水中3种微囊藻毒素的高效液相色谱测定方法优化

对天然水体中3种痕量微囊藻毒素（MC-RR、MC-YR、MC-LR）的淋洗、洗脱、液相色谱测定等环节进行单因素不同水平考察,结果表明：以体积分数为45%的甲醇水溶液（含0.1%的TFA）为固相萃取淋洗剂、10 mL甲醇（含01%TFA）为固相萃取洗脱剂,体积分数为70%的甲醇水溶液（含0.1%TFA）为液相色谱流动相,可在6 min内有效分离MC-RR、MC-YR、MC-LR。将优化后的方法用于实际加标水样的测定,MC-RR、MC-YR、MC-LR的方法检出限分别为0.064 μg/L、0.098 μg/L、0.095 μg/L,加标回收率为87.0%~116%,RSD为10.2%~18.8%。     

基于ZIF-L的微固相萃取技术测定地表水中痕量典型多环芳烃

制备类沸石咪唑酯骨架ZIF-L材料,将其用作微固相萃取吸附剂,处理水中萘、苊、苊烯、芴、菲、蒽、荧蒽、芘等8种痕量典型多环芳烃,再用HPLC测定。试验表明,ZIF-L对上述多环芳烃的萃取效率明显高于商品化萃取材料C 18和多壁碳纳米管。方法在0.100μg/L^200μg/L范围内线性良好,方法检出限为0.02μg/L^0.03μg/L,标准溶液5次测定结果的RSD为4.7%~9.5%,实际水样加标回收率为84.5%~115%。将该方法用于北太湖5个点位水样的测定,测定值为未检出~3.40μg/L。     

响应面法优化养殖水体中炔雌醇的固相萃取条件

在单因素试验、Plackett-Burman设计试验基础上,采用Box-Behnken响应面法对养殖水体中炔雌醇(EE2)的固相萃取条件进行优化。结果表明,洗脱液体积、洗脱液组成和淋洗液体积是影响EE2固相萃取回收率的3个主要因素;EE2的最佳固相萃取条件为:水样pH值为3,进样流量为3.0 mL/min,淋洗液为体积分数为10%的甲醇水溶液,淋洗液体积7.0 mL,洗脱液为乙酸乙酯-正己烷混合溶液(体积比为9∶1),洗脱液体积12.0 mL。该条件下养殖水样中EE2固相萃取回收率为81.6%～86.7%。     

平煤十矿底板巷穿层钻孔瓦斯抽采模拟研究

为了降低平煤十矿己15-16-24130工作面运输巷掘进中的突出危险性,基于实际工程背景,考虑瓦斯抽采中的瓦斯运移及煤岩变形等因素,建立了瓦斯抽采气固耦合模型,并利用COMSOL Multiphysics软件对平煤十矿己15-16煤层的底板巷穿层钻孔瓦斯抽采方案进行数值模拟,研究了瓦斯抽采对于降低掘进过程中突出危险性的影响。研究结果表明:在己18煤层开挖底板巷对己15-16煤层进行穿层钻孔瓦斯抽采,瓦斯抽采180 d后,己15-16-24130工作面运输巷附近煤层残余瓦斯压力及瓦斯含量分别降至0.315 MPa和3.84 m3/t;将底板巷穿层钻孔瓦斯抽采方案进行工程应用,实测抽采后的残余瓦斯压力及瓦斯含量在0.32 MPa和3.17 m3/t,均小于平煤十矿煤与瓦斯突出防治规定的“双6”指标（残余瓦斯压力小于0.6 MPa,残余瓦斯含量小于6 m3/t）,可有效降低运输巷掘进过程中的突出危险性。     

采油废水回注处理技术的现状及展望

阐述了目前采油废水回注处理的技术及工艺现状,重点探讨了膜分离技术在采油废水回注处理中的研究及应用情况,分析了各技术存在的问题,并展望了采油废水回注处理技术的发展趋势。     

Mobility of radium and trace metals in sediments of the Winterbeek: Application of sequential extraction and DGT techniques

For several decades, phosphate ores containing ²²⁶Ra as well as several trace metals have been processed in Belgium to produce calcium phosphate for use in cattle food. The waste water is discharged in two small rivers, the Laak and the Winterbeek.In this study, the levels of ²²⁶Ra and trace metals in surface water and sediments of the Winterbeek were investigated and the mobility of these compounds was assessed using DGT (Diffusive Gradient in Thin Films) and sequential extraction techniques.The concentrations of ²²⁶Ra and trace metals in water and sediment indicate a decreasing trend in inputs to the Winterbeek.The mobility of ²²⁶Ra, assessed by DGT, is related to the reductive mobilization of Fe. The sequential extraction technique shows that at some stations an important fraction of ²²⁶Ra is found to labile sediment phases.Diffusive ²²⁶Ra sediment fluxes, are however, relatively small and have only a minor contribution to the water column concentration of ²²⁶Ra.     

