国内外体内X射线荧光骨铅检测系统比较研究

血铅生物半衰期较短,只能反应人体短近铅中毒状况,存在一定局限性;骨铅生物半衰期较长,能够反应人体铅负荷的累积效应,有必要进行检测。体内X射线荧光骨铅检测系统从发明至今已有30多年的历史,文章根据激发源的不同将其分为三类系统进行分析讨论,作为国内开展相关研究工作的借鉴。     

同步辐射XRF和XANES研究重金属污染环境中小羽藓体内硫元素的生物指示作用

在实验室将小羽藓(Haplocladium)暴露于不同浓度的铅、铁、铬重金属环境下进行培育,分别应用同步辐射X射线荧光(SRXRF)方法测定小羽藓植株硫元素的含量和X射线吸收近边结构(XANES)分析不同价态的硫所占的相对含量.结果表明,暴露于铅、铁下的小羽藓植株内硫的含量明显增加,铅、铁浓度分别为400 mg/L和200 mg/L时,硫元素含量下降.培养周期为15 d时,小羽藓在100 mg/L铅胁迫下,低价硫由对照组的17.8%升高到23.6%,而同时以硫酸盐形式存在的硫由对照组的56.3%下降到51.2%.在400 mg/L铅胁迫时,低价硫含量增加到24.8%,硫酸盐中的硫所占的比例下降到48.4%.小羽藓植株内的胱氨酸、半胱氨酸、甲硫氨酸和谷胱甘肽中所含低价态硫的总相对含量增加,以硫酸盐态存在的硫相对含量明显下降.研究表明,重金属污染环境导致小羽藓硫吸收同化过程中硫元素含量和价态变化特征具有一定的生物指示作用.     

Recovery of phosphorus as struvite from sewage sludge ash

Phosphorus (P) is an element vital for all living organisms, yet the world's reserves of phosphate rock are becoming depleted. This study investigated an effective P recovery method from sludge ash via struvite precipitation. Results showed that more than 95% of the total P content was extracted from sludge ash by applying 0.5 mol/L HCl at a liquid/solid ratio of 50 mL/g. Although heavy metal leaching also occurred during P extraction, cation exchange resin efficiently removed the heavy metals from the P-rich solution. Orthogonal tests showed that the optimal parameters for P precipitation as struvite would be a Mg:N:P molar ratio of 1.6:1.6:1 at pH 10.0. X-ray diffraction analysis validated the formation of struvite. Further investigations revealed that the harvested precipitate had a high struvite content (97%), high P bioavailability (94%), and low heavy metal content, which could be considered a high quality fertilizer.     

TiO2/Ag modified penta-bismuth hepta-oxide nitrate and its adsorption performance for azo dye removal

A modified hydrophilic penta-bismuth hepta-oxide nitrate (Bi₅O₇NO₃) surface was synthesized via a precipitation method using TiO₂ and Ag as modified agents. The synthesized product was characterized by different analytical techniques. The removal efficiency was evaluated using mono-and di-sulphonated azo dyes as model pollutants. Different kinetic, isotherm and diffusion models were chosen to describe the adsorption process. X-ray photoelectron spectroscopy (XPS) results revealed no noticeable differences in the chemical states of modified adsorbent when compared to pure Bi₅O₇NO₃;however, the presence of hydrophilic centres such as TiO₂ and Ag developed positively charged surface groups and improved its adsorption performance to a wide range of azo dyes. Dyes removal was found to be a function of adsorbent dosage, initial dye concentration, solution pH and temperature. The reduction of Langmuir 1,2-mixed order kinetics to the second or first-order kinetics could be successfully used to describe the adsorption of dyes onto the modified adsorbent. Mass transfer can be described by intra-particle diffusion at a certain stage, but it was not the rate limiting step that controlled the adsorption process. Homogenous behavior of adsorbent surface can be explored by applying Langmuir isotherm to fit the adsorption data.     

共沉淀-离心-X射线荧光法快速测定表层海水中的Fe,Ni,Mn,Cu,Zn,Pb

基于共沉淀的富集作用,采用自制的离心管离心沉淀,以手持式X-射线荧光仪(XRF)测定,由此建立了表层海水中Fe,Ni,Mn,Cu,Zn,Pb的共沉淀-离心-XRF快速分析方法。测定时间为5 min/样;线性范围125μg/L～1 000μg/L,可以满足近岸表层海水中铁和锰的分析要求;基底加标200μg/L回收率为94.5%～116%;连续7次测定6种金属浓度均为500μg/L的海水加标样品,相对标准偏差(RSD)为2.86%～5.85%。与ICP-MS法比较,测定结果无显著性差异。本方法具有化学试剂污染小、方便快捷、可现场快速测定方法等优点。该方法已成功应用于厦门西港和福建九龙江河口表层海水中可溶态铁锰的现场测定,并在现场以手持式XRF对颗粒物中铁锰进行了测定,获得了该海域颗粒物中和海水中铁锰的分布。     

