液液萃取—气相色谱-质谱法测定丙傲来、烯酸生产废水中的特征污染物

建立了液液萃取—气相色谱-质谱法快速测定丙烯酸生产废水中苯系物、酯类、醇类、醛类和酮类等12种半挥发性有机物的分析方法。液液萃取条件为：以二氯甲烷为萃取剂,废水pH 7,分散剂甲醇加入量10 mL/L,盐析剂NaCl加入量300 g/L。各组分的工作曲线的线性关系良好。各组分的加标回收率为95.2%~116.0%,各组分的方法检出限为0.001~0.179 μg/L,相对标准偏差均小于3.5%。该方法可用于丙烯酸生产废水中主要特征有机物的快速定量检测。     

液液萃取—气相色谱-质谱法测定丙烯酸生产废水中的特征污染物

建立了液液萃取—气相色谱-质谱法快速测定丙烯酸生产废水中苯系物、酯类、醇类、醛类和酮类等12种半挥发性有机物的分析方法。液液萃取条件为:以二氯甲烷为萃取剂,废水p H 7,分散剂甲醇加入量10 m L/L,盐析剂Na Cl加入量300 g/L。各组分的工作曲线的线性关系良好。各组分的加标回收率为95.2%~116.0%,各组分的方法检出限为0.001~0.179μg/L,相对标准偏差均小于3.5%。该方法可用于丙烯酸生产废水中主要特征有机物的快速定量检测。     

加压流体萃取—气相色谱-质谱法检测土壤中邻/间/对硝基甲苯

建立加压流体萃取—气相色谱-质谱法检测土壤中邻/间/对硝基甲苯的含量.选用二氯甲烷-正己烷混合溶液(体积比1:1)作为萃取溶剂,采用加压流体萃取仪对冷冻干燥土壤样品进行萃取,经硅酸镁小柱净化后,内标法定量.实验结果表明,邻/间/对硝基甲苯在质量浓度1.0～20.0μg/mL范围内线性关系良好,相关系数不小于0.999,...     

固相微萃取—气相色谱法测定水中痕量硝基苯类化合物

建立了固相微萃取种类与气相色谱联用测定地下水中12种硝基苯类化合物的分析方法,对萃取头种类、萃取时间、萃取温度、进样口衬管种类等分析条件进行了优化。实验结果表明,该方法的检出限为0.001~0.050 μg/L,线性范围0.005~500 μg/L（相关系数大于0.997）,加标回收率为72.1%~122.0%,相对标准偏差为3.65%~12.60%。应用该方法对地下水及地表水样品进行分析,结果表明该方法具有环保、灵敏、快速、简便等特点,适用于水中痕量硝基苯、硝基甲苯类化合物和硝基氯苯类化合物的测定。     

炼油厂二硫醚恶臭污染物的监测

建立了气相色谱-质谱法(GC-MS)及硫化学发光检测气相色谱法(GC - SCD)定性和定量测定炼油厂二硫醚类恶臭污染物二甲二硫、乙基甲基二硫醚和二乙基二硫醚的方法.当进样体积为0.1mL时,GC - SCD法的二硫醚最低检出限为0.1～0.2 mg/m3,二甲二硫和乙基甲基二硫醚的RSD不超过2.4％(n=5),二甲...     

气相色谱-质谱联用法快速检测溴代物阻燃剂

建立了废旧电子电器产品塑料及线路板中溴代物阻燃剂的气相色谱-质谱联用快速检测方法。以氯仿-正己烷（体积比为1：1）为萃取剂，超声萃取1h后，4种阻燃剂的回收率均高于91％，相对标准偏差低于0．51％，方法检出限为5mg／kg。该方法萃取时间短，操作简便，实用性强，可成功用于多种多溴联苯醚和四溴双酚A的检测。     

固相萃取—微波衍生化—GC-MS法同时测定水中6种雌激素物质

建立了固相萃取—微波衍生化—气相色谱-质谱联用法快速同时测定水中雌酮（E1）、17α-雌二醇（α-E2）、17β-雌二醇（β-E2）、雌三醇（E3）、17α-乙炔基雌二醇（EE2）、双酚A（BPA）等6种雌激素物质的分析方法,对色谱柱升温程序、固相萃取及衍生化条件进行了优化。色谱柱最佳升温程序为：初始温度50 ℃,保持2 min;以20 ℃/min速率升至260 ℃,保持5 min;最后以10 ℃/min速率升至280 ℃,保持5 min。实验结果表明,在选取 HC-C18萃取小柱、添加双（三甲基硅烷基）三氟乙酰胺（BSTFA）+1%三甲基氯硅烷（TMCS）+吡啶作为衍生化试剂、微波315 W衍生化加热4 min的条件下,6种目标物标准曲线的相关系数均大于0.999,BPA、E1、EE2及E3的线性范围为3~300 ng/L,17α-E2及17β-E2的线性范围为5~300 ng/L,方法检出限为2.0~5.0 ng/L,加标回收率为76.45%~96.24%。     

