吹扫捕集-GC/MS法测定饮用水中致嗅物质

采用吹扫捕集-气相色谱/质谱联用法测定饮用水中6种致嗅物质,优化了吹扫捕集条件。方法线性良好,甲硫醚、二甲二硫、甲苯、异佛尔酮、癸醛、β-环柠檬醛的检出限分别为10.5μg/L、0.558μg/L、0.862μg/L、47.4μg/L、4.75μg/L、3.77μg/L,标准溶液平行测定的RSD≤10.9%,加标回收率为71.0%～125%。     

吹扫捕集-色质联机测定水中挥发性硫醚

采用吹扫捕集-色质联机测定水中挥发性硫醚,采用外标法,使用SIM模式对甲硫醚、乙硫醚和二甲二硫醚三种成分进行定量,方法的检出限分别为0.02、0.05和0.08μg/L,三种物质浓度在0.40~40μg/L范围内,测定结果有良好的线性,一次回归曲线的相关系数分别为0.9998、0.9999和0.9999。利用该方法对内河等实际样品进行分析,结果平行性良好,加标回收率在75.2%~88.4%之间。     

吹扫捕集-气相色谱法测定水中四乙基铅

通过探讨影响四乙基铅富集效率的捕集管类型、吹扫温度和吹扫时间等因素,建立了吹扫捕集-气相色谱法测定水质中四乙基铅的分析方法。实验结果表明,使用Tenax捕集管,在吹扫温度为50℃、吹扫15 min的条件下测定水质中的四乙基铅,捕集效率为97.6%~98.2%,在0~100μg/L范围内线性良好,检出限为0.03μg/L,加标回收率为93.2%~100.5%,相对标准偏差为1.6%~3.2%。方法操作简便快捷、准确、实用且绿色环保不消耗有机溶剂,适于水质中四乙基铅的测定。     

吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈和吡啶

水中的乙醛、丙烯醛、丙烯腈和吡啶经吹扫捕集、解吸后,用HP-VOC毛细管色谱柱进行GC分离,用GC-MS法选择离子模式(SIM)下进行检测,外标法定量。结果表明,选择取样量25 m L,吹扫流量为40 m L/min,吹扫温度为40℃,吹扫时间为15 min,解吸时间为2 min,解吸温度为200℃,烘焙时间20 min,乙醛和吡啶质量浓度在0.025~0.60 mg/L之间,丙烯醛和丙烯腈质量浓度在0.002 5~0.10 mg/L之间时,校准曲线呈线性关系,相关系数r0.995,乙醛、丙烯醛、丙烯腈和吡啶的方法检出限分别为0.001 6,0.001 3,0.000 5和0.002 1 mg/L。对3个不同浓度样品进行空白加标实验,测量的回收率为87.8%~114.3%,相对标准偏差(n=6)为2.51%~10.4%。对3批实际水样进行分析,其中一个废水水样加标回收率为79.2%~103.8%,相对标准偏差(n=6)为3.04%~6.39%。     

P&T-GC-MS法测定水中54种挥发性有机物

建立了同时测定水中54种挥发性有机物(VOCs)的吹扫捕集-气相色谱-质谱联用法,并对吹扫捕集条件进行了优化。优化后的方法,54种VOCs在0.50~40.00μg/L质量浓度范围内线性良好,相关系数R2均0.995 6,检出限为0.021~0.105μg/L,加标回收率为76.4%~110.8%,相对标准偏差为2.33%~15.8%。该法操作简单,消耗费用低,分析速度快,具有良好的灵敏度、回收率和重现性,能够满足生活饮用水中54种VOCs的同时测定。     

吹扫捕集装置在测定地表水中挥发性有机物的最佳测试条件

吹扫捕集法自1974年提出以来被广泛的用于地表水、地下水、饮用水和废水中挥发性、半挥发性有机物的检测。吹扫捕集／气相色谱联机有很好的方法检测限,可以检测出浓度为0．1μg／L的挥发性有机物,但水样中这类有机物的含量通常是痕量级别,要做到准确测量,需要仪器检测时的条件处于最佳,现对吹扫捕集装置的性能、吹扫时间、解吸时间和解吸温度等条件进行选择。     

三甲基氯硅烷及六甲基二硅氮烷水解产物分析方法研究

研究采用吹扫捕集-气相色谱-质谱法测定三甲基氯硅烷及六甲基二硅氮烷水解产物的分析方法。结果表明,两种物质遇水迅速水解,水解产物均为三甲基硅醇与六甲基二硅氧烷。以该方法测定六甲基二硅氧烷的检出限为0.02ng/ml,精密度为1.3%～10.6%,线性范围为0.05～60ng/ml。水解动力学研究结果表明,三甲基氯硅烷及六甲基二硅氮烷水解产物含量随时间减少而降低,强酸、强碱条件下测试未发现生成其他的水解产物。该方法可为同类污染物的应急测试提供参考。     

