表层沉积物(生物膜)非残渣态组分的选择性萃取分离及其吸附铜/锌的特性

采用化学萃取技术对表层沉积物(生物膜)的非残渣态组分(铁、锰氧化物及有机质)进行了分离, 并研究了表层沉积物(生物膜)非残渣态和残渣态组分吸附铜、锌的特性. 结果表明, 0.1 mol/L NH2OH·HCl+0.1 mol/L HNO3, (NH4)2C2O4-H2C2O4缓冲溶液和体积分数为30%的H2O2可选择性地萃取分离表层沉积物(生物膜)非残渣态的锰氧化物、铁锰氧化物和有机质, 萃取率为63.15%～97.59%, 同时对非目的组分影响较小; 表层沉积物(生物膜)及其各组分对铜的吸附能力均大于对锌的吸附能力, 且生物膜及其各组分对铜、锌的吸附能力均高于表层沉积物及其相应组分对铜、锌的吸附能力; 表层沉积物(生物膜)非残渣态组分对铜、锌的吸附能力均大于残渣态组分, 且非残渣态组分中锰氧化物的单位吸附能力最强, 其次是铁氧化物, 而有机质的单位吸附能力较弱, 比锰氧化物低2个数量级, 说明生物膜对水体中痕量重金属的迁移转化作用强于表层沉积物, 而表层沉积物(生物膜)中金属(铁、锰)氧化物对水中痕量重金属起主要控制作用.     

采集的生物膜中痕量重金属的形态分布特征

采用改进的Tessier连续萃取方法对从松花江中采集的生物膜中锰、 铁、 铜、 铅、 锌及镉的化学形态进行分析, 考察了生物膜上铁、 锰氧化物和有机质吸附重金属的相对作用, 同时讨论了在研究培养的生物膜吸附痕量重金属时所建立的选择性萃取方法对于采集的生物膜组分分离的适用性. 研究结果表明, 在采集的生物膜上痕量重金属以铁、 锰的氧化物为主要结合形态存在, 以此种形态存在的铜、 锌、 铅和镉分别占其总含量的62.9%, 58.3%, 53.8%和32.6%, 而以有机结合态存在的铜、 锌、 铅和镉, 分别占其总含量的1.1%, 0.6%, 9.9%和1.8%, 表明采集的生物膜上铁、 锰氧化物在吸附重金属的过程中起主要的控制作用, 而有机质的作用相对较小, 与以往利用选择性萃取技术研究培养的生物膜吸附重金属的规律一致. 进一步分析表明, 如扣除生物膜上铁的残渣态部分, 则选择性萃取分离技术可以有效地将采集的生物膜上的铁、 锰氧化物及有机质分离开.     

自然水体生物膜吸附Co,Ni和Cu的特征研究

研究了在自然水体中培养的生物膜吸附Co,Ni和Cu等3种重金属的热力学和动力学特征,并对生物膜吸附各重金属的热力学数据进行了非线性拟合.结果表明,3种重金属的吸附过程均符合Langmuir吸附等温曲线.在溶液中重金属浓度<0.5μmol/L时,生物膜对3种重金属元素的吸附能力顺序是Co>Cu>Ni;在重金属浓度>0.5μmol/L时,顺序是Cu>Co>Ni.对动力学数据进行非线性拟合的结果表明,生物膜对Co,Ni和Cu的吸附均在数小时内达到平衡,吸附过程符合Langmuir等动力学曲线.     

A Comparison of Conventional and Ultrasound-Assisted BCR Sequential Extraction Methods for the Fractionation of Heavy Metals in Sewage Sludge of Different Characteristics