浮选水中PPb级α—松油醇的热导气相色谱法

作者使用自行设计的V型浓缩器,以石油醚萃取浓缩浮选水中α-松油醇。整个分析操作中用正辛醇作内标物。在大量使用盐析剂的条件下,相比可达40,一次萃取收率达95％,实际富集比可达8000—20000倍。经浓缩富集的样品以热导气相色谱法定量。该方法的最低检测浓度为2ppb。在50ppb处的相对标准偏差为2—3％。     

萃取浓缩-薄涂柱气相色谱法测定煤焦油废水中的联苯和菲

用苯萃取浓缩煤焦油废水中的联苯和菲，然后用薄涂柱气相色谱法进行测定。试验表明：该法具有色谱柱温低、快速、准确等特点。     

用顶空色谱—质谱法直接测定化工废水中挥发性有机污染物

化工废水中挥发性有机污染物常属于有毒有害化合物,当对污染源监督监测时,若采用萃取法,则存在溶剂干扰待测轻组分、预处理步骤繁琐、分析时间长等缺点。本文介绍测定化工废水中挥发性有机污染物的顶空色谱-质谱法。该方法采用质谱定性,并省去了样品的预处理步骤,使分析时间缩短。     

Development of a simple and sensitive method for the characterization of odorous waste gas emissions by means of solid-phase microextraction (SPME) and GC-MS/olfactometry

A solid-phase microextraction (SPME) method has been developed for the extraction of odorous compounds from waste gas. The enriched compounds were characterized by gas chromatography-mass spectrometry (GC-MS) and gas chromatography followed by simultaneous flame ionization detection and olfactometry (GC-FID/O). Five different SPME fiber coatings were tested, and the carboxen/polydimethylsiloxane (CAR/PDMS) fiber showed the highest ability to extract odorous compounds from the waste gas. Furthermore, parameters such as exposure time, desorption temperature, and desorption time have been optimized. The SPME method was successfully used to characterize an odorous waste gas from a fat refinery prior to and after waste gas treatment in order to describe the treatment efficiency of the used laboratory scale plant which consisted of a bioscrubber/biofilter combination and an activated carbon adsorber. The developed method is a valuable approach to provide detailed information of waste gas composition and complements existing methods for the determination of odors. However, caution should be exercised if CAR/PDMS fibers are used for the quantification of odorous compounds in multi-component matrices like waste gas emissions since the relative affinity of each analyte was shown to differ according to the total amount of analytes present in the sample.     

Industrial wastewater analysis: a toxicity-directed approach

Methods of toxicity-directed analysis have been developed for the characterization and identification of toxic organic constituents in industrial wastewater. Sequential solid-phase extraction is followed by high-performance liquid chromatography (HPLC) fractionation or by automated multiple development thin-layer chromatography fractionation (AMD–TLC) of the toxic extracts. Toxic fractions were finally analyzed by gas chromatography–mass spectroscopy (GC–MS). Toxicity was detected before each of the analytical steps by the bioluminescence inhibition of Vibrio fischeri, which was performed on microtiter plates and on the developed TLC plates. While sequential extraction broadens the polarity range of the procedure, the new variants of the luminescence test make the method very versatile and fast. The potential of this kind of toxicity-directed analysis with respect to resolution and polarity of analytes is discussed and applications to partial effluents of a tannery, to molasses wastewater and a spent dyeing bath are presented. A variety of benzothiazoles and more polar organics were identified as major toxic compounds in tannery effluents. It is shown that the procedures are well suited to detect individual toxic components in complex industrial wastewaters. The use of LC-MS is proposed to extend the polarity range of the final identification step. ©     

Substance-specific detection and pursuit of non-eliminable compounds during biological treatment of waste water from the pharmaceutical industry

Up to now comprehensive examination and assessment of the elimination behaviour of many different pollutants in biological waste water treatment failed above all because of limited possibilities to pursue polar organic compounds of anthropogenic and biogenic origin. In this case the behaviour of waste water constituents during the treatment of waste water from the pharmaceutical industry was studied with the help of mass-spectrometric detection (MS). After completest possible extraction and concentration by liquid/liquid and solid phase extraction (SPE) from samples of influent and effluent of a pilot plant, substance-specific determination and identification was done after chromatographic separation and with the help of mixture analysis, respectively. Separation by gas chromatography coupled with MS was applied to pursue the organic compounds, which are volatile without decomposition, during the waste water treatment process. Flow injection analysis (FIA) bypassing the analytical column combined with soft-ionizing interfaces served for screening of the polar compounds. Then they were separated by liquid chromatographic methods to recognize changes in the qualitative and quantitative compound spectrum. Mixture analysis by FIA combined with tandem mass spectrometry (FIA/MS/MS) was used for identification of the pollutants without previous chromatographic separation. A laboratory-made daughter ion library helped to identify some of the poorly eliminable pollutants detected. The presentation of the monitoring procedures applied was made in such a way that the treatment results were visually recognizable. Due to the use of time-saving FIA/MS, this method may serve for substance-specific monitoring of the treatment of possibly problematic waste waters. ©     

