On-line dechlorination–hydrogenation of chlorinated paraffin mixtures using GC and GC/MS

Chlorinated paraffins (CPs) are straight chain hydrocarbons that are produced as complex mixtures and are used as flame retardants and paint additives. These mixtures are extremely difficult to characterize using conventional chromatographic methods, as conventional gas chromatography results in unresolved complex chromatograms that preclude the identification and quantification of individual congeners or any reasonable assessment of the average carbon chain length. Carbon chain length is an important parameter for assessing physical properties and the toxicity of these materials. We have modified and improved a previously published gas chromatography–flame ionization detector method that uses Pd catalyst held in the gas chromatograph injector to simultaneously dechlorinate the CPs and separate the resulting alkanes. In addition, we have adapted this method to gas chromatography–mass spectrometry. Dehalogenation of other compounds was also studied with this system to investigate potential application to other complex halogenated mixtures.     

U PLC- ESI- MS/MS法同时测定水中7种抗生素

采用超高效液相色谱-电喷雾二级质谱联用技术同时测定水中7种抗生素,优化了试验条件.磺胺甲恶唑、诺氟沙星、环丙沙星、氧氟沙星、四环素在1.00 ng/L～1000 ng/L范围内线性良好,定量下限为1 ng/L,土霉素、金霉素在10.0 ng/L-2 000 ng/L范围内线性良好,定量下限为10 ng/L,去离子水和地表水样加标回收率为72.1%-112%,RSD为0.6%～9.2%.     

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.     

多氯联苯的气相色谱/质谱/质谱(GC/MS/MS)法测定

采用气相色谱/质谱/质谱(GC/MS/MS)法测定多氯联苯(PCB),具有良好的灵敏度和选择性,在地表水样品检测时,样品只须进行简单的液液萃取-浓缩,不须任何净化过程即可上机分析,方法检出限低于ng/L级。     

GC/MS法测定黄浦江水中挥发性有机化合物

采用吹扫捕集装置与GC／MS联用仪的全自动恒流控制,对黄浦江7个断面水样中47种挥发性有机化合物进行了分析。结果表明,被查的47种挥发性有机化合物基本都有检出,其中甲苯、异丙苯的绝对检出量最高。四氯化碳的检出值也较高,吴淞口四氯化碳的平均浓度已经远远超过GB3838—2002《地表水环境质量标准》,并且四氯化碳浓度在黄浦江流域各个断面的分布具有一定规律性。     

ICP—MS法测定饮用水中的铅

采用ICP—MS法对饮用水中的铅进行了分析测定。并进行了载气流量的选择、定量离子质荷比的选择和内标的选择等实验．本实验铅的质荷比选用206，207和208三个加在一起计算。方法的检测限为0．5×10-3mg／L，精密度实验的变异系数为3．25％～7．63％。     

施工现场中有毒气体的GC／MS分析

通过对某单位在建楼打桩挖井中的毒气，用毛细管色谱／质谱法测试分析，毒气成份主要为ＣＯ，其浓度超出居民区最高允许浓度９６倍，同时对产生ＣＯ的原因作了分析。     

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.     

HS/SPME-GC/MS/MS法测定水中痕量2-甲基异莰醇和土臭素

建立了测定水中痕量2-甲基异莰醇(2-MIB)和土臭素(GSM)的顶空固相微萃取-气相色谱/二级质谱联用法(HS/SPME-GC/MS/MS),并对HS/SPME条件进行优化。优化后的方法 2-MIB和GSM在1.00~50.0 ng/L范围内,线性良好(r≥0.999 4),RSD分别为7.36%和7.75%,方法检出限分别为0.226和0.239 ng/L,加标回收率分别为87.0%~97.0%和85.2%~112%。结果表明,所建立的方法操作简便、准确度高、重现性好、灵敏度高,无需有机溶剂,适用于水中痕量2-MIB和GSM的测定。     

GC／MS法测定自来水中挥发性有机化合物

应用ＧＣ／ＭＳ联用仪对自来水中挥发性有机化合物进行了测定,实现了了吹扫－捕集装置与联用仪的连接,并由ＤＰＦＣ控制,使整个过程自动化。检测的自来水样中,主要有氯甲烷类,溴氯甲烷类和苯类等挥发性化合物。     

