气相色谱/质谱测定苯酚丙酮生产废水中半挥发性有机物

建立了用二氯甲烷液液萃取对苯酚丙酮生产废水进行预处理,气相色谱/质谱法同时测定废水中半挥发性有毒有机物异丁酸、异丙苯、α-甲基苯乙烯、2-苯基丙醛、苯乙酮、2-苯基-2-丙醇、α-甲基苯甲醇、苯酚和苯甲酸等的定性定量分析方法。色谱条件为:DB-17MS型色谱柱,程序升温,进样量为1μL,质量选择检测器(MSD)。实验结果表明,该色谱条件对苯酚丙酮生产废水中各半挥发性组分具有较好的分离效果。而对9种组分的最低检出限均低于0.04mg/L,精密度实验相对标准偏差2.14%～5.15%,实际水样的加标回收率稳定。苯酚丙酮生产废水中的主要污染物为2-苯基-2-丙醇,其次为苯酚、异丁酸和异丙苯。     

固相萃取—气相色谱—质谱测定再生水中邻苯二甲酸酯类物质

探讨了一种再生水中邻苯二甲酸酯类物质的测定方法——固相萃取—气相色谱—质谱,检测了相关再生水标准中涉及的邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)两类物质。在质量浓度为20～1 000μg/L时,两类物质的回归方程的相关系数均大于0.999,检出限分别是0.060、0.002μg/L,DBP、DEHP的相对标准偏差分别为4.1%～7.4%、5.1%～6.1%。利用固相萃取技术进行预处理,平均加标回收率为96.6%、89.6%。检测了北京市4座再生水厂出水中DBP和DEHP含量,其中,DBP在1.74～5.59μg/L,低于《城市污水再生利用景观环境用水水质》(GB/T 18921—2002)规定的限值(不超过0.1mg/L),但高于《城市污水再生利用地下水回灌水质》(GB/T 19772—2005)规定的限值(不超过3μg/L);DEHP在0.42～4.93μg/L,满足GB/T 19772—2005要求(不超过8μg/L)。     

单液滴微萃取—气相色谱/质谱法检测水中多环芳烃

采用单液滴微萃取-气相色谱/质谱(GC/MS)法建立了检测水中多环芳烃(PAHs)的方法,研究了萃取溶剂种类、萃取时间、搅拌速度对萃取效率的影响,确定了最佳单液滴微萃取条件,该法用于水中PAHs的检测,16种PAHs的线性范围为0.2～7.0μg/mL,相关系数≥0.9784,检出限为0.002～0.190μg/mL,相对标准偏差为7.1%～15.1%,加标回收率在81%～122%.     

二次热解吸-气相色谱-质谱分析室内挥发性有机化合物

采用二次热解吸-气相色谱.质谱法对室内空气进行了定量和定性分析,共检出挥发性有机物245种,包括烷烃、烯烃、芳香类化合物、卤代烃、醇、醛、酮、酯、醚等化合物,住宅类室内空气中挥发性有机化合物浓度平均值明显高于办公类室内这些物质的浓度平均值,对室内空气样品分析中的特例进行了可能的污染源解析,推测室内过量使用液体胶粘剂有可能是引起污染物严重超标的原因之一.     

丙烯酸装置废水特征有机污染物及其荧光特性

采用吹扫捕集-气相色谱/质谱法(P&T-GC/MS),液液萃取-气相色谱/质谱法(LLE-GC/MS)等方法对丙烯酸装置废水中主要特征有机污染物进行了定性、定量分析,研究了废水和各主要特征污染物的三维荧光特性。结果表明,废水中共检出有机酸、苯系物、酯、醛、醇等24种有机污染物,其中含量较大的有乙酸55.13%,丙烯酸23%,甲醛21.81%,甲苯0.03%,4-羟基-2-丁酮0.02%,丙烯酸甲酯0.01%,正丁醇0.01%。丙烯酸废水中含有3个荧光峰,区域IV内的荧光峰(λex/em=290/355 nm)主要由废水中高浓度的丙烯酸产生,区域V内的2个荧光峰(λex/em=390/495 nm,λex/em=295/480 nm)由水中的腐殖质产生。丙烯酸抑制了甲苯、甲醛、乙酸等3种荧光物质对丙烯酸废水荧光强度的贡献。4种荧光物质的荧光基团影响力大小:碳碳双键+羧基> 苯环> 羰基> 羧基。     

