了杂质性气体对气固催化反应的作用机制,明确了SO_2作用下硫酸铜的生成是催化剂硫中毒的根本原因,提出了相应的抗硫中毒措施,讨论了水蒸气对低浓度甲烷催化燃烧的影响。最后,就该技术的未来发展进行了分析与展望,得出的认识如下:①后续的研究应该侧重颗粒尺寸变化对流态化燃烧带来的影响;②应寻找更加廉价、催化活性更优的催化剂替代;③对惰性颗粒下低浓度甲烷流态化燃烧,缺乏燃烧机理分析,需要进一步从理论角度进行深度挖掘。     

电解分离-ICP-AES法测定硫酸铜中杂质元素

对硫酸铜水溶液直接进行电解,控制电解电流为3 A,电解30 min后将电解液用水稀释至100 m L并进行测定,建立电解分离-电感耦合等离子体发射光谱法(ICP-AES)测定硫酸铜中15种杂质元素(Al、Be、Ca、Cd、Co、Cr、Fe、Li、Mg、Mn、Ni、Si、Sr、V、Zn)的方法。测定各杂质元素的检出限在0.002~1.5 mg/kg之间。对硫酸铜样品中杂质元素平行测定并进行加标回收试验,各元素测定的相对标准偏差在0.62%~1.88%(RSD,n=6)之间,各元素平均加标回收率在92.22%~109.93%(n=6)之间。该方法操作简单、电解时间短,能有效去除样品溶液中的铜基体,大大降低了基体效应,具有良好的精密度和准确度,并可以对多种杂质元素同时测定。     

Ultra-trace Analysis of Enantiomeric Impurities in Proteinogenic N-Fmoc-Amino-acid Samples on Cinchona Alkaloid-based Chiral Stationary Phases

The enantiomeric purity of N_α-Fmoc-protected amino acids is crucial from the viewpoint of peptide synthesis; therefore, a sensitive high-performance liquid chromatographic protocol was developed for the identification and quantification of enantiomeric impurities of commercially available N_α-Fmoc-protected amino acids on Cinchona alkaloid quinine- and quinidine-based weak anion exchanger-type chiral stationary phases. In the course of the evaluation of the chiral chromatographic method, the effect of the mobile phase composition, nature, and concentration of different additives were optimized. The specific phenomenon that quinine- and quinidine-based chiral stationary phases behave as pseudo-enantiomers permits that the sequence of elution of the enantiomers might be reversed by simple column switching. This is quite advantageous as regards the separation of the minor component in the presence of the major one. The method developed permits detection of less than 0.01 % enantiomeric impurity in the presence of the major enantiomer.     

ICP-AES法测定三苯基膦氯化铑中的微量杂质

将三苯基膦氯化铑用硝酸、高氯酸消解,以混合酸溶解样品,用ICP-AES法测定三苯基膦氯化铑中的微量Al、Cu、Fe、Mg、Pd、Ni、Pb、Pt、Zn杂质元素含量。选择合适波长消除光谱干扰,用背景点扣除的方式消除铑对Fe、Ni、Pb、Pt、Zn的基体干扰。各杂质元素的检测范围为0.001%~0.1%,加标回收率为93.25%~117.0%,精密度(RSD)为0.18%~15.41%。与直流电弧发射光谱分析方法相比,准确度和精密度均得到提高,高纯铑基体消耗减少,操作简化。     

Sc,La对Al-Mg焊料中杂质元素偏聚的调控作用

采用金相显微镜、扫描电镜、能谱分析和X射线衍射仪,研究了添加微量钪、镧对铝镁焊料中杂质元素偏聚的调控作用. 结果表明,在铝镁焊料合金凝固过程中,铁、硅等杂质元素在晶界有偏聚效应,添加微量钪、镧可以降低铁、硅杂质在晶界的偏聚浓度. 钪与镧减轻杂质元素在晶界偏聚的效果存在差别,添加钪的合金比添加镧的合金晶界处杂质元素偏聚强度明显减弱. 造成这种差别的原因是,钪、镧对杂质元素偏聚的调控机制不同.     

A facile pathway to prepare molybdenum boride powder from molybdenum and boron carbide

Molybdenum boride is an ideal hard and wear-resistant material. In this study, a new method is proposed for preparing molybdenum boride, by which Mo first reacts with B₄C to generate the mixture of molybdenum boride and C, and then the product is decarburized by molten Ca to generate CaC₂. Pure molybdenum boride could be obtained after acid leaching to remove the by-product CaC₂. According to the experimental and thermodynamic calculation results, it is concluded that the single-phase MoB could be successfully prepared, while Mo₂B, Mo₂B₅, and MoB₄ could not be synthesized by this method. Moreover, it was found that the particle size of finally prepared MoB is determined by particle size of raw Mo powder. The residual carbon content of the product could be decreased to 0.10 wt% after first reaction at 1673 K for 6 hours and then decarburization reaction at 1673 K for 6 hours.