吹扫捕集-气相色谱/质谱法测定水中的乙醛、丙烯醛、丙烯腈、吡啶、松节油和丁基黄原酸

建立了一种吹扫捕集-气相色谱/质谱法同时测定水中的乙醛、丙烯醛、丙烯腈、吡啶、松节油和丁基黄原酸的分析方法。结果表明,吹扫时间、脱附时间、脱附温度和盐酸用量是影响目标化合物测定的关键因素,对吹扫捕集条件优化后,各目标化合物线性良好,相关系数均0.998,检出限为0.13~2.22μg/L,加标回收率为80.5%~111%,相对标准偏差为1.1%~10.9%,能够满足地表水环境质量标准的要求。     

吹扫捕集-气相色谱质谱法测定土壤中四乙基铅

文章系统研究了土壤中四乙基铅的吹扫捕集-气相色谱质谱测定方法，优化了吹扫捕集前处理条件参数。结果表明，吹扫时间13 min、吹扫温度60℃，脱附温度190℃，脱附时间1 min为最佳的吹扫捕集方法参数。校正曲线的线性关系良好，相关系数大于0.999，方法检出限为0.3 μg/kg。采用该方法测定农田、公路两侧、加油站附近等3种不同类型的土壤样品并进行了加标回收实验，回收率范围为81.5%~108%。     

吹扫捕集气质联用法同时测定水中氯乙烯、乙醛、丙烯醛、丙烯腈、吡啶和松节油

建立了一种采用吹扫捕集气质联用法同时测定水中氯乙烯、乙醛、丙烯醛、丙烯腈、吡啶和松节油的分析方法,研究并优化了吹扫捕集前处理条件参数。结果表明,吹扫时间、吹扫温度和脱附时间是影响目标物的吹扫捕集效率的关键因素;优化后方法线性良好,相关系数均大于0.999,检出限范围为0.20~1.48μg/L,加标回收率范围为86.9%~105%,相对标准偏差为1.1%~9.8%。建立的吹扫捕集GC-MS联用法简便、快速、灵敏度高、定性定量准确可靠,可同时满足对自来水、地表水、地下水等水样中痕量氯乙烯、乙醛、丙烯醛、丙烯腈、吡啶和松节油监测的要求。     

大气痕量有机硫化物的光电离色谱法测定及硫酸铵在湿浸土壤中释放有机硫化物的研究

采用国产光电离色谱仪(GC-PID)对有机硫化物:乙基硫醇,二甲基硫,二甲基二硫进行了分离分析,其最小检知量在亚微克/升级,并对北京郊区的某些天然源环境样品进行了有机硫化物浓度的测定,实验数据证实,在鸡场,猪场,水稻田与塑料蔬菜大棚等环境大气中含有机硫化物。研究了硫酸铵作为氮肥加入到水浸土壤中后,由于缺氧而生成有机硫化物的现象,观察了其对有机硫化物的释放规律及硫酸铵与葡萄糖分别作为硫源与碳源对有机硫化物生成的影响,实验结果认为:硫酸铵在五种不同类型的水浸土壤中(环境温度25℃),均可解离释放出有机硫化物,随其在土壤中加入量的增多,释放气中的有机硫浓度增加,二甲基硫的释放量最大。     

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.     

High Resolution GC - MS Analysis of VOCs in Wastewater and Sludge

High resolution gas chromatography - mass spectrometry (GC-MS) has been widely used in the field of environmental sample analysis for volatile organic compounds (VOCs) (Gryder-Boutet, et al., 1988). Such a technique was applied to the analysis of VOCs at a local municipal wastewater treatment plant. The combination of purge and trap sample preparation and thermal desorption with cryofocusing technology, allows for the detection of a wide range of volatiles in wastewater and sludge samples. Results show that a large variety of organics present in samples are aliphatic and aromatic hydrocarbons. Their concentrations are in part per billion levels between 10 to 150 g/L. Others identified using this method are chlorinated hydrocarbons, sulfides and organic acids. By comparing the chromatograms of different wastewater and sludge samples collected from various treatment process units, it can be seen that most volatiles were removed or degraded after the aeration or digestion process. Information that provides an insight to the measurement of organic compounds in sludges is also discussed in this paper.     

Patterns and levels of halogenated volatile compounds in Portuguese surface waters

The present study focused on monitoring the concentration of 14 halogenated volatile organic compounds in surface waters, including sea, estuarine, river water and industrial effluents in order to determine the most ubiquitous compounds and their concentration levels, which were used to establish their geographical and temporal distribution. EPA Method 502, based on purge and trap techniques, was used. In this method volatile organic pollutants are extracted (purged) from the water sample by bubbling inert gas through the aqueous sample. Purged sample components are trapped in a cartridge containing the polymeric sorbent Tenax and, thereafter, the cartridge is heated and backflushed with helium to desorb the trapped sample components directly into a gas chromatograph with electron capture detector (GC-ECD). The linearity range of the method varied from 0.1 to 4 microg L(-1) with a limit of detection at the low microg L(-1) level. The present study consisted of a monthly monitoring of 46 points throughout Portugal, during 14 months. Chloroform was found in 50% of the samples analyzed, its presence being correlated to both agricultural and industrial activities. Other compounds detected were tetrachloroethylene, trichloroethylene, carbon tetrachloride and 1,2,4 trichlorobenzene, which were present in 10-20% of the samples at concentrations up to 18 microg L(-1). 1,1,2,2-Tetrachloroethane and its degradation product 1,1,2-trichloroethane were found in 5% of the samples, the levels of the latter being higher than those of the parent compound in most samples. Sporadic high concentrations of some volatile halogenated organic compounds were attributed to local uses as solvents.     