固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃

采用固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃(PAHs)。通过正交试验,得到最佳固相萃取条件为:上样流速为5mL/min、采用二氯甲烷洗脱、洗脱剂用量为3mL、洗脱流速为2mL/min。测定结果显示,固相萃取与气相色谱—质谱联用技术对萘、菲、荧蒽3种PAHs的检出限为0.03～0.07μg/L,加标回收率为70%～100%,相对标准偏差为3.90%～9.58%。该方法精密度高、准确度好,能满足实际水样中痕量PAHs的测定要求。     

液相色谱/质谱联用检测刚果红及其微电解降解的研究

采用液相色谱/质谱联用(LC/MS)检测了模拟印染废水中的刚果红,并用微电解对其进行了降解研究.LC/MS检测刚果红的结果表明,在流动相为甲醇:水(体积比)=70:30、流速为0.6 mL/min、色谱柱为Zorbax XDB0-C18(150 mm× 4.6 mm,5μm)条件下,刚果红的准分子离子的质荷比(m/z)...     

氧弹燃烧-离子色谱法和气相色谱-质谱联用法测定废旧冰箱保温材料中CFC-11的含量

介绍了一种测定废旧冰箱保温材料（聚氨酯硬泡）中CFC-11含量的方法。聚氨酯硬泡中的CFC-11测定包含两部分：一是通过氧弹燃烧-离子色谱法测定材料燃烧后的氯离子含量,另一部分是用气相色谱一质谱联用法测定材料燃烧后CFC-11的含量。     

预处理-水解酸化-厌氧-好氧工艺对玉米淀粉废水有机污染物的降解

采用气相色谱/质谱(GC/MS)、三维荧光光谱(EEM)等检测手段分析预处理/水解酸化/厌氧/好氧组合工艺对玉米淀粉废水有机污染物的降解情况。结果表明,竖流沉淀预处理阶段对TOC平均去除率36.7%,废水中主要为芳烃、烷烯烃以及杂环类物质,EEM产生的5个荧光峰均为芳香蛋白类有机物;水解酸化阶段大部分杂环以及芳烃类有机物水解成有机酸和醇类物质,TOC平均去除率22.7%;厌氧阶段TOC平均去除率最高,达到97.8%,废水中以芳烃和烷烯烃为主,荧光峰减少至2个且强度减弱;好氧阶段TOC平均去除率为61.3%,有机物主要为难降解的长链烷烃物质,芳香蛋白类有机物荧光峰全部消失,新生成了与微生物代谢相关的腐殖酸类物质。     

饮用水中典型致嗅物质吹扫捕集-气相色谱质谱检测方法及优化

采用吹扫捕集/气相色谱-质谱（GC-MS）法对饮用水中致嗅物质2-甲基异茨醇（2-MIB）和土臭素（GSM）进行测定。通过调整吹扫温度、吹扫时间、吹扫时捕集阱的温度、六通阀温度和传输管线温度,分析吹扫捕集条件对吹扫捕集效率的影响,并确定最佳吹扫捕集条件。2-MIB和GSM的方法检出限（MDL）分别为0.729 ng·L-1和1.037 ng·L-1,方法定量限（MQL）分别为2.187 ng·L-1和3.112 ng·L-1,平均加标回收率分别在92%~108%和88%~104%范围内,相对标准偏差分别小于6.5%和9.0%.在20~300 ng·L-1的范围内,各异嗅化合物浓度与响应值的线性关系均良好,相关系数均大于0.999。该方法具有操作简便、检出限低,相关性良好、灵敏度高、重复性好等优点。     

On-Site Gas Chromatography/Mass Spectrometry (GC/MS) Analysis to Streamline Vapor Intrusion Investigations

Distinguishing between vapor intrusion and indoor sources of volatile organic compounds (VOCs) is a significant challenge in conventional vapor intrusion assessments. For this research project, the authors developed a step-by-step protocol to streamline building-specific investigations by using on-site gas chromatography/mass spectrometry (GC/MS) analysis and building pressure manipulation to determine the source of VOCs in indoor air during a 1-day field investigation. Protocol validation included implementation in industrial buildings and testing alongside conventional methods. The new protocol compares favorably to conventional approaches, yielding more definitive results in less time. This article presents three case studies which illustrate application of the protocol.     

