固相萃取-UPLC-MS/MS法测定环境水体中多种抗生素

采用固相萃取-超高效液相色谱串联质谱法测定环境水样中25种磺胺类和喹诺酮类抗生素,通过优化试验条件,使方法在2.00μg/L～200μg/L范围内线性良好,方法检出限为1.01ng/L～2.85ng/L,7次测定结果的RSD为2.3%～8.0%。将该方法用于自来水和地表水测定,结果均为未检出,高、低质量浓度水平的加标回收率为61.2%～102%。     

HPLC-三重四级杆质谱法测定医疗废水中抗生素残留

采用固相萃取/高效液相色谱-三重四级杆质谱法同时测定医疗废水中的20种超痕量抗生素残留,通过优化试验条件,使方法在100μg/L～100μg/L范围内线性良好,方法检出限为024ng/L～122ng/L。空白水样和实际水样3个质量浓度水平的加标回收率分别为80.2%～108%和75.8%～114%,6次测定结果的RSD分别为2.4%～8.4%和1.7%～8.1%。将该方法用于测定重庆市2家三甲医院医疗废水中的超痕量抗生素残留,结果有11种抗生素检出,其余均为未检出。     

液液萃取-气相色谱/串联质谱法测定水中五氯酚及其钠盐

采用液液萃取处理水样,用气相色谱-串联质谱法测定样品中五氯酚及其钠盐,通过优化测定条件,使方法在1.00μg/L～500μg/L范围内线性良好.检出限和定量限分别为1.00μg/L和5.00μg/L,空白水样五氯酚钠3个质量浓度水平的加标回收率为89.8％～98.4％,5次平行试验测定结果的RSD为5.5％～10.7％...     

Highly efficient conversion of sugarcane bagasse pretreated with liquid hot water into ethanol at high solid loading

Liquid hot water (LHW), an environmental-friendly physico-chemical treatment, was applied to pretreat the sugarcane bagasse (SCB). Tween80, a non-ionic surfactant, was used to enhance the enzymatic hydrolysis of the pretreated SCB. It found that 0.125 mL Tween80 /g dry matter could make the maximum increase (33.2%) of the glycan conversion of the LHW-pretreated SCB. A self-designed laboratory facility with a plate-and-frame impeller was applied to conduct batch hydrolysis, fed-batch hydrolysis, and the process of high-temperature (50°C) fed-batch hydrolysis following low-temperature (30°C) simultaneous saccharification and fermentation (SSF) which was adopted to overcome the incompatible optimum temperature of saccharification and fermentation in the SSF process. After hydrolyzing LHW-pretreated SCB for 120 h with commercial cellulase, the total sugar concentration and glycan conversion obtained from fed-batch hydrolysis were 91.6 g/L and 68.3%, respectively, which were 9.7 g/L and 7.3% higher than those obtained from batch hydrolysis. With Saccharomyces cerevisiae Y2034 fermenting under the non-sterile condition, the ethanol production and theoretical yield obtained from the process of SSF after fed-batch hydrolysis were 55.4 g/L and 88.3% for 72h, respectively, which were 15.5 g/L and 24.7% higher than those from separate fed-batch hydrolysis and fermentation. The result of this work was superior to the reported results obtained from the LHW-pretreated SCB.     

Mathematical Modeling of Column and Field Dense Nonaqueous Phase Liquid Tracer Tests

Mathematical models for the simulation of dense nonaqueous phase liquid tracer tests (DTTs) in laboratory columns and in the field are developed and examined. The DTT technique is a means of estimating the quantity of dense nonaqueous phase liquid (DNAPL) in a domain of interest in an aquifer. The two-dimensional field DTT model uses the Method of Principal Directions and an asymmetrical upwind algorithm for describing advective transport. Both models include diffusion transport of tracer into and from low-permeability porous structures such as clay lenses, as well as the mass transport kinetics of partitioning tracer to and from the DNAPL droplets. The dependence of the effluent tracer concentration curves on the parameters of the models is explored, and conclusions are drawn regarding the applicability of, and several possible problems with, the DTT technique. Model results indicate that the DTT performs well at locating distributed droplets of DNAPL, but is unlikely to be useful in the assessment of pooled DNAPL.     

宁波市饮用水源地爆发蓝藻水华时微囊藻毒素的污染分析

通过固相萃取净化,建立了超高效液相色谱-串联四极杆质谱法测定水中微囊藻毒素MC-LR和MC-RR的方法,并用该方法监测了宁波市两个饮用水源地爆发蓝藻水华时水体中的微囊藻毒素.监测结果表明,姚江水体中的微囊藻毒素污染水平低,MC-LR和MC-RR没有被检出;梅湖水库水体中MC-RR也未被检出,采取措施后,虽MC-LR有时被检出,但最高时也低于国家标准值(1.0μg/L).     