The purpose of this study was to determine the heavy metal (HM: Cd, Cr, Cu, Ni, Pb, Zn, and Hg) content in particular chemical fractions (forms) of sewage sludge with different characteristics (primary and dewatered sludge) using conventional (CSE) and ultrasound-assisted (USE) BCR sequential extraction methods (Community Bureau of Reference, now the Standards, Measurements and Testing Programme). The concentrations of HMs were determined using inductively coupled plasma optical spectrometry (ICP-OES). Only mercury was assayed with cold vapor atomic absorption spectrometry (CVAAS). Ultrasound treatment was conducted in the ultrasonic bath (Sonic 5, Polsonic). The optimal sonication time (30 min) was determined using ERM-CC144 (Joint Research Center; JCR) certified reference material. The conducted experiment revealed that the use of ultrasound waves shortened the extraction time to 4 h and 30 min (Stages I to III). The recoveries (R_M) of heavy metals ranged from 62.8% to 130.2% (CSE) and from 79.8% to 135.7% (USE) for primary sludge, and from 87.2% to 113.2% (CSE) and from 87.8% to 112.0% (USE) for dewatered sludge. The only exception was Hg in dewatered sludge. The conducted research revealed minor differences in the concentrations and fractionation patterns for Cd, Ni, and Zn extracted from sludge samples by the tested methods. However, it was confirmed that the above findings do not significantly affect the results of a potential ecological risk assessment (with minor exceptions for Cd and Zn in the primary sludge), which is extremely essential for the natural use of sludge, and especially dewatered sludge (the final sludge). The shorter extraction time and lower energy consumption prove that ultrasound-assisted extraction is a fast and simple method for HM fractionation, and that it provides an alternative to the conventional procedure. Therefore, it can be considered a “green method” for the assessment of the bioavailability and mobility of heavy metals in solid samples.     

Investigation of Adsorption Rates of Pb, Cd, Cu, Co and Ni to Fresh-water Surface Coatings Developed in Nanhu Lake

IntroductionSurfacecoatingsaccountforawiderangeofmi crobialorganismsontheearth[1] ,formonthevarioussurfacesundervariedconditions ,andcoverthesur facesofallthematerialsinrivers,lakes ,andwet lands ,suchasrocksandsediments[2 ] .Theyplayadominantroleindeterminingthetransportandulti matefateofcontaminantsinnaturalaquaticenviron ment,whichisduetoinpartthatcontaminantsmustreachandcrosssurfacecoatingsbeforetheycontactthesubstrates[3] .Ithasbeenprovedthatamongthemaincomponentsinsurfacecoatings,mangane…     

Comparison of Pb, Cd Adsorption to Surface Coatings Developed in Natural Waters with that in Plant Effluents

The comparative studies of Pb and Cd adsorption to the surface coatings (Fe, Mn, AI oxides, organic materials, and associated minerals), which were developed on glass slides in five natural and two technical waters (plant effluents), were carried out under controlled |aboratory conditions(mineral salts solution with defined speciation, ionic strength 0.05 mol/L, 25 ℃ and pH 6. 0). The classical Langmuir adsorption isotherm was applied to estimating the equilibrium coefficients of Pb and Cd adsorption to the surface coat-ings. The results show that the maximum adsorption of Pb and Cd to the surface coatings mentioned above varied widely. There was a systemic increase in the maximum adsorption of Pb and Cd to the surface coatings with increasing the contents of Mn and Fe oxides in the surface coatings in significant correlation, respective-ly, not only highlighting the relative importance of the metal oxide fraction for Pb and Cd adsorption to the surface coatings developed in natural and technical water samples, but also implying the same adsorption mechanisms of Pb and Cd to the surface coatings developed both in natural and technical water samples.     

磷酸溶液中DDA在锌表面的吸附及其缓蚀作用

采用失重法及电化学法研究了锌在含或不含十二烷基胺（DDA）的磷酸溶液中的腐蚀作用，得出相应的动力学方程，求得有关的动力学及热力学参数.用光电子能谱（XPS）检测发现，在40～70 ℃区间，锌在磷酸溶液中生成Zn(OH)x覆盖层，表现出较强的自缓蚀效果，而在30～40 ℃区间，因DDA以及, 等微粒同时吸附在锌表面，DDA在磷酸溶液中表现出较强的缓蚀作用.用吸附理论讨论了这种缓蚀作用产生的原因.     

Optimization Studies of Porous Carbon Preparation from Oil Shale Using Response Surface Methodology and Its Application for Phenol Adsorption

This paper discusses the elaboration of adsorbents from oil shale. The experimental designs a response surface methodology(RSM), which has been applied to optimize the significant preparation factors, such as temperature, time, and the activating agent percentage. The results obtained from central composite design(CCD) revealed that the interaction between the factors was significant for the maximum quantity of adsorption(response). Planned results have shown that a maximum quantity of adsorption for methylene blue is 65 mg/g, which could be achieved with a temperature of 275℃ over 2 h and a percentage of the activating agent of 45%. The predicted values agreed with the experimental finding, with a determination coefficient(R²) of 0.96. The model has been validated by experiments after conditions optimization. The new material(RHO) was characterized by cation exchange capacity, zero charge pH, surface functions, X-ray fluorescence, specific surface area, and electron microscopy analysis. Phenol adsorption was determined using Langmuir, Freundlich and Temkin, which were used to describe the adsorption isotherms. The adsorption capacity of the material was about 263 mg/g, and the kinetic studies showed rapid adsorption.     

