环境空气中丙烯酸乙酯的气相色谱法测定

建立了环境空气中丙烯酸乙酯的TenaxGC吸附 -热解吸气相色谱测定方法。方法回收率为 87 3%～1 0 7 1 % ,变异系数为 5 3%～ 7 2 %。当采样体积为 2L时 ,检测限为 0 0 2mg/m3,具有采样时间短 ,不用任何溶剂等特点。     

厌氧水环境中噬菌体MS2的存活和团聚特性及理化因素的影响

为探究病毒在厌氧水环境中的存活特性,以噬菌体MS2为模式病毒,采用双层平板法进行噬菌体MS2的定量检测,研究温度、pH值、悬浮颗粒物、乙酸等理化条件对噬菌体MS2的影响,分析其衰减动力学特征,并通过测定Zeta电位和噬菌斑直径考察噬菌体颗粒在不同条件下的聚集状况.结果表明,在厌氧水环境中,噬菌体MS2的衰减符合一阶指数衰减模型.在众多研究因素中,温度是影响噬菌体MS2存活的最主要因素.噬菌体MS2在4,17,25和35℃时的T₉₀分别为20.36,6.14,5.15和0.46d.35℃条件下12h后噬菌体失活率高达2.44lg,而4℃条件下7d后噬菌体失活率仅有0.78lg.增加乙酸浓度能明显提高噬菌体MS2的衰减速率.低pH值和悬浮颗粒物条件会促进噬菌体的团聚,使噬菌体颗粒Zeta电位降低,水力学直径增大,但悬浮颗粒物浓度过高会影响颗粒间的静电作用.噬菌体的团聚也增加了噬菌斑的直径,pH=6和20mg/L的悬浮颗粒物条件下,直径1.0mm以上的大噬菌斑数量占比分别达到了45.61%和57.74%.明确厌氧水环境中各种理化因素对噬菌体MS2的影响,可为水环境病毒控制提供科学依据.     

Identification and characterization of Fe3O4/peroxodisulfate advanced oxidation products from sulfameter

Sulfonamides (SAs) are one of the most widely used antibiotics and their residuals in the environment could cause some negative environmental issues. Advanced oxidation such as Fenton-like reaction has been widely applied in the treatment of SAs polluted water. Degradation rates of 95%-99.7% were achieved in this work for the tested 8 SAs, including sulfisomidine, sulfameter (SME), phthalylsulfathiazole, sulfamethoxypyridazine, sulfamonomethoxine, sulfisoxazole, sulfachloropyridazine, and sulfadimethoxine, in the Fe₃O₄/peroxodisulfate (PDS) oxidation system after the optimization of PDS concentration and pH. Meanwhile, it was found that a lot of unknown oxidation products were formed, which brought up the uncertainty of health risks to the environment, and the identification of these unknown products was critical. Therefore, SME was selected as the model compound, from which the oxidation products were never elucidated, to identify these intermediates/products. With liquid chromatography-high resolution tandem mass spectrometry (LC-HRMS/MS), 10 new products were identified, in which 2-amino-5-methoxypyrimidine (AMP) was confirmed by its standard. The investigation of the oxidation process of SME indicated that most of the products were not stable and the degradation pathways were very complicated as multiple reactions, such as oxidation of the amino group, SO₂ extrusion, and potential cross-reaction occurred simultaneously. Though most of the products were not verified due to the lack of standards, our results could be helpful in the evaluation of the treatment performance of SAs containing wastewater.     

固相萃取-超高效液相色谱-串联质谱测定水中痕量苯甲地那铵

苯甲地那铵是一种广泛使用的苦味剂,近年来被发现在欧洲水体中普遍存在。建立灵敏可靠的环境样品前处理分析方法对评价其环境行为具有重要意义。通过优化关键前处理过程参数,建立了水中苯甲地那铵的固相萃取-超高效液相色谱串联质谱分析方法,系统考察了该方法的准确度、精密度、基质效应、检出限以及线性范围。研究表明:当调节水样pH至8以上,采用混合型阳离子交换小柱(200 mg,3 mL)富集水样,采用含体积分数2%甲酸的甲醇溶液洗脱时,该方法可获得最佳回收率;纯水和环境水样中加标回收率分别为97%~105%和89%~119%,相对标准偏差小于7%;基质效应均在24%以内;方法检出限为0.07 ng/L,线性范围为0.01~50 μg/L。该方法可用于环境水体中苯甲地那铵的痕量检测。     

高效液相色谱串联质谱法直接测定环境水样中8种有机磷农药

建立了一种高效液相色谱-串联质谱法（LC-MS/MS）同时测定环境水样中8种有机磷农药的分析方法。以地表水、地下水、污水和废水样品作为代表性水样基底,前处理方法仅采用简单的滤膜过滤,在C₁₈柱分离后,在多反应监测模式下进行分析检测。结果表明,敌百虫、毒死蜱等有机磷农药在样品保存过程中迅速发生降解,分析须在样本采集后1 d内完成;该方法的检出限为0.10~0.20 μg/L,线性拟合相关系数（r）均>0.995;不同基底、不同浓度的加标回收实验表明,8种有机磷农药在环境基底中的回收率为74.5%~118%,相对标准偏差为0.4%~8.6%。该方法操作简便、灵敏度高、准确性好,在未来环境监测工作中具有较好的应用前景。     

