重点行业企业用地地下水中挥发性有机物分析方法探究

通过优化顶空条件(氯化钠加入量、顶空平衡温度、顶空平衡时间),对采用顶空-气相色谱-质谱联用法测定地下水中55种挥发性有机物的方法进行探究。结果表明:该方法检出限为0.24~2.30μg/L,相对标准偏差为0.76%~13.2%,实际样品加标回收率为82.7%~119%。该方法具有较高的灵敏度、精密度和准确度,操作简便,可用于企业用地地下水中挥发性有机物的检测。     

土壤中挥发性芳香烃的顶空前处理方法研究

本方法针对土壤中挥发性芳香烃顶空前处理条件进行了研究,优化了顶空密封垫的选择、顶空平衡温度、加热平衡时间、进样时间和顶空瓶压力等顶空前处理条件,测定条件科学、准确,完全能够满足土壤中挥发性芳香烃监测分析的灵敏度和准确度相关的技术要求。该方法精密度为1.7%~9.8%,准确度为34.3%~83.7%,检出限为2.0~4.2μg/kg。为制订土壤中挥发性芳香烃监测分析方法提供了技术支持。     

顶空-气相色谱-质谱法测定土壤中卤代烃

建立顶空-气相色谱-质谱法同时测定土壤中挥发性及半挥发性卤代烃的方法。实验优化顶空平衡温度、顶空平衡时间及盐度条件,并对优化后方法的线性、检出限、精密度及回收率进行分析。结果表明:29种目标化合物在线性范围内线性良好,相关系数均大于0.997,方法检出限为2.2~5.9μg/kg,样品不同浓度水平加标回收率范围为80.0%~120%,相对标准偏差小于20%。该方法适用于土壤样品中挥发及半挥发性卤代烃的测定。     

对固体废物中挥发性有机物浸出方法的几点实验探讨

采用零顶空提取器,对陈旧油墨渣和蒽琨渣样品中的挥发性有机物进行了浸出实验和分析测定,浸出液采用静态顶空分流进样、GC/MS法分析。对影响挥发性有机物浸出效率的因素进行了研究,结果表明,浸提剂加入方式、浸出时间和浸出液收集方法等对分析结果准确度有较大影响。     

顶空气相色谱质谱法测定土壤中挥发性卤代烃方法研究

采用顶空气相色谱质谱法(HS/GC-MS)对土壤中挥发性卤代烃进行了测定,优化了分析的顶空条件、气相色谱质谱分离条件。在优化条件下成功实现了24种挥发性卤代烃的分离,确定了分析方法的检出限、测定下限、精密度及回收率等质量控制参数。方法的检出限为0.8~4.4μg/kg,测定下限为3.2~17.6μg/kg。当加标量为100μg/kg和250μg/kg时,相对标准偏差分别为1.3%~12.6%和2.6%~8.7%,加标回收率分别为71.4%~126%和63.1%~121%。     

加压流体萃取-GC/MS法测定土壤中半挥发性有机物

采用加压流体萃取〖CD*2〗气相色谱/质谱联用法（ASE GC/MS）测定土壤中9种半挥发性有机物,分别考察萃取条件、氮吹浓缩、硅酸镁小柱净化和浓缩定容等前处理条件对半挥发性有机物测定的影响。通过优化试验条件,使方法在100 μg/L～1 000 μg/L范围内线性良好,方法检出限为0.01 mg/kg～0.04 mg/kg。土壤样品加标回收率为72.4%～954%,4次测定结果的RSD为2.1%～6.0%。将该方法应用于测定某重点行业企业用地周边土壤,除苯并（a）芘外其余8种半挥发性有机物均为未检出。     

顶空气相色谱法测定土壤中BTEX

本文采用顶空气相色谱法从土壤样品中分离挥发性有机物。应用该技术,苯、甲苯、乙基苯及二甲苯异构体（ＢＴＥＸ）均得到有效分离。该方法有较好的精密度（变异系数６５％,回收率８９～１０３％）和低的检出限（对于苯为０５ｎｇ／ｇ）。土壤样品中加入水或加热,可提高方法的灵敏度。     

Elite-FFAP色谱柱气相色谱法测定水中苯系物方法探索

本方法利用顶空-毛细柱气相色谱技术对水中的苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯七种挥发性苯系物进行同时测定。对样品平衡温度、样品平衡时间、程序升温的条件控制、氯化钠的浓度等条件进行了摸索,建立了利用了Elite-FFAP色谱柱测定水中七种挥发性苯系物的方法。     