Determination of antibiotics in sewage from hospitals, nursery and slaughter house, wastewater treatment plant and source water in Chongqing region of Three Gorge Reservoir in China

Sewage samples from 4 hospitals, 1 nursery, 1 slaughter house, 1 wastewater treatment plant and 5 source water samples of Chongqing region of Three Gorge Reservoir were analyzed for macrolide, lincosamide, trimethoprim, fluorouinolone, sulfonamide and tetracycline antibiotics by online solid-phase extraction and liquid chromatography-tandem mass spectrometry. Results showed that the concentration of ofloxacin (OFX) in hospital was the highest among all water environments ranged from 1.660 μg/L to 4.240 μg/L and norfloxacin (NOR, 0.136-1.620 μg/L), ciproflaxacin (CIP, ranged from 0.011 μg/L to 0.136 μg/L), trimethoprim (TMP, 0.061-0.174 μg/L) were commonly detected. Removal range of antibiotics in the wastewater treatment plant was 18-100% and the removal ratio of tylosin, oxytetracycline and tetracycline were 100%. Relatively higher removal efficiencies were observed for tylosin (TYL), oxytetracycline (OXY) and tetracycline (TET)(100%), while lower removal efficiencies were observed for Trimethoprim (TMP, 1%), Epi-iso-chlorotetracycline (EICIC, 18%) and Erythromycin-H₂O (ERY-H₂O, 24%). Antibiotics were removed more efficiently in primary treatment compared with those in secondary treatment.     

Electro-remediation of tailings from a multi-metal sulphide mine: comparing removal efficiencies of Pb,Zn, Cu and Cd

Sulphidic mine tailings characterised by high concentrations of heavy metals (Pb 3532?±?97?mg/kg, Zn 8450?±?154?mg/kg, Cu 239?±?18?mg/kg and Cd 14.1?±?0.3?mg/kg) and abundant carbonate (17%) were subjected to eight lab-scale electrodialytic remediation (EDR) experiments to investigate the influence of current density, treatment time and particle size on removal efficiency. Pb and Cu removal improved when increasing current density, while Zn and Cd removal did not. In contrast Zn and Cd removal improved by grinding the tailings, while Pb and Cu removal did not. At the highest current density (1.2?mA/cm²), 94%, 75%, 71% and 67% removal of Pb, Zn, Cu and Cd could be achieved, respectively, on grinded tailings in 28 days. Sequential chemical extraction made before and after EDR revealed larger oxidisable fractions of Zn, Cu and Cd, representing large fractions of sulphides, which was likely to be the main barrier to be removed as efficiently as Pb. This was in accordance with acid/base extraction tests in which Pb showed high solubility at both high and low pH (up to 65% and 86% of extraction, respectively), while considerable extraction of Zn (55%) happened only at low pH; and very limited extraction (<20%) of Cu and Cd occurred at any pH.     

Molecularly imprinted polymer for analysis of trace atrazine herbicide in water

A molecularly imprinted polymer (MIP) for atrazine was synthesized by non-covalent method. The binding capacity of MIP was 1.00 mg g^{? 1} polymer. The selectivity and recovery were investigated with various pesticides which are mostly, found in the environment, for both similar and different chemical structure of atrazine. The competitive recognition between atrazine and structurally similar compounds was evaluated and it was found that the system provided highest recovery and selectivity for atrazine while low recovery and selectivity were obtained for the other compounds. The highest recovery was obtained from MIP compared with non-imprinted polymer (NIP), a commercial C₁₈ and a granular activated carbon (GAC) sorbent. The method provided high recoveries ranged from 94 to 99% at two spiked levels with relative standard deviations less than 2%. The lower detection limit of the method was 80 ng L^{? 1}. This method was successfully applied for analysis of environmental water samples.     

Evaluation of C18 solid‐phase extraction cartridges for the isolation of select pesticides and metabolites

Abstract

Nine different C₁₈ solid‐phase extraction (SPE) cartridges were evaluated for their efficiency at extracting nine pesticides and two s‐triazine metabolites from spiked deionized water samples. The SPE cartridges were found to contain nitrogen (N) and/or phosphorus (P) contaminants and varied in their extraction efficiency for certain pesticides and metabolites. Four of the nine SPE cartridges gave acceptable (70 to 120%) pesticide and metabolite recovery percentages, while five cartridges had marginal (50 to 70%) to poor (< 50%) recoveries. Statistical analyses showed that the poor to marginal recoveries found for three compounds could not be explained by considering several indigenous chemical and physical traits of the cartridge. It is suggested that proper SPE cartridge selection for pesticide recovery should be evaluated using several different cartridges.