Identification of Odor Causing Compounds in a Commercial Dairy Farm

The odorous air emissions from confined animal feeding operations (CAFOs), such as swine, poultry and dairy farms, are increasingly raising community complaints. Odorous emissions can result in health damages, psychological discomforts and adverse aesthetic effects in the community. However, these emissions are not well characterized up to now due to the lack of legislation, the limitations in sampling and instrumentation techniques, and the complexity of the emissions themselves. This study is aimed at the development of a high volume sampler and sorbent assembly to identify the odor causing compounds from a diary CAFO. The sorbent was custom designed to target the potential compounds that may exist in a dairy farm and was validated in laboratory with a synthetic odor from the swine manure. The actual samples at the diary farm were collected in spring and summer of 2005. The sorbents were solvent extracted and individual odor compounds were identified using GC–MS (gas chromatography–mass spectroscopy). The data obtained indicated that high volume sampling can shorten the sampling time from days to within 4 h. Both volatile organic compounds (VOCs) and volatile fatty acids (VFAs) have been identified from the dairy farm, such as phenol, methylphenol, 4-ethyl phenol, indole, methyl indole, benzyl alcohol, hexanoic acid, valeric acid and iso-valeric acid, together with some nitrogen containing compounds that have not been reported before.     

有机硫恶臭物质采样和分析检测技术研究

本研究以二甲二硫醚和甲硫醇为代表对有机硫恶臭物质的采样浓缩,热解析和ＧＣ,ＧＣ／ＭＳ的色谱分离,定性鉴定和定量检测方法进行了实验技术研究。与此同时研制开发了恶臭污染监测的系列配套装置－采样管,微型采样泵,热解析色谱进行装置和标准气体物质发生装置。经筛选确认,国产ＧＤＸＥ１０５采样管可对ＤＭＤＳ和ＣＨ３ＳＨ实现直接常温采样浓缩,样品回收率分别为１００％和６０％。ＧＣ／ＦＰＤ对二种硫化物的检出下限分别     

投菌生物接触氧化法处理洁霉素废水的机理研究

研究了“水解酸化－二段生物接触氧化－混凝”工艺处理高浓度洁霉素废水处理系统中好氧微生物膜特性,分布规律、降解作用,高效降解菌的选育,投加菌在反应器中能否保持优势等问题,以探讨用投菌生物接触氧化法处理洁霉素废水的机理,对本系统好氧微生物膜进行后仍存于反应器中并占有优势,最优势菌株经鉴定属气单胞菌属、通过对中试好氧处理出水进行定性定量分析,寻找其引起剩余ＣＯＤｃｒ值的原因。     

Molecular characterization of effluent organic matter in secondary effluent and reclaimed water: Comparison to natural organic matter in source water

Municipal wastewater reclamation is becoming of increasing importance in the world to solve the problem of water scarcity. A better understanding of the molecular composition of effluent organic matter(Ef OM) in the treated effluents of municipal wastewater treatment plants(WWTPs) is crucial for ensuring the safety of water reuse. In this study, the molecular composition of Ef OM in the secondary effluent of a WWTP in Beijing and the reclaimed water further treated with a coagulation–sedimentation–ozonation process were characterized using a non-target Fourier transform ion cyclotron resonance mass spectrometry(FT-ICR MS) method and compared to that of natural organic matter(NOM) in the local source water from a reservoir. It was found that the molecular composition of Ef OM in the secondary effluent and reclaimed water was dominated by CHOS formulas, while NOM in the source water was dominated by CHO formulas. The CHO formulas of the three samples had similar origins. Anthropogenic surfactants were responsible for the CHOS formulas in Ef OM of the secondary effluent and were not well removed by the coagulation-sedimentation-ozonation treatment process adopted.     

液相色谱-串联质谱法检测甲醛暴露产生的两种DNA加合物

针对两种甲醛-DNA加合物,N~6-羟甲基腺嘌呤(N~6-HOMe-d A)和N2-羟甲基鸟嘌呤(N_2-HOMe-d G),本实验室建立了基于液相色谱串联质谱的分析方法,以便从DNA分子水平上探讨甲醛暴露对DNA的损伤作用机理,其中[~(15)N_5]N~6-Me-d A和[~(13)C_(10)~(15)N_5]N_2-Me-d G为内标;液相分离所用色谱柱为Thermo Polar Advantage II C_(18);方法的精密度较好(RSD5%)、灵敏度较高(检出限分别为0.014和0.0064 ng·m L~(-1))、回收率良好(94.9%~111%).后用小牛胸腺DNA进行体外染毒实验,设置甲醛染毒的浓度梯度(0.001,0.01,0.05,0.1,0.5和1 mmol·L~(-1))和染毒时间组(0、2、4、8、12、16、24 h),利用建立的LC-MS/MS方法检测了DNA中N~6-HOMe-d A和N_2-HOMe-d G的含量.结果表明,两种甲醛-DNA加合物N~6-HOMe-d A和N2-HOMe-d G的量与甲醛暴露存在剂量-反应和时间-反应关系.