顶空-气相色谱/质谱法测定土壤中挥发性有机物

本方法采用静态顶空进样技术对土壤样品进行处理,利用气相色谱质谱联用对土壤中挥发性有机物(37种)进行了测定分析,通过测定得到最低检出浓度为:0.39～1.76μg/kg;加标回收率为:69.8%～110.2%;RSD为:3.1%～10%。本实验分析时间短,操作简单,灵敏度及测定结果较为满意。     

车载顶空-气相色谱质谱法在水体挥发性有机污染物应急监测中的应用

建立了车载顶空-气相色谱质谱法(GC/MS)测定水中22种挥发性有机物(VOCs)的方法,顶空平衡温度和平衡时间的最优设置分别为80℃和30 min。该方法各目标化合物分离良好,在目标化合物质量浓度5~100μg/L范围内,线性良好,相关系数均0.995,方法的检出限为1.16~2.88μg/L,RSD为7.71%~26.5%,加标回收率为52.3%~129%,能够满足应急监测工作的需要。     

Characterization of an urban landfill soil by using physicochemical analysis and solid phase microextraction (SPME)—GC/MS

We have aimed at characterizing top soil samples taken in-situ from five different locations of the unregulated dumping site in Eskişehir/Turkey for a period of six months. The study is the first attempt in the city and in Turkey, regarding particularly the SPME (Solid Phase Microextraction Technique) analysis method utilized. A comprehensive research has been conducted to produce critical soil data to be used for indicating current risks as well as the urgency of rehabilitating the site and establishing a sanitary landfill in the site. Conventional physicochemical analytical methods and SPME technique were used to analyze the samples. Physicochemical analyses were performed for determining the pH, total dried matter, volatile matter, total nitrogen, phosphorus, macro elements and heavy metals. Meteorological data were also recorded for the same period. SPSS.10.0 statistical program was used to determine the correlation between meteorological data and physicochemical analysis results. Mean values were used in the correlation analyses. These data indicated that the air temperature and precipitation have significant effects on soil characteristics. SPME, coupled with GC/MS, was used to identify eighty six volatile and semi-volatile organic compounds contained in soil samples. The samples were extracted by headspace SPME with heating (δHS-SPME). SPME analyses were conducted using a commercially available polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber having a film thickness of 65 μm (Supelco) as a capture medium. The experimentally optimized headspace sampling conditions were arranged (15 min. at 50^˚C) before a 30 min. sampling period.     

土壤中挥发性有机污染物现场快速监测技术应用进展

在总结我国突发性环境事故发生现状的基础上,提出了我国环境现场快速监测工作缺少规范化管理,以及标准监测技术方法不完善等问题。探讨了土壤中挥发性有机污染物快速监测技术的研究进展,重点讨论了检测管,手持式气体检测器,便携式气相色谱(配置光离子化检测器、氢火焰离子化检测器或串/并联检测器)及便携式气相色谱-质谱等技术在快速检测土壤中挥发性有机污染物方面的性能特点与应用情况,并对我国建立土壤中挥发性有机污染物现场快速监测标准方法提出了建议。     

Visualising the equilibrium distribution and mobility of organic contaminants in soil using the chemical partitioning space

Assessing the behaviour of organic chemicals in soil is a complex task as it is governed by the physical chemical properties of the chemicals, the characteristics of the soil as well as the ambient conditions of the environment. The chemical partitioning space, defined by the air-water partition coefficient (K(AW)) and the soil organic carbon-water partition coefficient (K(OC)), was employed to visualize the equilibrium distribution of organic contaminants between the air-filled pores, the pore water and the solid phases of the bulk soil and the relative importance of the three transport processes removing contaminants from soil (evaporation, leaching and particle erosion). The partitioning properties of twenty neutral organic chemicals (i.e. herbicides, pharmaceuticals, polychlorinated biphenyls and volatile chemicals) were estimated using poly-parameter linear free energy relationships and superimposed onto these maps. This allows instantaneous estimation of the equilibrium phase distribution and mobility of neutral organic chemicals in soil. Although there is a link between the major phase and the dominant transport process, such that chemicals found in air-filled pore space are subject to evaporation, those in water-filled pore space undergo leaching and those in the sorbed phase are associated with particle erosion, the partitioning coefficient thresholds for distribution and mobility can often deviate by many orders of magnitude. In particular, even a small fraction of chemical in pore water or pore air allows for evaporation and leaching to dominate over solid phase transport. Multiple maps that represent soils that differ in the amount and type of soil organic matter, water saturation, temperature, depth of surface soil horizon, and mineral matters were evaluated.     