Analysis of chlorothalonil and degradation products in soil and water by GC/MS and LC/MS

We present a method using gas chromatography (GC) and liquid chromatography (LC) coupled to a mass selective detector to measure concentrations of the fungicide chlorothalonil and several of its metabolites in soil and water. The methods employed solid-phase extraction using a hydrophobic polymeric phase for the isolation of analytes. In lake water, average analyte recoveries ranged from 70% to 110%, with exception of pentachloronitrobenzene that gave low recoveries (23%). The method detection limits were determined to be in the range of 1 and 0.1microg l(-1) for the LC and GC methods, respectively. In soil samples, recoveries ranged from 80% to 95% for 4-hydroxy-2,5,6-trichloroisophthalonitrile (metabolite II) and 1,3-dicarbamoyl-2,4,5,6-tetrachlorobenzene (metabolite III). Limits of detection (LOD) were 0.05 and 0.02microg g(-1), respectively. Chlorothalonil and other metabolites were analyzed by GC giving recoveries ranging from 54% to 130% with LOD of 0.001-0.005microg g(-1).     

饮用水源水、出厂水有机污染物GC/MS分析

于1998年对成都市饮用水源水、出厂水的有机污染物进行了GC／MS分析,该市饮用水和出厂水均存在有机物污染,且含有优先控制污染物;污染来源主要为生活污水。枯水期有机物检出率高于丰水期。     

Characterisation of odorants emissions from landfills by SPME and GC/MS

Odorous compounds from a landfill have been characterised by gas-chromatography-mass-spectrometry, identifying about 100 volatile organic compounds. Air samples from different landfill sites and from the environment have been analysed after a solid-phase microextraction on a three-phase fiber, DVB/Carboxen/PDMS, which allowed a preconcentration and the chromatographic data obtained from the most significant emission sources have been submitted to chemometric analysis in order to better establish specific markers of olfactory pollution. For example limonene was a typical tracer of fresh wastes, while p-cymene was characteristic of leachate and biogas. By the developed analytical procedure it has been evaluated the efficiency of a scrubber plant utilised in the landfill in order to remove malodour compounds. The average removal efficiency was not very high (about 23.5%) due to scarce ability in removing low polarity compounds. Furthermore, it has been demonstrated the suitability of a microgas chromatograph for the continuous on-site monitoring of air pollution in order to rapidly individuate emission sources of olfactive nuisances.     

Analysis of polycyclic aromatic hydrocarbons (PAHs) in airborne particles by direct sample introduction thermal desorption GC/MS

The technique of thermal desorption (TD)–GC/MS was evaluated for measuring airborne, 4–6 ring polycyclic aromatic hydrocarbons (PAHs) collected onto quartz filters. TD provides a more readily automated and sensitive alternative to traditional solvent extraction, decreasing the time/cost of analysis and reducing the risk of analyte loss or sample contamination. The developed method was successfully applied to the analysis of PAH standard solutions loaded on sorbent tubes packed with quartz wool and the graphitized carbon black sorbent Carbograph2. The optimized method showed high desorption efficiency over the whole range of target PAHs with good precision, linearity and sensitivity. The proposed method was verified on an urban dust Standard Reference Material (SRM 1649a); the experimentally determined concentrations agreed with the certified ranges (95% confidence limit) for all target compounds except benzo[a]anthracene, which fell just outside the narrow certified range. The desorption efficiency and the reproducibility of the method was evaluated by analysing pieces of real sample filters sampled from urban air for a period of 24 h. The results confirmed the homogeneity of the filter and showed high recovery efficiencies for all target PAHs.     

