Photodegradation of acetochlor in water and UV photoproducts identified by mass spectrometry

The sunlight photodegradation half-lives of 20 mg/L acetochlor were 151, 154 and 169 days in de-ionized water, river water and paddy water, respectively. When exposed to ultraviolet (UV) light, acetochlor in aqueous solution was rapidly degraded. The half-lives were7.1, 10.1, and 11.5 min in de-ionized water, river water and paddy water, respectively. Photopreduets of acetochlor were identified by gas chromatography/mass spectrometry(GC/MS) and found at least twelve photoproducts resulted from dechlorination with subsequent hydrtrxylation and cyclization processes. The chemical structures of ten photoproducts were presumed on the basis of mass spectrum interpretation and literature data. Photoproducts are identified as 2-ethyl-6-methylaniline; N, N-diethylaniline ; 4, 8-dimethyl-2-oxo- 1,2,3,4- tetrahydroquino-line; 2-oxo-N-(2-ethyl-6-methylphenyl)-N-(ethoxymethyl) acetamide; N-(ethoxymethyl)-2‘-ethyl-6‘-methylformanilide; 1-hydroxyaeetyl-2-ethoxyl-7-ethylind ole; 8-ethyl-l-ethoxymethyl-2-oxo-1, 2, 3, 4-tetrahydroquinoline; 4, 8-dimethyl-l-ethoxymethyl-2-oxo-1, 2, 3, 4-tetrahydroquinoline; 2-hydroxy-2‘-ethyl-6‘-methyl-N-(ethoxymethyl) acetanilide and a compound related to acetochlor. The other two photoproducts were detected by GC/MS although their chemical structure was unknown.     

吹扫捕集与色谱质谱联用测定水中挥发性有机物

采用吹扫描集与色谱质谱联用的对水中１９种挥发性有机物同时进行富集分离，定性和定量检测，结果表明，不同化合物的平均回收率大于９０％相对偏差小于５％，该方法的检测限约为０．１－０．４μ／Ｌ。实验证明吹扫描集与色谱质谱联用技术是快速测定水中挥发性有要峨的有效手段。     

上海市大气PM2.5中溶剂可抽提有机物的特征研究

利用溶剂抽提、分离、毛细管气相色谱-质谱联用技术对2000年10月至2001年8月上海市5个不同功能区采集的大气PM_(2.5)样品中的溶剂可抽提有机物进行了检测,共检测出正构烷烃、单环芳烃、多环芳烃、有机酸、有机醇、有机酯等各类溶剂可抽提有机化合物267种。检出的82种多环芳烃中有15种属于美国EPA优先控制污染物名单。比较了不同季节、不同区域PM_(2.5)样品中正构烷烃、多环芳烃等化合物分布特征的差异。检出的喹啉类含氮杂环类化合物以及有机酸等污染物表现出一定的机动车排放特征。     

环境中二噁(口英)及其检测技术进展

从二(?)(?)类化合物的结构、来源、毒性等简要说明对其监测的必要性,且从仪器监测(包括气相色谱、气质联用、串联质谱等)和生物监测(包括利用指示生物、生物标志物等)概述了80年代以来国内外对二(?)(?)类物质尤其是几种极毒性化合物如多氯代二苯二(?)(?)(PCDDs)和多氯代二苯呋喃(PCDFs)等化合物的检测技术成果。     

毛细管色谱-多离子检测质谱法测定土壤中2,3,7,8-四氯二苯并二噁(2,3,7,8-TCDD)

环境中的多氯二苯并二(口恶)(口英)(PCDD_s)和多氯二苯并呋喃(PCDF_s)是当今最受重视的污染物之一,其中PCDD_s有75个异构体而PCDF_s有135个异构体,它们的毒性大小显著地依赖于氯原子的取代数和取代位置,由于这类污染物的低溶解度和高的辛醇/水分配系数,主要分布在土壤(85％)和沉积物(14％)中,只有1％进入空气、水和生物体.在自然环境中这类污染物代谢降解速度缓慢,从而增加了环境污染的复杂性.而鉴别这类污染物就成为一个主要研究课题.     