Application of HS-SPME in the determination of potentially toxic organic compounds emitted from resin-based dental materials

Leaching of volatile substances from resin-based dental materials may have a potential impact on the biocompatibility as well as safety of these materials. Information from manufacturers on ingredients in the materials is very often incomplete. Patients and dentists may be in contact with components emitted from cured dental fillings or from substrates applied in their preparation. Therefore, determination of the components of these materials is necessary for better prevention from possible harmful effects caused by dental fillings. The aim of this work was the isolation and identification of organic compounds evolved from four commercial resin-modified glass-ionomer cements (resin-based dental materials applied in dentistry) by using an alternative method of volatile compounds analysis-HS-SPME (headspace-solid phase microextraction). Dental materials were heated in closed vial at various temperatures and volatile substances released into the headspace phase above the sample were isolated on a thin polymeric fibre placed in SPME syringe. Identification was performed by using the GC-MS (gas chromatography-mass spectrometry) technique. Almost 50 RMGIC (resin-modified glass-ionomer cement) components (monomers and additives) were identified. The main identified leachables were: iodobenzene (DPICls-diphenyliodonium chloride degradation product), camphorquinone (photo-initiator), tert-butyl-p-hydroxyanisole (inhibitor), 4-(dimethylamino)ethyl benzoate (co-initiator), ethylene glycol dimethacrylate (monomer).     

室内人造板材制品释放挥发性有机化合物研究

通过对浸渍纸层压木质地板、实木地板、实木复合地板、竹地板、胶合板、细木工板6种共39个人造板材中的挥发性有机物进行定性研究,确定了家用人造板材制品释放的主要挥发性有机物种类,以及人造板材制品中芳香族化合物的主要来源.通过对5间购入新家具的室内环境空气中甲醛、苯、甲苯和总挥发性有机化合物(TVOC)的定量分析,确定了人造板材制品释放挥发性有机化合物的污染水平.研究表明,人造板材释放的挥发性有机化合物以烯烃、芳香族、酯类化合物为主,其中芳香族化合物主要来源于胶合板和细木工板,室内人造板材制品的使用可以使室内环境空气中挥发性有机化合物的质量浓度显著提高.     

吹扫捕集-气相色谱质谱法分析土壤和沉积物中挥发性有机物

采用吹扫捕集-气相色谱质谱法对土壤和沉积物中挥发性有机物进行分析,优化了实验条件,所有物质的相对标准偏差小于5.0％,土壤样回收率在78.2％ ～99.8％之间,沉积物样的回收率在55.2％～95.2％之间.     

对TH_PKU-300B挥发性有机物快速在线监测系统的改进

针对现有TH_PKU-300B挥发性有机机物快速在线监测系统在测定含氧挥发性有机化合物(OVOCs)、含氮挥发性有机物(NVOCs)和高沸点挥发性有机物时存在灵敏度低、精密度差、线性响应较差、记忆效应明显等不足,根据其原理,对其GC-MS通道的部分气路进行改进。通过实验对比分析,证明改进后的仪器系统响应更加灵敏、线性拟合度更高、精密度及解析效率均显著提高,同时检出限也由改进前的体积分数0.1×10~(-9)~1.0×10~(-9)降低至0.02×10~(-9)~0.08×10~(-9),并解决了记忆效应问题。改进后的系统在OVOCs、NVOCs和高沸点挥发性有机物测定方面要优于原系统。     

HS-SPME/GC–MS analysis of volatile and semi-volatile organic compounds emitted from municipal sewage sludge

The aim of the research involved identification and semi-quantitative determination of unknown volatile and semi-volatile organic compounds emitted to air by sewage sludge formed in the process of municipal wastewater treatment in a sewage treatment plant. Samples taken directly after completion of the technological process as well as the sludge stored on the premise of the sewage treatment plant were analyzed. A simple method using off-line headspace solid-phase microextraction combined with gas chromatography–mass spectrometry has been proposed for extraction and detection of organic pollutants. For reliable identification of compounds, combination of two independent parameters: mass spectra and linear temperature programmed retention indices were employed. Over 170 compounds of different structure were identified including aliphatic and aromatic hydrocarbons, alcohols, esters, carbonyls, as well as sulfur, nitrogen, and chlorine containing compounds. The prevailing substances included: ethyl ether, n-hexane, p-xylene, o-xylene, mesitylene, m-ethylbenzene, limonene, n-decane, n-undecane, and n-dodecane. A few compounds such as methanetiol, dimethyl polisulfide, octaatomic sulfur, phthalic anhydride, and indoles were identified in the sludge for the first time.