粉末标准曲线XRF法检测土壤中的重/类金属

建立并验证一种简便、快速、准确、可靠的土壤中7种典型重金属元素(铅、镉、汞、铬、铜、锌、镍)和1种类金属元素(砷)的粉末标准曲线XRF检测方法。研究XRF检测中土壤样品的粒度、密度、样品量、XRF检测参数及干扰效应等的影响,优化XRF检测土壤样品的前处理方法、检测条件和定量标准曲线,以建立土壤样品中铅、镉、汞、铬、砷、铜、锌、镍的XRF检测方法。研究表明,通过选择合适的滤光片,可明显提高XRF检测灵敏度;随着粒度的减小,样品均匀度不断提高,样品密度也随着提高,XRF响应也逐渐下降及稳定,相对标准偏差从1.4%~14.1%降至0.5%~2.0%,最终选择粒度200目的土壤样品4 g,装入样品罐中手动抖实后,进行XRF检测;使用土壤加标样品制作XRF检测定量标准曲线,线性相关系数r20.99,再通过土壤标准样品进行验证、校正,降低不同土壤样品基质对定量产生的影响。所建XRF检测方法与ICP-MS方法检测结果吻合度高,方法稳定性好,方法检测限低(4.5~58.9 mg/kg),其中5种元素满足GB15618-1995中一级限量标准的检测要求。土壤监测结果表明,目标区土壤均符合二级土壤限量标准,其中2个样品符合一级标准,该区土壤环境质量总体较好。     

Removal of arsenate with hydrous ferric oxide coprecipitation：Effect of humic acid

Insights from the adverse effect of humic acid(HA) on arsenate removal with hydrous ferric oxide(HFO) coprecipitation can further our understanding of the fate of As(V) in water treatment process. The motivation of our study is to explore the competitive adsorption mechanisms of humic acid and As(V) on HFO on the molecular scale. Multiple complementary techniques were used including macroscopic adsorption experiments, surface enhanced Raman scattering(SERS), extended X-ray absorption fine structure(EXAFS) spectroscopy, flow-cell attenuated total reflectance Fourier transform infrared(ATR-FTIR) measurement, and charge distribution multisite complexation(CDMUSIC) modeling. The As(V) removal efficiency was reduced from over 95% to about 10% with the increasing HA concentration to 25 times of As(V) mass concentration. The SERS analysis excluded the HA-As(V) complex formation. The EXAFS results indicate that As(V) formed bidentate binuclear surface complexes in the presence of HA as evidenced by an As-Fe distance of 3.26–3.31 ?. The in situ ATR-FTIR measurements show that As(V) replaces surface hydroxyl groups and forms innersphere complex. High concentrations of HA may physically block the surface sites and inhibit the As(V) access. The adsorption of As(V) and HA decreased the point of zero charge of HFO from 7.8 to 5.8 and 6.3, respectively. The CD-MUSIC model described the zeta potential curves and adsorption edges of As(V) and HA reasonably well.     

Graphene-supported nanoscale zero-valent iron：Removal of phosphorus from aqueous solution and mechanistic study

Excess phosphorus from non-point pollution sources is one of the key factors causing eutrophication in many lakes in China,so finding a cost-effective method to remove phosphorus from non-point pollution sources is very important for the health of the aqueous environment. Graphene was selected to support nanoscale zero-valent iron(nZVI)for phosphorus removal from synthetic rainwater runoff in this article. Compared with nZVI supported on other porous materials,graphene-supported nZVI(G-nZVI) could remove phosphorus more efficiently. The amount of nZVI in G-nZVI was an important factor in the removal of phosphorus by G-nZVI,and G-nZVI with 20 wt.% nZVI(20% G-nZVI)could remove phosphorus most efficiently. The nZVI was very stable and could disperse very well on graphene,as characterized by transmission electron microscopy(TEM) and scanning electron microscopy(SEM). X-ray photoelectron spectroscopy(XPS),Fourier Transform infrared spectroscopy(FT-IR) and Raman spectroscopy were used to elucidate the reaction process,and the results indicated that Fe-O-P was formed after phosphorus was adsorbed by G-nZVI. The results obtained from X-ray diffraction(XRD) indicated that the reaction product between nZVI supported on graphene and phosphorus was Fe3(PO4)2·8H2O(Vivianite). It was confirmed that the specific reaction mechanism for the removal of phosphorus with nZVI or G-nZVI was mainly due to chemical reaction between nZVI and phosphorus.     