吹扫捕集-气质联用法测定水中9种酯类物质

采用吹扫捕集-气相色谱／质谱联用法测定水中9种酯类有机物，加入硫酸钠盐提高灵敏度，当硫酸钠过饱和时，吹扫捕集效率最高。9种酯类有机物在一定的质量浓度范围内线性关系良好，方法检出限为0．14μg／L～0．25μg／L，模拟样品平行测定的RSD为0．6％～1．8％，加标回收率为80％～106％。     

高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素

建立高浓度有机废水中5种喹诺酮类抗生素的高效液相色谱-串联质谱测定方法。水样经HLB固相萃取小柱富集净化,12 ml甲醇洗脱、浓缩并加入内标溶液后,定容至1 mL待测。以C18柱为分离柱,含0.01%甲酸的甲醇-含0.01%甲酸的水溶液为流动相,目标物质在10 min内分离。在0.25~1 250 ng/mL范围内,目标物质线性关系良好(R20.99)。基质加标试验结果表明,纯水中的回收率为61.40%~91.92%,废水中的回收率为54.92%~101.87%,检出限为0.25~2.5 ng/L,方法定量限为0.36~3.99 ng/L。应用该方法对21家猪场的64份废水样品进行分析,5种喹诺酮类抗生素的检出频率为47%~95%,平均检出浓度为980~5 734 ng/L。该方法快速、准确,适用于高浓度有机废水中喹诺酮类抗生素的同时测定。     

Comprehensive screening and priority ranking of volatile organic compounds in Daliao River,China

An analytical strategy for comprehensive screening of target and non-target volatile organic compounds (VOCs) in surface water was developed, and it was applied to the analysis of VOCs in water samples from Daliao River. The target VOCs were quantified using purge and trap-gas chromatography-mass spectrometry (P&T-GC/MS). Among 20 water samples, 34 VOCs were detected at least once. For the screening of non-target VOCs, the double distillation apparatus was used for the pre-concentration of VOCs prior to P&T-GC/MS analysis. Subsequently, deconvolution software and NIST mass spectral library were applied for the identification of the non-target compounds. A total of 17 non-target VOCs were identified. The most frequently detected VOCs (detection frequencies >80 %) included toluene, benzene, naphthalene, 1,2-dichloroethane, 1,1,2-trichloroethane, and methyl tert-butyl ether. The distribution of VOCs obviously varied according to the sampling sites. The total concentrations of VOCs in water samples collected from the heavily industrialized cities (Anshan and Liaoyang) and the busy port city (Yingkou) were relatively high. The top ten priority VOCs, including naphthalene, 1,2-dichloroethane, o-xylene, 1,3-dichlorobenzene, tetrachloroethene, 1,2-dichlorobenzene, 1,2,4-trichlorobenzene, ethylbenzene, m-xylene, and p-xylene, were obtained by the ranking of the detected VOCs according to their occurrence and ecological effects. These compounds should be given more attention in monitoring and drainage control strategies.     

气相色谱/质谱联用法测定环境空气中恶臭类硫化物

采用冷阱预浓缩-气相色谱/质谱联用法测定环境空气中硫化氢、甲硫醇、甲硫醚、二硫化碳、二甲二硫、噻吩等6种硫化物,讨论了采样容器材质的影响。方法线性良好,6种硫化物的检出限为1.0μg/m3～5.0μg/m3,混合标准气平行测定的RSD≤8.1%,加标回收率为93.5%～97.3%。     

吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯

采用吹扫捕集-气相色谱/质谱联用法测定地表水中氯丁二烯。当进样体积为20 mL时,方法在0.100μg/L~50.0μg/L范围内线性良好,检出限为0.05μg/L,标准溶液平行测定的RSD≤3.7%,地表水样加标回收率为91.0%~101%,方法可用于地表水中卤代烃、苯系物等其他21种挥发性有机物的同时测定。     

吹扫—捕集／气相色谱法测定水中挥发性有机物

为提高样品分析效率，研究并建立了吹扫-捕集／气相色谱／氢火焰检测器联用同时测定水中1，2-二氯乙烷、苯、甲苯、氯苯、乙苯、对-二甲苯、间-二甲苯、苯乙烯、邻-二甲苯、异丙苯、1，4-二氯苯、1，2-二氯苯、硝基苯、1，3，5-三氯苯、1，2，4-三氯苯、1，2，3-三氯苯、六氯丁二烯17种挥发性有机物的分析方法。结果表明，当进样体积为25．0ml时，最低检出限为0．0034-0．1088μg/L，相对标准偏差为1．8％～6．4％，加标平均回收率为97．6％-105．8％。该方法可快速、简便、准确、高灵敏度的测定水中17种挥发性有机物，并适用于饮用水和地表水中挥发性有机物的测定。