影响气相色谱保留时间的因素及解决方法

保留时间是气相色谱 (ＧＣ)定性的重要依据。在实际工作中发现 ,保留时间具有变异性 ,主要表现为 :来回波动、漂移和突然改变。1　保留时间来回波动在配有自动进样器和工作站的ＧＣ系统中 ,通过重复进样观察组分的保留时间 ,发现样品的保留时间在某一范围内左右波动 ,而且经排序后相邻值的差大都为 0 0 0 3ｍｉｎ(见表 1 )。这是由计算机的数据采集频率决定的。计算机在一个信号运行过程中无法确定比一个数据采集间隔更精确的保留时间 ,当操作者将数据采集频率设置为 5Ｈｚ时 ,数据采集间隔约为 0 0 0 3ｍｉｎ。降低数据采集频率虽可缩短…     

吹扫捕集／气相色谱-质谱联用测定水中26种挥发性有机物

建立了吹扫-捕集与气相色谱-质谱（GC-MS）联用测定水中卤代烃、氯苯类化合物和苯系物等挥发性有机物（VOCs）的方法．采用吹扫-捕集法对水中的VOCs进行富集,热解吸后导入GC-MS分离各组分并用选择离子检测（SIM）进行测定,一次进样可同时对水中26种VOCs进行准确定性和定量．VOCs的线性相关系数为0．9974（0．9999,平均加标回收率为92．3％（96．5％,相对标准偏差为1．35％（5．18％（n=6）,方法检出限为0．001（0．05g／L）．     

吹扫捕集气相色谱质谱法测定土壤中挥发性有机物

建立了吹扫捕集气相色谱质谱法同时测定土壤中卤代烃类、苯系物类、氯代苯类等二十多种挥发性有机物.使用模拟土壤和实际土壤样品优化了吹扫时间、吹扫温度等参数;采用内标法绘制了校正曲线,各目标化合物5个浓度水平的响应因子的相对标准偏差均小于20%,相关系数均大于0.999;测定了方法检出限,采用2g土壤,各目标化合物方法检出限界于0.02～1.00μg/kg;对两种总有机碳含量的实际土壤样品进行了加标回收实验,回收率范围64%～123%.     

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。     

吹扫捕集-气相色谱/质谱法同时测定水中的27种挥发性有机物

水中的VOCs经吹扫富集、解吸后,用HP-VOC色谱柱分离,采用全扫描和选择离子监测模式分析,内标法定量。最佳富集条件为:吹扫流速为40 m L/min,吹扫温度为40℃,吹扫时间为15 min,解吸温度为200℃,解吸时间为2 min。该法27种VOCs在一定的质量浓度范围内与其峰面积呈线性关系,相关系数r0.995,检出限为0.02~1.18μg/L。以空白样品为基体进行加标回收试验,测得回收率为79.8%~114%,相对标准偏差为0.3%~12%。     

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。     

预冷浓缩系统与气相色谱——质谱法测定室内空气中挥发性有机物

针对室内空气挥发性有机物测定方法的不足,本文采用预冷浓缩系统和气相色谱,质谱联用。建立了测定室内空气中39种挥发性有机物的分析方法,该方法采用苏码罐采样,经液氮预冷冻浓缩后,用心城由检测。该方法灵敏度高,操作简便、重现性好、准确度高,适用于室内空气中挥发性有机物的测定。     

预浓缩系统-全二维气相色谱-飞行时间质谱分析环境空气中挥发性有机物

采用SummA罐采集样品,自动进样器进样,三级冷阱预浓缩样品,全二维气相色谱／飞行时间质谱法（GC×GC／TOFMS）测试分析,以较长的非极性柱Rxi-5MS（60m×320μm×1．0μm）作为第一维柱,较短的中等极性柱DB-17MS（2．0×0．1mm×0．1μm）作为第二维柱,对环境空气中的VOC成分进行了定性定量分析。通过考察方法的线性范围、精密度、加标回收率、检出限与《空气和废气监测分析方法》（四版）给出的两个方法比较,证实该方法特性不仅满足方法学要求,而且能够更加准确快速监测环境空气中VOC。     