Characteristics of secondary inorganic aerosol and sulfate species in size-fractionated aerosol particles in Shanghai

Sulfate, nitrate and ammonium(SNA) are the dominant species in secondary inorganic aerosol, and are considered an important factor in regional haze formation. Size-fractionated aerosol particles for a whole year were collected to study the size distribution of SNA as well as their chemical species in Shanghai. SNA mainly accumulated in fine particles and the highest average ratio of SNA to particulate matter(PM) was observed to be 47% in the fine size fraction(0.49–0.95 μm). Higher sulfur oxidation ratio and nitrogen oxidation ratio values were observed in PM of fine size less than 0.95 μm. Ion balance calculations indicated that more secondary sulfate and nitrate would be generated in PM of fine size(0.49–0.95 μm). Sulfur K-edge X-ray absorption near-edge structure(XANES) spectra of typical samples were analyzed. Results revealed that sulfur mainly existed as sulfate with a proportion(atomic basis) more than 73% in all size of PM and even higher at 90% in fine particles. Sulfate mainly existed as(NH4)2SO4 and gypsum in PM of Shanghai. Compared to non-haze days, a dramatic increase of(NH4)2SO4 content was found in fine particles on haze days only, which suggested the promoting impact of(NH4)2SO4 on haze formation. According to the result of air mass backward trajectory analysis, more(NH4)2SO4 would be generated during the periods of air mass stagnation. Based on XANES, analysis of sulfate species in size-fractionated aerosol particles can be an effective way to evaluate the impact of sulfate aerosols on regional haze formation.     

能量色散X射线荧光分析技术在环境空气质量监测中对铅测定的应用

采用EDXRF(能量色散X射线荧光法)测定环境空气中的铅,对监测数据进行了重复性、均匀性、代表性、平行性和准确性方面的分析。实验结果表明,该方法与ICP法测定结果相符,不仅有效可行,而且具有应用推广价值。     

浅谈特种设备制造和检验工作中的X射线辐射防护

介绍了x射线的辐射防护方法，并对x射线检测工作中存在的问题提出了建议。     

石油测井用中子源辐射屏蔽研究

放射源测井技术是当今石油勘探和开发中必不可少的手段，开展对测井人员的屏蔽防护研究十分必要。将聚乙（丙）烯与碳化硼和氧化铝等以不同比例混合后制成的板材和织物具有良好的热中子、中能中子和快中子屏蔽效果，加工成屏蔽装置后，可使镅－铍源中子的屏蔽率达到６２．０６％，γ射线屏蔽率达到３２．４３％，结合中子辐射防护服和防护围裙等的使用，可较好地解决测井人员的辐射防护问题。     

铅蓄电池企业废气中铅及其化合物便携式XRF检测方法

在企业污染源现场实现污染物排放浓度水平的快速判定和超标风险筛查,对生态环境管理部门提高执法效率、企业提高环境管理水平意义重大。铅是一种对人体危害极大的有毒重金属,目前缺少含铅废气中铅及其化合物的便携式直读检测设备和检测方法。探索性地将X射线荧光光谱(XRF)法应用于铅蓄电池企业含铅废气中铅及其化合物的便携式快速、直读检测。研究结果表明,基于XRF的面密度法适用于铅蓄电池企业含铅废气处理设施后铅及其化合物的快速、直读检测,相对国标方法具有快速、直读、对样品无损、便于复测等特点,可用于铅及其化合物排放浓度水平的快速判定和超标风险筛查。     

化学气相沉积法对13X分子筛孔径修饰及吸附性能研究

化学气相沉积法可对１３Ｘ分子筛进行孔径修饰，并用于含重金属离子废水的净化处理。研究结果表明，随１３Ｘ分子筛外表面ＳｉＯ２沉积量的增加，孔径收缩。