基于三维荧光及平行因子分析的南昌市某河可溶性有机物溯源及治理策略

地表河流污染物溯源对污染物防治及河流生态环境改善具有重要意义。三维荧光光谱(3D-EEM)的图谱形状、荧光峰位置、荧光峰强度、荧光峰个数信息和荧光参数可作为水体中可溶性有机物(DOM)的荧光特征。结合平行因子分析(PARAFAC)对南昌市某河的3D-EEMs进行分析并进行DOM溯源研究,结果表明,该河DOM主要包含3个荧光组分,分别为类腐殖质荧光组分C1(λ_Ex/λ_Em=245 nm/430 nm)、类氨基酸和类腐殖质组分的混合物C2(λ_Ex/λ_Em=240,300 nm/365 nm)和类色氨酸荧光组分C3(λ_Ex/λ_Em=225,275 nm/335 nm),分别占总荧光组分的35.93%,26.62%和37.45%。该河基本满足地表水环境质量标准(GB 3838-2002)III类水标准,浮游植物主要为蓝绿藻,河流中磷的来源复杂。污染物溯源结果表明,该河DOM腐殖化程度较低,生物活性较强,主要来源于浮游植物和微生物代谢降解和沉积物在冲击和水力作用下产生的内源污染。建议该河采用生态修复技术并辅助水体曝气系统治理DOM污染,并持续防止河流引入外源污染。     

Development and validation of a GC/MS method for determination of phenolic xenoestrogens in aquatic samples

A simple and sensitive GC/MS method for the quantitative determination of the estrogenic phenolic compounds 4-nonylphenol, 4-t-octylphenol, bisphenol A, 3-t-butyl-4-hydroxyanisole, 2-t-butyl-4-methylphenol, 4-hydroxybiphenyl, 2-hydroxybiphenyl, 4-chloro-3-methylphenol, and 4-chloro-2-methylphenol in aquatic samples was developed. The method for assessing their occurrence in sewage, surface and drinking waters consists of solid phase extraction (SPE) using a polystyrene copolymer phase. After methylation of the extract HRGC/LRMS analysis was possible without any clean up, even in raw sewage samples. Limits of detection and determination were between <0.01 and 0.05 ng/l and 0.01 and 0.05 ng/l, respectively. Recoveries were above 70% with exception of 3-t-butyl-4-hydroxyanisole.     

活性炭纤维固相微萃取-气质联用色谱测定废煤气脱硫剂中的萘

采用活性炭纤维固相微萃取-气质联用色谱法测定废煤气脱硫剂中的萘含量,探讨了萃取方式、萃取时间、萃取温度、解吸条件对萃取效率的影响.结果表明,最优萃取条件为40℃下顶空萃取10 min,260℃下解吸2 min.最优萃取条件下,检测方法的线性范围为200～870 mg/L,相关系数为0.998,检测限为10 ng/L.利...     

超声波辅助萃取—气质联用色谱法测定活性污泥中的多溴联苯醚

建立了活性污泥中多溴联苯醚(PBDEs)的分析方法。活性污泥经超声波辅助萃取,用酸性硅胶、铜粉及复合硅胶柱纯化后,采用气质联用色谱(GC/MS)对7种PBDEs单体进行测定,内标法定量。结果表明,该方法具有很好的精密性和准确性,方法检测限为17～121 pg/g,加标回收率为84.5%～109.0%,相对标准偏差(RSD)为0.5%～2.8%,回收率指示物3,3’,4,4’-四溴联苯醚(BDE-77)的回收率平均值为89.2%,RSD为0.8%,能够满足活性污泥中PBDEs的测定要求。采用所建立的方法对杭州和台州的活性污泥样品进行了测定,结果显示,台州样品中PBDEs含量高于杭州样品,但两者都低于相关文献所报道的北美及欧洲国家活性污泥中PBDEs的含量。     

超声波辅助萃取GC／MS法测定垃圾渗滤液中的有机污染物

垃圾渗滤液中有机污染物众多,成分复杂.以二氯甲烷为萃取剂,超声波辅助萃取后用GC/MS法测定垃圾渗滤液中的有机污染物.与传统振荡萃取相比,超声波辅助萃取明显提高了萃取效率.在GC/MS分析部分,研究了不同极性色谱柱对有机污染物分析结果的影响.实验结果表明,极性柱比较适于测定垃圾渗滤液中极性大的有机酸、醇类等物质.非极性柱能大大提高难生化降解的烷烃类、酯类等物质的检出率.