PVC包装材料中酞酸酯增塑剂残留的ASE-GC-MS分析

针对PVC包装材料中酞酸酯（PAEs）增塑剂残留，采用加速溶剂萃取（ASE）和GC／MS联用技术分析5种PAEs（DMP，DEP，DBP，BBP，DEHP），结果表明加速溶剂萃取用于PVC包装材料中PAEs的提取，最佳温度条件为120℃，最佳循环次数为3次。方法检出限达到0．1mg／kg，回收率达到95．5％-99．8％；并且具有很好的重现性和精密度。     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

Pyrolysis of waste animal fats in a fixed-bed reactor: Production and characterization of bio-oil and bio-char

Several animal (lamb, poultry and swine) fatty wastes were pyrolyzed under nitrogen, in a laboratory scale fixed-bed reactor and the main products (liquid bio-oil, solid bio-char and syngas) were obtained. The purpose of this study is to produce and characterize bio-oil and bio-char obtained from pyrolysis of animal fatty wastes. The maximum production of bio-oil was achieved at a pyrolysis temperature of 500 °C and a heating rate of 5 °C/min. The chemical (GC–MS analyses) and spectroscopic analyses (FTIR analyses) of bio-oil showed that it is a complex mixture consisting of different classes of organic compounds, i.e., hydrocarbons (alkanes, alkenes, cyclic compounds…etc.), carboxylic acids, aldehydes, ketones, esters,…etc. According to fuel properties, produced bio-oils showed good properties, suitable for its use as an engine fuel or as a potential source for synthetic fuels and chemical feedstock. Obtained bio-chars had low carbon content and high ash content which make them unattractive for as renewable source energy.     

沉积物中雌激素及壬基酚、辛基酚、双酚A的测定

近些年来雌激素及烷基酚类化合物由于其对水生生物的内分泌干扰作用越来越受到广泛关注.沉积物作为环境中有机污染物的重要储存库,研究目标物在其中的浓度分布对于探明此类物质在环境中的迁移转化具有重要意义.但沉积物中基质组成复杂而雌激素又痕量存在,这增加了前处理的难度.本研究从雌激素及烷基酚类化合物的理化性质入手,采用碱液提取、液液萃取和LC-MS/MS分析测定沉积物样品中的雌激素及壬基酚、辛基酚、双酚A.结果表明,经过优化的方法对7种目标物的回收率介于61.9%～93.7%之间.该方法能有效去除沉积物中那些不溶于强碱和既溶于酸又溶于碱的有机污染物,同时操作简单、成本低,但回收率高、检出限低,可广泛适用于河流沉积物样品及土壤样品的前处理.     

Electrochemical treatment of olive mill wastewater: Treatment extent and effluent phenolic compounds monitoring using some uncommon analytical tools

Problems related with industrials effluents can be divided in two parts: (1) their toxicity associated to their chemical content which should be removed before discharging the wastewater into the receptor media; (2) and the second part is linked to the difficulties of pollution characterisation and monitoring caused by the complexity of these matrixes. This investigation deals with these two aspects, an electrochemical treatment method of an olive mill wastewater (OMW) under platinized expanded titanium electrodes using a modified Grignard reactor for toxicity removal as well as the exploration of the use of some specific analytical tools to monitor effluent phenolic compounds elimination. The results showed that electrochemical oxidation is able to remove/mitigate the OMW pollution. Indeed, 87% of OMW color was removed and all aromatic compounds were disappeared from the solution by anodic oxidation. Moreover, 55% of the chemical oxygen demand (COD) and the total organic carbon (TOC) were reduced. On the other hand, UV- Visible spectrophotometry, Gaz chromatography/mass spectrometry, cyclic voltammetry and 13 C Nuclear Magnetic Resonance (NMR) showed that the used treatment seems efficaciously to eliminate phenolic compounds from OMW. It was concluded that electrochemical oxidation in a modified Grignard reactor is a promising process for the destruction of all phenolic compounds present in OMW. Among the monitoring analytical tools applied, cyclic voltammetry and 13 C NMR are among the techniques that are introduced for the first time to control the advancement of the OMW treatment and gave a close insight on polyphenols disappearance.