微波消解–石墨炉原子吸收法测定化妆品中的铅

建立了微波消解–石墨炉原子吸收光谱法测定化妆品中铅的方法。探讨了样品前处理条件、基体改性剂的选择和优化、石墨炉升温条件等对测定结果的影响。在优化的试验条件下,铅的质量浓度在0~100 ng/mL范围内与吸光度具有良好的线性关系,线性相关系数r=0.9991,检出限为0.33 ng/mL。用该法对5种化妆品中的铅进行测定,加标回收率在95.0%~106.1%之间,测定结果的相对标准偏差不大于3.6%。该方法可应用于化妆品中痕量铅的分析。     

Determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry using Pd/Mg chemical modifier and slurry sampling

Effectiveness of Pd/Mg chemical modifier for the accurate direct determination of zinc in marine/lacustrine sediments by graphite furnace atomic absorption spectrometry (GF-AAS) using slurry samples was evaluated. A calibration curve prepared by aqueous zinc standard solution with addition of Pd/Mg chemical modifier is used to determine the zinc concentration in the sediment. The accuracy of the proposed method was confirmed using Certified Reference Materials, NMIJ CRM 7303-a (lacustrine sediment) from National Metrology Institute of Japan, National Institute of Advanced Industrial Science and Technology, Japan, and MESS-3 (marine sediment) and PACS-2 (marine sediment) from National Research Council, Canada. The analytical results obtained by employing Pd/Mg modifier are in good agreement with the certified values of all the reference sediment materials. Although for NRC MESS-3 an accurate determination of zinc is achieved even without the chemical modifier, the use of Pd/Mg chemical modifier is recommended as it leads to establishment of a reliable and accurate direct analytical method. One quantitative analysis takes less than 15 minutes after we obtain dried sediment samples, which is several tens of times faster than conventional analytical methods using acid digested sample solutions. The detection limits are 0.13?µg?g^?1 (213.9?nm) and 16?µg?g^?1 (307.6?nm), respectively, in sediment samples, when 40?mg of dried powdered samples are suspended in 20?mL of 0.1?mol?L^?1 nitric acid and a 10?µl portion of the slurry sample is measured. The precision of the proposed method is 8–15% (RSD).     

Phase Systems and Post-Column Dithizone Reaction Detection for the Analysis of Organo-Mercurials by HPLC

Abstract

The suitability of HPLC (normal and reversed phase adsorption) with UV or post-column reaction detection for the analysis of organomercurials was investigated systematically. The separation of organomercurials is best carried out on a reversed phase system with a C-8 bonded phase material as the stationary phase and acetonitrile-aqueous sodium bromide mixtures as the mobile phase.

The precision and detection limit of the method and the efficiency of the extraction procedure were established. For the alkylmercury compounds the lowest limit of detection (80ppb) was obtained with the dithizone reaction detection and for the phenylmercury compounds with UV detection (60ppb). A chromatogram of a spiked fish (2ppmHg) and a river water sample (50ppbHg) is shown.     

基于气基直接还原-熔分的硼铁矿高效利用新工艺

实验室条件下,以含硼铁精矿为原料制备氧化球团,对含硼铁精矿气基竖炉直接还原-电炉熔分新工艺进行了研究.结果表明,含硼铁精矿是良好的造球原料,1 200℃下焙烧20 min后,成品球团抗压强度可达2 500 N以上,满足气基竖炉直接还原工艺要求.在H2与CO体积比大于2/5且温度在850~1 000℃条件下,含硼铁精矿氧化球团还原率达到95%的时间为15~60 min,还原膨胀率不高于15%.在高温下电热熔化DRI后硼和铁可以高效分离,硼、铁收得率均可达到98%以上,富硼渣中B2O3的质量分数在21%以上,活性可达89%左右,是"一步法"生产硼酸的优良原料.含硼铁精矿气基竖炉直接还原电炉熔分新工艺可以实现硼铁高效分离和清洁利用.     