大气固定污染源低浓度颗粒物采样及分析技术研究进展

简述了我国现阶段大气固定污染源颗粒物监测中遇到的问题及低浓度颗粒物采样与分析技术研究的必要性,归纳了国外低浓度颗粒物采样分析技术要点,包括大体积采样、滤筒上游采样设备堆积颗粒物的回收、有效称重步骤的确立等,并对我国开展低浓度颗粒物采样及分析技术研究提出了相关建议.     

生化需氧量测定的方法改进

生化需氧量测定中接种液的制备和稀释倍数的确定是2个关键的步骤,本文提出一种可行的制备接种液的方法,根据实践经验,总结出一种稀释倍数计算方法,适合在实际分析中使用。     

Effect of soil moisture dynamics on dense nonaqueous phase liquid (DNAPL) spill zone architecture in heterogeneous porous media

The amount, location, and form of NAPL in contaminated vadose zones are controlled by the spatial distribution of water saturation and soil permeability, the NAPL spill scenario, water infiltration events, and vapor transport. To evaluate the effects of these processes, we used the three-phase flow simulator STOMP, which includes a new permeability-liquid saturation-capillary pressure (k-S-P) constitutive model. This new constitutive model considers three NAPL forms: free, residual, and trapped. A 2-D vertical cross-section with five stratigraphic layers was assumed, and simulations were performed for seven cases. The conceptual model of the soil heterogeneity was based upon the stratigraphy at the Hanford carbon tetrachloride (CT) spill site. Some cases considered co-disposal of NAPL with large volumes of wastewater, as also occurred at the Hanford CT site. In these cases, the form and location of NAPL were most strongly influenced by high water discharge rates and NAPL evaporation to the atmosphere. In order to investigate the impact of heterogeneity, the hydraulic conductivity within the lower permeability layer was modeled as a realization of a random field having three different classes. For six extreme cases of 100 realizations, the CT mass that reached the water table varied by a factor of two, and was primarily controlled by the degree of lateral connectivity of the low conductivity class within the lowest permeability layer. The grid size at the top boundary had a dramatic impact on NAPL diffusive flux just after the spill event when the NAPL was present near the ground surface. NAPL evaporation with a fine grid spacing at the top boundary decreased CT mass that reached the water table by 74%, compared to the case with a coarse grid spacing, while barometric pumping had a marginal effect for the case of a continuous NAPL spill scenario considered in this work. For low water infiltration rate scenarios, the distribution of water content prior to a NAPL spill event decreased CT mass that reached the water table by 98% and had a significant impact on the formation of trapped NAPL. For all cases simulated, use of the new constitutive model that allows the formation of residual NAPL increased the amount of NAPL retained in the vadose zone. Density-driven advective gas flow from the ground surface controlled vapor migration in strongly anisotropic layers, causing NAPL mass flux to the lower layer to be reduced. These simulations indicate that consideration of the formation of residual and trapped NAPLs and dynamic boundary conditions (e.g., areas, rates, and periods of different NAPL and water discharge and fluctuations of atmospheric pressure) in the context of full three-phase flow are needed, especially for NAPL spill events at the ground surface. In addition, NAPL evaporation, density-driven gas advection, and NAPL vertical movement enhanced by water flow must be considered in order to predict NAPL distribution and migration in the vadose zone.     

碳包覆Pd/Al2O3催化剂催化4-溴苯酚加氢脱溴的活性和稳定性调控研究

在污染物液相催化加氢脱卤过程中,提高催化剂的稳定性至关重要.以水热合成法制备了不同碳包覆量的Pd/Al₂O₃@C催化剂,对催化剂进行了系列表征,并将催化剂应用于4-溴苯酚(4-BP)污染物的催化加氢脱溴反应.表征结果显示碳层提高了Pd/Al₂O₃的表面疏水性,有利于4-BP在催化剂上的吸附.并且在Pd/Al₂O₃@C催化剂的碳化过程中,碳还原部分Pd颗粒,并保留部分正价态Pd活性位,增强了4-BP中C-Br键的活化.与Pd/Al₂O₃相比,碳涂层提高了催化剂的催化活性.但当碳包覆量超过最佳包覆量后,暴露的Pd粒子随碳包覆量的增加而减少,导致活性下降.此外,碳层修饰后,催化剂的稳定性显著提高,从而大大抑制了Pd粒子的团聚和损耗.Pd/Al₂O₃@C表面的碳涂层对卤素具有较高的耐受性,从而减轻了液相催化加氢脱卤反应中活性中心的中毒.