X射线荧光光谱法测定土壤样品中铅的不确定度评定

用实例对X射线荧光光谱法测定土壤样品中铅的不确定度进行了评定.测量结果的不确定度由仪器综合稳定性、制样、标准物质、回归工作曲线、重复测量等所引入的不确定度分量组成.在对各个不确定度分量进行量化的基础上,通过合成得到测量结果的标准不确定度,再乘以95%置信概率下的扩展因子2,得到测量结果的扩展不确定度.     

进口含锌物料的表征和鉴别

采用X射线荧光光谱(XRF)、X射线衍射光谱(XRD)等分析手段,对4种进口疑似固体废物的含锌物料进行了表征。通过分析含锌物料的主要元素组成、物相组成和常规理化特征,结合外观特征,与含锌矿物、含锌产品及相关文献资料等进行比对,推导出含锌物料的产生来源。然后,参照我国《进口废物管理目录》得出鉴别结论。结果表明:4种含锌物料分别为锌矿、湿法冶炼锌浸出渣、热镀锌灰和固定CO2产物;后3种属于我国目前禁止进口的固体废物。     

磷对降低土壤中铅的生物有效性的X-衍射及电镜分析

通过盆栽实验,对不同磷化合物处理的铅污染土壤和植物分别进行X-衍射(XRD)、能谱扫描电镜(SEM-EDS)及能谱透射电镜(TEM-EDS)分析.结果显示,不同磷化合物处理土样的X-衍射图在0.288 nm、0.296 nm及0.321 nm处有明显衍射峰生成,以SSP5、HA5及HASSP2处理土样的X-衍射谱图中生成的衍射峰比较明显,而PR5处理的衍射峰相对较弱,其原因可能与磷矿粉的弱溶解特性有关.这显示了土壤经不同磷化合物处理后,土壤中新生成了较多的磷酸铅及Ca-Pb磷酸铅盐的沉淀,不同程度地降低了土壤中铅的迁移和转化特性.对植株根系的SEM分析结果表明,土壤中加入不同的磷化合物处理后,磷酸铅类化合物在植株根表细胞有明显的晶体沉淀物.对植物根细胞的透射电镜分析结果发现,在不同磷处理土壤中,铅以不同的磷酸盐化合物的形式沉淀在植物的细胞壁及细胞间隙,从而有效地阻止了铅离子向原生质细胞及植物中柱内的迁移,不同程度地降低了污染土壤中铅的蓄积毒性.     

X射线荧光光谱法测定土壤及底泥中多种元素

采用粉末压片、X射线荧光光谱法测定土壤及底泥样品中铜、铅、铬、锌、镍等多种元素.优化了测量条件,采用理论α系数法校正基体效应,校准样品校正谱线重叠干扰,经标准样品及不同分析方法验证,该方法定量准确,分析速度快,精密度和准确度均符合要求.     

X射线荧光分析法及其在环境监测中的应用

综述了X射线荧光分析法在水质分析和大气颗粒物分析中的应用,介绍了粉状固态物、液体、气体等环境试样的制备方法,以及标准曲线法、标准加入法、内标法、散射线监控法、稀释法等定量分析方法,指出X射线荧光分析法前处理简单,分析精度高,操作简便、快速．在环境监测领域具有广阔的发展前景。     

Analysis for Chemical Characterization of Atmospheric Aerosols Application of X-ray Microprobe System and Double Thin Film Method

The X-ray microprobe system was applied to ultra trace characterization of single Kosa aerosols and non-Kosa aerosols simultaneously collected at Yasaka, Japan and TaeAnn, Korea. We demonstrated remarkable mass increase of heavy metals as well as soil components in individual particles during the Kosa event compared with the non-Kosa period at Yasaka. Backward trajectory analysis suggested that the Kosa samples were in the mixing state of mineral components and anthropogenic heavy elements. Double thin film method was applied to investigate the seasonal change of the mixing states of single sea-salt aerosols associated with chlorine loss due to the heterogeneous reactions between sea-salt particles and acidic gases. It was revealed that the percentages of both chloride-nitrate mixed particles and sulfate-nitrate ones were larger in wintertime than those in summertime and fraction of chloride-nitrate mixed particles increased with an increase of particle size. Comparison between the size-segregated bulk analysis and the single particle analysis demonstrated that remarkable chloride depletion occurred in coarse particles sampled on May in the former analysis, while chloride depletion in coarse particles was not marked in the latter analysis. The discrepancy attributes to the difference of the sampling time between both analyses because significant change of air mass route occurred during the bulk sampling after completion of the single particle sampling.     

能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素

建立了偏振能量色散X射线荧光光谱法测定土壤和沉积物中稀土元素的方法,该方法较传统的方法具有前处理简单、测量自动化程度高、灵敏度高和检出限低(检出限范围为0.05~2.80 mg/kg)等优点。对土壤和沉积物标准物质的测定结果表明:测定结果与认定值能较好吻合,相对标准偏差范围为0.2%~9.4%,能满足测试的需求。分别用该方法和电感耦合等离子体质谱法对实际样品进行测定,2种方法的测定结果有较好的一致性,表明该方法测定结果准确可靠,可用于实际样品的测定。     

Simulation and source identification of X-ray contrast media in the water cycle of Berlin

This article describes the development of a model to simulate the fate of iodinated X-ray contrast media (XRC) in the water cycle of the German capital, Berlin. It also handles data uncertainties concerning the different amounts and sources of input for XRC via source densities in single districts for the XRC usage by inhabitants, hospitals, and radiologists. As well, different degradation rates for the behavior of the adsorbable organic iodine (AOI) were investigated in single water compartments. The introduced model consists of mass balances and includes, in addition to naturally branched bodies of water, the water distribution network between waterways and wastewater treatment plants, which are coupled to natural surface waters at numerous points. Scenarios were calculated according to the data uncertainties that were statistically evaluated to identify the scenario with the highest agreement among the provided measurement data. The simulation of X-ray contrast media in the water cycle of Berlin showed that medical institutions have to be considered as point sources for congested urban areas due to their high levels of X-ray contrast media emission. The calculations identified hospitals, represented by their capacity (number of hospital beds), as the most relevant point sources, while the inhabitants served as important diffusive sources. Deployed for almost inert substances like contrast media, the model can be used for qualitative statements and, therefore, as a decision-support tool.     

Optimizing the preparation parameters of mesoporous nanocrystalline titania and its photocatalytic activity in water: Physical properties and growth mechanisms

Titania nanomaterial with an anatase structure and 5.6 nm crystallite size and 280.7 m² g⁻¹ specific surface areas had been successfully prepared by sol–gel/hydrothermal route. The effect of pH as a type of autoclave and calcination was studied. Crystallite size and phase composition of the prepared samples were identified. X-ray diffraction analyses showed the presence of anatase with little or no rutile phases. The crystallite size of the prepared TiO₂ with acidic catalyst was both smaller than that prepared with basic catalyst, and was increasing after acidic calcinations by a factor 4–5. Basic calcinations produced a specific increase of 1.5. Rutile ratio and the particle size were increased after calcination at 500 °C. However, TiO₂ powder synthesized using a basic catalyst persisted the anatase phase and a loosely aggregation of particles. Anatase TiO₂ as prepared with acidic catalyst in Teflon lined stainless steel autoclave demonstrated the highest photocatalytic activity for degradation of 2,6-dichlorophenol-indophenol under ultraviolet irradiation with t_½ 0.8 min.