电感耦合等离子体质谱法测定铅锌矿中镓铟锗铊

稀散元素是铅锌矿石中重要的伴生元素,为了综合利用铅锌矿资源,在地质、选矿上经常要考查稀散元素镓、锗、铟、铊的含量。研究了利用电感耦合等离子体质谱法测定铅锌矿中镓、铟、锗、铊4种稀散元素,选取了最佳仪器分析条件,通过在线加入内标校正基体效应和接口效应,检出限分别为0.02μg·g-1、0.01μg·g-1、0.03μg·g-1和0.05μg·g-1,相对标准偏差(RSD)为0.85%~2.84%,回收率在93.3%~102.3%之间,明显优于其他分析方法。该方法样品前处理简便、快捷,测定结果准确,令人满意。     

Laser direct writing of β-Co/Ga and Mn/Ga alloy microstructures from organometallic single-source precursors

β-Co/Ga and Mn/Ga alloys have been deposited on various substrates by laser direct write chemical vapour deposition (LCVD) from novel single-source precursors. The preformed alloy stoichiometry of 1:1 defined by the metal ratio of the precursors, (CO)₄Co-GaEt₂(NMe₃) (1) and (CO)₅Mn-GaEt₂(NMe₃) (2), is retained within the deposited structures. The depositions were up to 1.5 μm thick and the lateral dimension (4 μm) was determined by the diameter of the laser focus. The deposited structures were contaminated with ∼10 at. % C and O (by AES).     

硅研磨片超声波清洗技术的研究

介绍了硅研磨片清洗的重要性,分析了影响硅研磨片质量的主要因素,即金属杂质和各种污染物.重点分析了硅研磨片表面沾污的原因,并且通过大量的实验分析得到了活性剂和碱性清洗液、去离子水的最佳体积比是0.20:1.00:10.0,清洗的最佳时间为3 min～5 min和最佳温度范围为40℃～50℃.     

超声法检测火药生产中非金属杂质的应用研究

火药生产中非金属杂质带来的安全隐患是一个尚未解决的关键问题;由于超声检测具有适应性强,检测灵敏度高、快捷,无污染,可达到无损检测等特点,选用其作为检测火药生产药料中非金属杂质的方法;对A扫描脉冲反射法应用于检测药料中杂质进行了探索研究,试验结果证实用超声法检测药料中的非金属杂质具有一定可行性.     

Optimization of Gallium concentration to improve the performance of ZnO nanopowders for nanophotonic applications

This study reports the effects of gallium concentration on the properties of doped zinc oxide nanopowders. Both pure and gallium doped zinc oxide (GZO) nanoparticles were prepared via a simple and effective sol-gel method. The structural, morphological and optical properties of synthesized GZO nanopowders were investigated using different characterization methods such as X-ray diffraction, Raman, X-ray photoelectron spectroscopy, Fourier transform infrared spectrometer, UV–Vis diffuse reflectance spectroscopy, Transmission electron microscopy, Photoluminescence spectroscopy, X-ray and ion-beam-induced luminescence (IBIL) measurements. Firstly, in the presence of Ga ions in the host the purity of synthesized sample was evaluated by X-ray diffraction analysis. X-ray photoelectron spectroscopy confirmed the presence of bonding states of Zn, O, and Ga on the surface of powders. Raman spectroscopy analysis showed that the increase of Ga content upper than 1 at.% leads to an increase in the number of defects in the ZnO lattice. Field emission scanning electron microscopy (FESEM) confirmed that the uniform integration of spherical and hexagonal rod shape particles can be found in the doped samples. According to FESEM images, the particle size of prepared nanopowders increased from 101 to 200 nm by increasing in the Ga doping concentration. The photoluminescence, X-ray and ion beam induced luminescence results of the pure and doped ZnO powders revealed novel blue-green emission band from 400 up to 550 nm at room temperature. Optical and structural studies confirmed the optimized Ga concentration is 1 at.%.     

棉短绒先打浆后蒸煮制浆新方法

棉短绒采用先打浆、后蒸煮的新制浆工艺,可去除棉短绒中80%以上的混杂物。浆料进行H₂O₂二步法蒸漂,还可去除油脂蜡质、提高白度、降低COD、节能降耗。     

电感耦合等离子体质谱法测定锡铅焊料中11种杂质元素

锡铅焊料中的杂质元素对焊点的抗氧化性、润湿性、扩展面积有重要影响,因此对其进行测定意义重大。采用硝酸、氢氟酸溶解样品,选择H₂动态反应池模式测定Fe,标准模式测定Al、P、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,同时以Sc校正Al、P、Fe、Cu,以Cs校正Zn、As、Ag、Cd,以Tl校正Sb、Au、Bi,实现了电感耦合等离子体质谱法(ICP-MS)对锡铅焊料中这11种杂质元素含量的测定。在优化的实验条件下,11种杂质元素校准曲线的相关系数均大于0.999,方法的检出限在0.002~0.80μg/g范围内,测定下限在0.007~2.73μg/g范围内。用建立的实验方法测定锡铅焊料样品中Al、P、Fe、Cu、Zn、As、Cd、Ag、Sb、Au、Bi,平行测定11次结果的相对标准偏差(RSD)为0.85%~3.5%,加标回收率为90%~110%。将实验方法应用于锡铅焊料标准物质YT9302中Al、Fe、Cu、Zn、As、Sb、Bi共7种杂质元素的测定,结果与认定值一致。     

基于Miedema模型的海绵钛铁杂质来源研究

基于二元Miedema模型和Troop三元拓展模型分别对Mg-Ti、Mg-Fe、Ti-Fe二元系及Mg-Ti-Fe三元系进行了混合焓、吉布斯自由能计算。计算结果表明,在Mg-Ti-Fe三元系中,低镁含量区域具有负值的混合焓和吉布斯自由能,即钛、铁具有较强的结合力。在镁热法海绵钛生产中,钢制反应容器为海绵钛铁杂质的主要来源,当反应容器的铁溶解进入液镁后,铁将优先与钛形成金属间化合物,并最终使其富集于靠近反应容器壁处。     

COS申请中质量研究的难点及启示

对COS申请中质量研究部分存在诸多难点(如标准更新速度快、标准品/对照品使用及来源、现场检查等)进行剖析,指出应对策略和对我们的启示。     

杂质吸附固相萃取–液相色谱串联质谱法同时测定粮食中15种真菌毒素

建立了同步检测粮食中15种真菌毒素的杂质吸附固相萃取–超高效液相色谱串联质谱方法。样品经0.1%酸化84%乙腈水溶液提取,杂质吸附柱Prime-HLB净化后,加入稳定同位素内标补偿基质效应干扰,选择Phenomenon Kinetex Bipheny l100A作为分离柱,采用梯度洗脱,超高效液相色谱–串联质谱（UPLC-MS/MS）检测,内标法定量。结果表明,15种真菌毒素的线性相关系数均大于0.996,检出限为0.2~15 μg/kg,定量限为0.8~30 μg/kg;三种基质3个添加水平的回收率为76.9%~116.1%,相对标准偏差（RSD）为1.4%~10%;对玉米基质标准物质进行检测验证,表明8种真菌毒素的检测值均在标示范围内;采用本方法检测了市售粮食135批次,共有97批样品检出真菌毒素,检出率为71%,多毒素同时污染现象较为普遍。方法可用于粮食及其制品中真菌毒素的快速检测。