污水厂二级出水中难凝聚有机物的臭氧化特性

以城市污水处理厂二级出水为原水,研究臭氧化处理对水中难凝聚有机物的去除效果.结果表明单独混凝对水中有机物的去除率较低,混凝过程中未被去除的有机物属于难凝聚有机物,加入臭氧进行氧化,随着臭氧投加量的增加,二级出水色度和UV254去除率逐渐增大,而DOC去除率变化较小.当臭氧投加量(以O3/DOC计)增加至1.5 mg·mg-1时,色度、UV254和DOC的去除率分别为45%、34%和20%,说明臭氧易于与不饱和结构有机物反应,而直接氧化的矿化能力较弱.为进一步明确二级出水有机物种类和含量的变化,测定了混凝和不同臭氧投加量下有机物的相对分子质量和三维荧光光谱.结果表明混凝对有机物含量的影响很小,而臭氧能够优先氧化分解难凝聚有机物中的大分子物质,明显减弱腐殖质类物质的荧光峰强度,但不改变荧光峰位置.同时采用光电子能谱分析有机物结构的变化规律,结果表明混凝能够去除含羧基类官能团有机物,而臭氧则易于与含苯环类难凝聚有机物反应,随着臭氧投加量的增大,脂肪类饱和有机物含量有所升高.     

外绝缘用液体硅橡胶老化现象的微观表征

本文针对近年来出现在一些变电站SF6电压、电流互感器的液体硅橡胶绝缘护套出现龟裂老化这一现象,对发生老化的硅橡胶材料进行了性能测试和试验,并利用红外光谱分析、XPS分析、热失重等手段分析了其微观结构和物质组成的变化。研究发现老化后的液体硅橡胶中Si-C、Si-O官能团和Si、C、O元素的相对含量发生了变化,且随着老化程度的增加呈现出较为明显的规律,老化越严重,Si-C键含量越少,C元素的含量越少,O元素含量越多。本文认为,用官能团含量、元素相对含量可以准确地表征液体硅橡胶材料的老化程度。通过对不同老化程度的液体硅橡胶进行的憎水性、耐漏电起痕性能的试验也证实了本文的观点。     

X射线衍射法在有机药物研究中的运用

目前随着新药开发、研制过程中对测试方法要求的不断增高,X射线衍射法因其能快速准确地判断药物晶体而被广泛应用于有机药物研究的各个领域.通过对X射线衍射法中装样方法、θ角度和狭缝的选择等参数研究,以获得该方法测定有机药物成分的最佳工作条件,使该法能为有机药物测定提供满意的图谱和更准确的测定结果.     

基于光电子能谱的高含水输油管道内壁腐蚀减薄试验分析

鄂尔多斯盆地高含水输油管道内壁腐蚀减薄现象普遍,腐蚀穿孔频次逐年上升,管道安全防护管理成为难题。为了识别输油管道内壁腐蚀减薄原因,作者在分析含水率、地层水水型、溶解氧对管道内腐蚀影响的基础上选择特征试验管段,基于X射线光电子能谱技术开展管道内壁厚度变化、金相组织、腐蚀产物特性、边缘腐蚀状态研究。结果表明:高含水输油管道内壁腐蚀减薄类型为Cl+O2+H2O环境下的垢下腐蚀,以溶解氧（O2）腐蚀为主,氯离子（Cl－）腐蚀为辅;内壁腐蚀减薄原因为原油含水率过高、水中氯离子含量过高、水中含有溶解氧和介质流速偏低。     

Effect of leachates from municipal solid wastes in the surface characteristics of calcareous soils located in Central Mexico

Anthropogenic activities induce changes in a series of soil features. For example, continuous contact between soil and municipal solid waste leachates can encourage weathering processes as well as other mineral transformation reactions; consequently, the soil loses the function of environmental protection. Pollution-induced changes in the surface properties and morphology of soils have been rarely studied. In this work, the surface characteristics of calcareous soil located at a municipal solid waste disposal site in central Mexico were studied. Soil characterisation was carried out to determine the mesoporous size, particle surface area and crystallinity of collected samples. Comparison of these characteristics was made between soil in continuous contact with leachate flow and soil not in contact with leachate. The characterisation was carried out using X-ray diffraction, thermal analysis and nitrogen adsorption at 77 K. The presence of Pb, Cd, Zn, Ni and Cr was examined in both soils. Leachates in contact with this soil showed characteristics typical of liquid produced by the decomposition of municipal solid waste (pH, dissolved oxygen, redox potential and alkalinity).