10种蕨类植物叶表皮特征的研究

利用光学显微镜对3科5属10种蕨类植物的叶表皮形态进行了观察和研究.结果表明:(1)它们的叶表皮细胞大多为不规则型,表皮细胞垂周壁均呈深波状;(2)气孔为下生型,多呈椭圆形;共观察到9种气孔器类型(不等细胞型、极细胞型、腋下细胞型、无规则四细胞型、放射状细胞型、聚合极细胞型、横列型、带状细胞型和围绕细胞型),每种植物具有2~6种不同类型的气孔器;(3)根据叶表皮特征,支持姬蕨科与碗蕨科合并,而凤尾蕨科与铁线蕨科单独成科.研究结果为姬蕨科、凤尾蕨科和铁线蕨科植物的系统演化及分类提供科学依据.     

高炉煤气流速对蝶阀区域粉尘沉降特性影响

高炉煤气含有大量粉尘,易沉积于管道三偏心蝶阀阀座密封面底部而造成阀板卡塞或损坏,影响高炉生产并造成严重经济损失。为获取管道内部高炉煤气流速对蝶阀区域粉尘沉降规律的影响机理,使用Pro/E建立了蝶阀及其区域流场的三维模型,基于ANSYS Workbench软件的FLUENT模块,采用标准k-ε湍流模型和DPM模型,对3种高炉煤气流速条件下的蝶阀区域粉尘运动轨迹进行了模拟分析。结果表明:流速为8m/s工况下,粉尘沉积质量随阀板开度增大而呈现先降后升的趋势,而12m/s和16m/s工况下,粉尘沉积质量随阀板开度增大而降低;阀板开度15°工况下,粉尘沉积率随高炉煤气流速增大而升高,而45°和75°工况下,粉尘沉积率随高炉煤气流速增大而降低。研究结果可为高炉煤气管道蝶阀区域粉尘自动清除装置的研制提供理论参考。     

正融土强度弱化特性研究的试验仪器及方法

冻土,特别是含冰透镜体的冻土解冻时,出现强度大幅度下降的弱化现象,这是季节冻土区内路基春季翻浆冒泥、地基失稳的重要原因.为探明路基土融化过程中的强度弱化机理,在此基础上制定有效的冻害预防措施,对国产土工静力三轴仪进行了一系列改造,并配以专用的冻土试样制备设备、冻土试样融化加热设备和外部保温设施,共同制成冻土解冻时的强度弱化试验仪.用该仪器进行了相关试验研究,结果表明,仪器得到的数据合理有效,该仪器设备可以在冻土学研究中推广应用.     

原子吸收光谱分析法测定补钙剂中钙含量

利用石墨炉原子吸收分光光度计对两种葡萄糖酸钙口服液中的钙进行了检测,分析了口服液中钙的含量。该方法准确便捷,为特定溶液样品中各种微量元素的检测提供了一条很好的途径。     

质量控制图用于石墨炉原子吸收光谱法检测海水中铅元素

为保证海水中重金属检测结果的准确可靠,以铅元素为例,每个工作日使用石墨炉原子吸收光谱仪平行测定铅质控样2次,收集20组有效数据后,通过计算均值、标准差得出上下控制限、警告线及辅助限,绘制出在当前实验室环境条件、仪器设备、试剂药品和人员水平等因素条件下的质量控制图。该质量控制图不仅用于实际检测过程中对检测结果进行监控,还可为该实验室的人员考核、留样复测等实验室质量控制行为提供结果判定依据。     

Recent progress in measurements of oscillatory forces and liquid properties under confinement

The present review paper focuses on direct measurements of oscillatory forces. Beside the surface forces apparatus (SFA), atomic force microscopy (AFM) has emerged as the most commonly used technique to measure surface forces. Recent instrumental advances of both methods are highlighted in the review. Different systems, showing oscillatory forces are classified. Principle distinction is made between 1-component liquids (water, organic liquids and liquid crystals), pseudo 1-component liquids (ionic liquids and microemulsions) and 2-component liquids (dispersions containing polyelectrolytes, micelles or nanoparticles). In the last few years, the oscillatory force studies address particle characterisation, synergistic effects in multicomponent systems, the introduction of ‘switchable’ forces, and resolving liquid properties under confinement. Last but not least, the ability of AFM and SFA to measure oscillatory forces is discussed.