HPLC和HPLC-MS/MS测定地表水中酚类化合物

采用高效液相色谱法(HPLC)和高效液相色谱-三重四级杆质谱联用法(HPLC-MS/MS)测定地表水及饮用水中11种酚类化合物,通过优化测定条件,使HPLC法在0.020 mg/L~50.0 mg/L范围内,HPLC-MS/MS法在0.500μg/L~250μg/L范围内线性良好,方法检出限分别为0.005μg/L~0.031μg/L和0.005μg/L~1.56μg/L。未检出的实际样品加标回收率分别为57.2%~96.7%和81.3%~113%,RSD分别为1.5%~5.3%和3.9%~17.7%。     

SPE-UPLC-MS/MS法测定地下水中多种农药残留

采用固相萃取超高效液相色谱串联质谱法(SPE-UPLC-MS/MS)同时测定地下水中涕灭威、克百威、2,4滴和五氯酚等4种农药残留,通过优化试验条件,使方法在10.0μg/L～200μg/L范围内线性良好,检出限为0.003μg/L～0.006μg/L.标准溶液低、中2个质量浓度水平的加标回收率为84.1％ ～98.8...     

GC-MS/MS法测定水中多种N-亚硝胺类化合物

采用固相萃取-GC-MS/MS法测定水中10种N-亚硝胺类化合物,通过试验优化前处理和测定条件,使方法在0. 500μg/L～100μg/L范围内线性良好。方法检出限为0. 6 ng/L～2. 1 ng/L,混合标准溶液6次测定结果的RSD 5%。将该方法用于测定实际水样,结果除N-亚硝基二甲胺、N-亚硝基甲基乙基胺和N-亚硝基二丙胺以外,其余目标物均为未检出,加标回收率为73. 1%～97. 6%。     

GC/MS法测定水中烷基酚聚氧乙烯醚和烷基酚

采用气相色谱/质谱联用测定环境水体中壬基酚、壬基酚一氧乙基醚、壬基酚二氧乙基醚、4-叔辛基酚、4-叔辛基酚一氧乙基醚和4-叔辛基酚二氧乙基醚,用二氯甲烷对水样液液萃取,浓缩后添加BSTFA+ TMCS(体积比为99∶1)在室温下衍生化0.5h.方法在0.001 mg/L～5.00 mg/L范围内线性良好,目标化合物的检出限范围为4.0×10-7 mg/L～8.8×10-7 mg/L,空白加标样品平行测定的RSD为5.1％ ～8.8％,回收率为85.6％～ 110％.     

ICP/ MS 法对实验室用水的分析

采用电感耦合等离子光谱和质谱法对超纯水、去离子水和蒸馏水3种实验用水进行半定量和定量分析。通过对主要相关元素的分析结果比较，超纯水的水质优于其他两种，更适宜作为无机元素痕量分析的实验用水。     

超声波萃取-GC/MS法测定土壤中多氯联苯

建立了超声波萃取、氟罗里硅土柱净化、气相色谱/质谱联用选择离子扫描模式测定土壤样品中多氯联苯Arochlor系列的方法.方法线性良好,灵敏度高,RSD为9.5%～12.2%,加标回收率为65.0%～105%,标准土壤样品的测定结果也符合要求.     

EPA方法524.2化合物的GC/MS分析

1 引言 EPA方法524.2 第4.1版(1995)是为配合实施美国国家饮用水的EPA标准而制订的,该方法采用吹脱捕集装置,用GC/MS 检测低浓度的被分析物质。其中有些被分析物质捕集效率很低,捕集后浓度刚刚达到方法的检测限且难以完全分离。本章简要介绍了Agilent公司成功分析EPA方法的各种条件,这些方法和步骤均经Agilent公司测试并全部符合EPA要求。所测化合物见EPA 524.2 (3.0版,1989),更详细的方法内容,参见EPA 524.2(4.1版)。 GC/MS具有以下优点:(1)比一般的GC检测器分析的物质范围更宽、更准,(2)可以鉴别复杂基质中的化合物,(3)可有效…     

SPE-GC-MS/MS法测定水源水中多种有机氯EDCs

采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。     

GC／MS在水污染事故监测中的应用

用ＧＣ／ＭＳ仪对一起严重的水污染事故水样进行了监测,检出的几十种化合物中,有多种与某化工厂的原料,产品及其中间体相吻合,该厂排放的污水与被污染河水水样有极其相似的指纹特征,迅速地判定了污染事故的责任者。