New methodology for a selective on-line monitoring of some polar priority industrial chemicals in waste water

A new methodology is described for the development of on-line measurements of selected hazardous polar pollutants in waste water. The on-line automated system consists of a selective solid-phase extraction in order to isolate, concentrate and clean up industrial waste water in one step followed by liquid chromatography and diode array or mass spectrometry detection. The new solid-phase extraction sorbents involve antigen–antibody interactions. Due to the high affinity and high selectivity of these interactions, extraction and clean-up of aqueous complex matrices are achieved on the same step. Therefore, chromatograms present very clean base-lines which greatly improves the detection and quantification of very polar analytes. Identification of analytes is reinforced since immunoextraction is based on a molecular structural recognition. Class-selective immunosorbents have been developed for the selective trapping of several groups of analytes structurally related such as polyaromatic hydrocarbons, benzidine and congeners, nitroaniline and aromatic amines. Comparison is given with real samples showing that most polar analytes cannot be detected at low level using conventional non-selective solid-phase extraction sorbents. Examples are presented for the determination of the two- to three-ring polyaromatic hydrocarbons as well as of basic polar industrial chemicals such as nitroaromatics and aromatic amines which are included in the US EPA or EEC priority lists of pollutants to be monitored in industrial effluents. These on-line procedures increase the speed of analysis, improve analyte delectability and can be integrated into on-site monitoring devices. ©     

Feedstock recycling from plastic and thermoset fractions of used computers (I): pyrolysis

The increasing production of computers, the progress in their performance, and the shorter time between innovation and production has led to increasing numbers of obsolete products. It has thus become necessary to recover some materials from old computers and to protect the environment from a new type of pollution. Such recycling is difficult because of the diversity of polymeric materials used, e.g., thermoplastics (polystyrene or acrylonitrile-butadiene-styrene) and thermosets (epoxy resins), and the relatively high levels of flame retardants (halogen- and nitrogen-containing compounds) added during production. Pyrolysis seems to be a suitable way to recover materials and energy from such waste without component separation if an efficient method for reducing toxic compounds can be applied. In this study, the pyrolysis of plastic and thermoset fractions (keyboards, casings, printed circuit boards, and mixtures thereof) of used computers was studied by thermogravimetry and batch reactor pyrolysis. The degradation products were separated into three fractions, solid, liquid, and gaseous, each of them being characterized by suitable methods such as gas chromatography (GC-MSD, gas chromatography-mass spectrometry detection; GC-AED, gas chromatography-atomic emission detection), infrared (FT-IR) and 1H-NMR (nuclear magnetic resonanace) spectroscopy, and elemental analysis. It has been established that most of the halogens, nitrogen, and sulfur is concentrated in the residue. However, the elimination of hazardous toxic compounds, mainly those containing bromine, is necessary before being able to safely use the pyrolysis oils as fuels or in refinery or petrochemical industry flows.     

Study of the Determination of the Ultimate Aerobic Biodegradability of Plastic Materials Under Controlled Composting Conditions

Several ISO standards for determining the ultimate aerobic/anaerobic biodegradability of plastic materials have been published. In particular, ISO 14855-1 is a common test method that measures evolved carbon dioxide using such methods as continuous infrared analysis, gas chromatography or titration and others (ISO 14855-1(2005.9)). This method is a small-scale test for determining the ultimate aerobic biodegradability of plastic materials, where the amounts of compost inoculum and test sample in one tenth comparing with that of ISO 14855-1. This method is well versed in ISO/DIS 14855-2 which the carbon dioxide evolved from test vessel is determined by gravimetric analysis of carbon dioxide absorbent. The focus of this study is to elucidate statistically the results of round robin test by seven countries used MODA, which were various deviations among the experiments.     

二恶英类化合物检测方法的研究现状及展望

介绍了二恶英类化合物的检测方法,并对各种检测方法的原理和应用进行了对比分析;其中高分辨率色谱/质谱法、荧光素酶报告基因法及酶免役分析法在实践中取得了很好的检测效果;CALUX 法与其他生物检测方法相比更适合于大批量样品中二恶英含量的快速定量筛选,对于二恶英污染调查有广阔的应用前景;综述了我国二恶英类化合物检测方法的研究现状,并对我国开展二恶英分析监测提出了建议和展望.     

油气生产过程中放空燃烧气的检测与回收利用现状

本文对油气生产中放空燃烧气的检测方法进行了总结,并对国内外放空气回收利用的主要技术进行了比较分析。指出:利用遥感监测数据计算放空燃烧气量具有较好的应用前景,但需同地面常规实测数据结合,改进反演算法,以减少不确定性;采用油气混输、天然气发电、压缩天然气（CNG）、液化天然气（LNG）、液态产品转化等回收利用手段将显著减少放空燃烧气带来的温室气体排放。