The role of chemometrics in single and sequential extraction assays: a review: part I. Extraction procedures, uni- and bivariate techniques and multivariate variable reduction techniques for pattern recognition

Element mobility and availability in natural solid matrices can be studied with single and sequential extraction procedures; such procedures provide reliable and useful information only if the experiments are correctly planned and executed and the results are properly interpreted. Chemometrics can be a valuable tool for these aims, especially taking into account the large amounts of data generated with extraction essays and the complexity of the processes under investigation. This review deals with the application of chemometrics in research studies involving single and sequential extractions on soils or sediments, for several purposes: the development and optimization of the extraction conditions, the calculation of element fractionation, the visual illustration of the experimental results, the acquisition of different areas of information, including relationships among variables, similarities and differences among samples, causes of the observed behaviour (e.g. source identification), risk assessment, models and predictions of future events. In Part I of the review, following an overview on extraction procedures, the applications of univariate and bivariate chemometric methods are reported; then the principles of multivariate techniques for pattern recognition based on variable reduction, their applications and the main findings obtained are addressed.     

富勒烯烟炱的吸附性及其在大气挥发性有机物分析中的应用

研究了富勒烯烟炱对挥发性有机物(VOCs)的吸附作用.17种VOCs气体在烟炱上的比保留体积V_g²⁰为17.4～2634L/g.富勒烯烟炱充填的吸附管对VOCs气体的吸附-热脱附回收率在40.8%～117%之间,大部分为(100±20)%.结果表明,富勒烯烟炱能够用于吸收和富集大气中痕量的VOCs     

Selective and competitive removal of three basic dyes from single,binary and ternary systems in aqueous solutions: A combined experimental and theoretical study

The present study evaluates the selective and competitive adsorption of three basic dyes, namely, Basic blue 9 (BB9), Basic blue 41 (BB41) and Basic yellow 28 (BY28) from single, binary and ternary solutions onto natural safiot clay (NSC). For this, the effect of various parameters such as initial pH, initial dye concentration, adsorbent dose and temperature of the solution was studied and examined in a batch mode. The tested adsorbent was characterized by X-ray fluorescence (XRF), Scanning Electron Microscopy (SEM), Dispersive X-ray spectroscopy (EDX), Fourier Transform Infrared (FT-IR) and X-Ray Diffraction (XRD). XRF results indicate high percentages of SiO₂ (47.44%) and Al₂O₃ (31.24%). X-ray diffraction diffractogram identified kaolinite as the main mineral phase in the presence of quartz, illite, calcite, and dolomite. The adsorption data were examined by Langmuir, Freundlich and Dubinin-Radushkevich isotherms. It was found that for single, binary and ternary systems the results indicated that Langmuir model provided the better correlation of experimental data. The experimental results obtained demonstrate high adsorption efficiency of dyes in the mono and multi systems by NSC. DFT calculations show that BB9 (ω = 6.18) is more electrophilic than BB41 (ω = 4.10) and BY28 (ω = 2.60) which indicates that BB9 is adsorbed first and favored compared to BB41 and BY28. Moreover, Molecular dynamics (MD) and Monte Carlo (MC) simulations are used as a powerful tool to provide a better theoretical scenario for understanding the mode of adsorption on the natural safiot clay (NSC).     

固相萃取净化-离子色谱测定不同生长期新鲜烟叶中的7种无机阴离子

目的 为了研究不同生长期新鲜烟叶中无机阴离子的含量和变换规律,建立了一种固相萃取净化/离子色谱方法测定新鲜烟叶中的7种无机阴离子（F-,Cl-,Br-,NO2-,NO3-,SO42-,PO43-）。方法 样品经0.1 mol/L NaOH水溶液超声提取,萃取液经RP1.0cc固相萃取柱净化后,使用AS11-HC（4 mm×250 mm）色谱柱进行分离,以KOH为流动相,梯度洗脱。 结果 7种无机阴离子在0.10-5.0 μg/mL范围内具有较好的线性（r>0.996）,检出限在0.01-0.04 μg/mL之间,定量限在0.04-0.14 μg/mL之间,加标回收率为96.3%～102.1%,相对标准偏差（RSD%）在2.7%~4.8%之间。结论 方法前处理操作简单,7种无机阴离子分离好,检测灵敏准确,可用于不同生长时期新鲜烟叶样品中多种无机阴离子含量的检测分析。     

