ASE-气相色谱法测定油田区土壤中多种石油烃

采用气相色谱法测定油田区土壤中C_(10)～C_(40)的石油烃,通过优化加速溶剂萃取的条件,使方法在62 mg/L～3 100 mg/L范围内线性良好,方法检出限为4.8 mg/kg。用该方法测定石油区短期、中期、长期油井污染土壤样品,5次测定结果的RSD为1.3%～5.2%,加标回收率为84.8%～98.5%,有证标准样品测定结果在可信区间内。     

加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。     

Heavy metal contamination in the vicinity of an industrial area near Bucharest

BACKGROUND, AIMS AND SCOPE: Chromium enters into the aquatic environment as a result of effluent discharge from steel works, electroplating, leather tanning industries and chemical industries. As the Cr(VI) is very harmful to living organisms, it should be quickly removed from the environment when it happens to be contaminated. Therefore, the aim of this laboratory research was to develop a rapid, simple and adaptable solvent extraction system to quantitatively remove Cr(VI) from polluted waters. METHODS: Aqueous salt-solutions containing Cr(VI) as CrO4(2-) at ppm level (4-6 ppm) were prepared. Equal volumes (5 ml) of aqueous and organic (2-PrOH) phases were mixed in a 10 ml centrifuge tube for 15 min, centrifuged and separated. Concentrations of Cr(VI), in both the aqueous and organic phases, were determined by atomic absorption spectrometry. The effects of salt and acid concentrations, and phase-contact time on the extraction of Cr(VI) were investigated. In addition, the extraction of Cr(VI) was assessed in the presence of tetramethylammonium chloride (TMAC) in 2-PrOH phase. Effects of some other metals, (Cd(II), Co(II), Cu(II), Ni(II) and Zn(II)), on the extraction of Cr(VI) were also investigated. RESULTS AND DISCUSSION: The Cr(VI) at ppm level was extracted quantitatively by salting-out the homogeneous system of water and 2-propanol(2-PrOH) using chloride salts, namely CaCl2 or NaCl, under acidic chloride media. The extracted chemical species of Cr(VI) was confirmed to be the CrO3Cl-. The ion-pair complex extracted into the organic phase was rationalized as the solvated ion-pair complex of [2-PrOH2+, CrO3Cl-]. The complex was no longer stable. It implied the reaction between extracted species. Studies revealed that salts and acid directly participated in the formation of the above complex. Use of extracting agents (TMAC) didn't show any significant effect on the extraction of Cr(VI) under high salting-out conditions. There is no significant interference effect on the extraction of Cr(VI) by the presence of other metals. The Cr(VI) in the organic phase was back-extracted using an aqueous ammonia solution (1.6 mol dm(-3)) containing 3 mol dm(-3) NaCl. The extraction mechanism of Cr(VI) is also discussed. CONCLUSIONS: Salting-out of homogeneous mixed solvent of 2-propanol can be employed to extract Cr(VI) quantitatively, as an ion-pair of [2-PrOH2+ * CrO3Cl-] solvated by 2-PrOH molecules. Then, the complex becomes 'solvent-like' and is readily separated into the organic phase. The increase of Cl- ion concentration in the aqueous phase favors the extraction. The 2-PrOH, salts and acid play important roles in the extraction process. There is no need to use an extracting agent at a high salting-out condition. RECOMMENDATIONS AND PERSPECTIVES: Chromium(VI) must be quickly removed before it enters into the natural cycle. As the 2-PrOH is water-miscible in any proportion, ion-pairing between 2-PrOH2+ and CrO3Cl- becomes very fast. As a result, Cr(VI) can easily be extracted. Therefore, the method is recommended as a simple, rapid and adaptable method to quickly separate Cr(VI) from aqueous samples.     

离子液体吸收废印刷线路板热拆解过程中挥发性有机物——基于COSMO-RS模型

模拟废印刷线路板（WPCB）的热拆解过程,分析热拆解过程中的挥发性有机物（VOCs）组分;利用真实溶剂似导体屏蔽（COSMO-RS）模型对浓度较高的污染物进行量子力学模拟,研究离子液体（ILs）组成单元对目标污染物溶解度的影响差异,分析溶解过程中主导分子间作用力类型,确定优选吸收剂;测定不同溶剂进行溶解性,验证模型适用性.结果表明：①乙酸乙酯和环戊酮是浓度较高的VOCs组分,在240和250℃时浓度分别为43.1,153mg/m³和105,252mg/m³,质量百分比总和分别为76.3%和67.3%.②高表面屏蔽电荷密度分布峰、长烷基链阴阳离子和亲电基团的存在可提高乙酸乙酯和环戊酮在ILs中的溶解度.双三氟甲磺酰基亚胺盐（NTf₂^-）类ILs是一类优良吸收剂.静电力和范德华力对溶解过程起主导作用.③COSMO-RS模型可定性和半定量用于预测乙酸乙酯和环戊酮的溶解度.     

Advanced molecular-fingerprinting analysis of dissolved organic sulfur by electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry using optimal spray solvent

Molecular level characterization of dissolved organic sulfur (DOS) by electrospray ionization-Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR MS) is necessary for further understanding of the role of DOS in the environment. Here, ESI spray solvent, a key parameter for ion production during ESI process, was investigated for its effect on the molecular characterization of DOS by ESI-FTICR MS. 100% MeOH as spray solvent was found for the first time to remarkably enhance the ionization efficiency of the majority of CHOS-molecules in NOM, which facilitated a total of 1473 CHOS-molecular formulas with one sulfur atom to be detected. The number of CHOS-molecular formulas obtained using 100%MeOH as spray solvent increased notably over 740 in comparison with those using 50% MeOH aqueous solution (731) or 50% ACN aqueous solution (653). Moreover, due to the enhancement of ionization efficiency of DOS during ESI processes, the tandem mass spectra of the NOM CHOS-molecules could be easily obtained using 100% MeOH as spray solvent, which were hardly obtained using 50% MeOH aqueous solution as spray solvent. The results of the tandem mass spectra suggested the first discovery of organosulfates or sulfonic acids in Suwannee River NOM sample. A simple method based on 100% MeOH as ESI spray solvent for advanced molecular characterization of DOS by ESI-FTICR MS was proposed and applied, and the results revealed more molecular information of DOS in sea DOM samples.     

国内外饮用水余氯限值及监测方法的研究进展

新型冠状病毒肺炎疫情期间大规模使用含氯消毒剂,其残留可能对水环境及人体健康造成影响.我国饮用水水源地质量标准并未设置余氯项目及其浓度限值,且缺乏统一的余氯现场快速分析方法标准.为公共卫生事件发生期间的水质余氯监测与评价提供参考,对国内外饮用水标准余氯限值、实验室标准分析方法、现场快速分析方法等进行汇总分析,结果表明:①不同国家和地区以及WHO（World Health Organization,世界卫生组织）在饮用水标准中分别设置了出厂水中余氯限值（范围为0.1~2.0 mg/L）、管网末梢水中余氯限值（范围为0.1~1.8 mg/L）及饮用水中余氯最大允许浓度（范围为4~5 mg/L）.②比色法、容量法因其具有反应迅速且稳定、准确度及精密度较高等优点而成为国内外实验室主要标准或推荐分析方法,高效液相色谱法检出限最低,灵敏度最高,可用于余氯痕量分析.③余氯现场快速分析方法多以比色法为主,在线监测方法多为电化学方法,但缺乏统一的标准方法.研究显示,国外饮用水标准中余氯最大允许浓度为5 mg/L,WHO推荐高风险环境下的管网末梢余氯浓度最低为0.5 mg/L,建议尽快开展水质余氯现场监测方法标准化研究.      

雨天硫酸盐化速率样品扩散分析

选择采样期不同降雨天数的碱片，测定余边的硫酸盐化速率含量，其结果为：采样期全月无雨时，余边上的硫酸盐均未检出；半月以上至全月有雨时检出率为１００％，检出量占样品量的２．７０～１５．９５％。经扩散试验，查清了余边上的硫酸盐主要是有效面积上采集的样品的扩散，并提出了相应的修正方法。     

电解-CASS工艺处理制药废水工艺研究与设计

采用电解 CASS工艺处理制药厂废水 ,实现了处理效率高 ,占地面积小 ,工程投资低等优点 ,处理后各项污染指标均达到国家《污水综合排放》(GB8978— 1996)的二级排放标准     

活性污泥法处理矿区生活污水剩余污泥量探讨

由于矿区生活污水中有机污染物浓度较低，采用活性污泥法处理工艺，有机污染物在生物氧化池内得到较彻底地降解，剩余污泥量少，每千吨生活污水产生剩余污泥量为2～3t。     

MBBR处理制药废水的试验研究

采用二级移动床生物膜反应器(MBBR)处理呋喃铵盐制药废水。在填充比为40%,总水力停留时间为32h时,COD的去除率为88.6%,TN的去除率为25.7%,第二级反应器对NH3-N的去除率为56.2%。