Sequential injection analysis for benzophenone-4 and phenylbenzimidazole sulphonic acid in sunscreen sprays by solid-phase extraction coupled with ultraviolet spectrometry

A sequential injection UV method was developed to determine benzophenone-4 (BZ4) and phenylbenzimidazole sulphonic acid (PBS) simultaneously, these being the most commonly used UV-filters in aqueous formulations used as sunscreen sprays. The selective elution of both was performed by on-line solid-phase extraction, by retention on a SAX microcolumn and separation by varying the pH of elution. The sensitivity obtained was 0.042±0.001 ml μg⁻¹ for PBS and 0.0159±0.0003 ml μg⁻¹ for BZ4. The limit of detection was 1.6 μg ml⁻¹ for PBS and 0.6 μg ml⁻¹ for BZ4. The R.S.D. of the results was 1-6% for PBS and 1-12% for BZ4. The method was validated using commercial sunscreen formulations with concentrations determined by a liquid chromatographic procedure. The two procedures gave comparable results. Automation of the method means the amount of reagents used and residues generated are decreased. The system allows the required analysis sequence to be programmed using suitable software.     

聚甲基三氟丙基硅氧烷固相微萃取涂层的制备及其对海水中酚类化合物的分析

采用溶胶-凝胶技术制备了聚甲基三氟丙基硅氧烷(PTFPMS)涂层,并将其作为萃取     

光纤SPR传感器的结构、膜材与应用进展

光纤表面等离子共振(Fiber optic surface plasmon resonance,FO-SPR)传感器由于体积小、易携带、抗电磁干扰等优点在生物、化学、医学及食品领域均具有广阔的应用前景。该文综述了光纤SPR传感器的结构、膜材料及其应用进展。其中终端反射式和在线传输式是光纤SPR传感器最重要的两种结构;最常用的膜材料包括金膜、银膜、复合膜和金属纳米颗粒。基于光纤SPR的实时检测、抗干扰能力强、可多通道检测等特点展望了其未来发展与应用前景。     

氯化1-乙基-3-甲基咪唑离子液体表面印迹聚合物的合成及其特异吸附和固相萃取性能研究

以氯化1-乙基-3-甲基咪唑(C₂mimCl)离子液体为模板分子, 甲基丙烯酸和乙二醇二甲基丙烯酸酯为双功能单体, 聚苯乙烯-二乙烯苯为载体, 制备了C₂mimCl表面印迹聚合物(C₂mimClMIP/PS-DVB). 采用红外、扫描电镜和Brunauer-Emmett-Teller分析技术对C₂mimClMIP/PS-DVB进行了表征. 通过静态吸附实验研究了C₂mimClMIP/PS-DVB对模板分子及其结构类似物的吸附行为和选择性识别特性. 结果表明, 聚合物对C₂mimCl和氯化1-丁基-3-甲基咪唑(C₄mimCl)两种离子液体有高度的选择性识别作用. 将C₂mimClMIP/PS-DVB作为固相萃取(SPE)剂制备成SPE柱, 并与高效液相色谱联用, 考察了C₂mimClMIP/PS-DVB的动态吸附性能. 结果表明, 在选定的参数条件下, SPE柱能够从结构类似物中选择性分离富集C₂mimCl和C₄mimCl, 且具备很好的稳定性和可再生性能. 将SPE柱用于地下水中C₂mimCl的分离富集, 显示出良好的实用性能.     

不粘锅涂层中全氟辛酸及其盐的快速溶剂萃取-气相色谱-质谱法测定

建立了不粘锅涂层中全氟辛酸(PFOA)及其盐残留量的气相色谱-负离子化学电离质谱（GC/NCI-MS）测定方法。样品经快速溶剂萃取仪提取及衍生化处理后进行GC/NCI-MS测定。PFOA的定量检测限为5 μg/kg;4个添加水平的平均回收率为90.9%~96.2%,相对标准偏差为1.37%~6.37%。该方法提取时间短,提取效率高,衍生化步骤简单,杂质干扰小,灵敏度高,适用性强。     

Comparison of Supercritical Fluid Extraction with Solvent Sonication for Chemical Warfare Agent Determination in Alkyd Painted Plates

Supercritical fluid extraction (SFE) of alkyl alkylphosphonofluoridates and dialkyl alkylphosphonates from painted plates was investigated. It was found that SFE recoveries compared favorably with conventional solvent sonication results. Stability studies of the samples were carried out over a period of two months. This investigation showed that the concentration of phosphonofluoridates decreased over a long period.