气相色谱法同时测定空气中六种挥发性有机物

借气相色谱电子捕获检测器检测、ＴｅｎａｘＧＣ富集柱富集、Ｐｏｒａｐａｋ－ＰＳ填充柱分离,同时测定空气中二氯甲烷、二硫化碳、,方法简便快速,变异系数小于１４％,加标回收率８７％－９９％,方法检出限０．３－１６μｇ／ｍ＾３。     

毛细管气相色谱法同时测定水中的7种挥发性卤代烃

用毛细管气相色谱法同时测定饮用水中7种挥发性卤代烃的研究．实验表明，该方法前处理简单，测定方便，具有较好的灵敏度、准确度和精密度，结果令人满意．样品的加标回收率在90％～110％，相对标准偏差小于5％．     

A dual channel gas chromatograph for atmospheric analysis of volatile organic compounds including oxygenated and monoterpene compounds

A dual channel gas chromatograph with flame ionisation detectors has been used extensively for analysis of volatile organic compounds in the atmosphere and forms the basis of two monitoring instruments contributing VOC data to the World Meteorological Organisation - Global Atmosphere Watch network. Recent modifications to the methodology have broadened the scope of the instrument; to incorporate measurements of selected monoterpenes, and achieve improved accuracy in the measurement of oxygenated volatile organic compounds. Analysis of selected monoterpenes has been achieved without any significant loss of resolution of the non-methane hydrocarbons or oxygenated compounds. Quantification of 64 different VOCs of varying functionalities are reported with detection limits in the range 1-5 parts per trillion. Here we present a summary of the instrumental and calibration details for the methodology, which continues to be used on many field projects, along with a discussion of the associated measurement uncertainties.     

光离子化检测器便携式气相色谱仪快速测定空气中苯系物

本文研究了使用光离子化检测器便携式气相色谱仪,直接测定空气中ｍｇ／ｍ３级苯系物（苯、甲苯、乙苯、邻、间、对位的二甲苯及异丙苯）的快速分析方法。方法的线性范围为０～１００ｍｇ／ｍ３,相关系数均在０．９９９以上,方法的变异系数分别为２．９～１２．５％（５ｍｇ／ｍ３）,３．４～７．９％（３０ｍｇ／ｍ３）,方法最低检测限达０．２～１．０ｍｇ／ｍ３。     

Determination of volatile organic compounds pollution sources in malaysian drinking water using multivariate analysis

A field investigation was conducted at all water treatment plants throughout 11 states and Federal Territory in Peninsular Malaysia. The sampling points in this study include treatment plant operation, service reservoir outlet and auxiliary outlet point at the water pipelines. Analysis was performed by solid phase micro-extraction technique with a 100 μm polydimethylsiloxane fibre using gas chromatography with mass spectrometry detection to analyse 54 volatile organic compounds (VOCs) of different chemical families in drinking water. The concentration of VOCs ranged from undetectable to 230.2 μg/l. Among all of the VOCs species, chloroform has the highest concentration and was detected in all drinking water samples. Average concentrations of total trihalomethanes (THMs) were almost similar among all states which were in the range of 28.4--33.0 μg/l. Apart from THMs, other abundant compounds detected were cis and trans-1,2-dichloroethylene, trichloroethylene, 1,2-dibromoethane, benzene, toluene, ethylbenzene, chlorobenzene, 1,4-dichlorobenzene and 1,2-dichloro - benzene. Principal component analysis (PCA) with the aid of varimax rotation, and parallel factor analysis (PARAFAC) method were used to statistically verify the correlation between VOCs and the source of pollution. The multivariate analysis pointed out that the maintenance of auxiliary pipelines in the distribution systems is vital as it can become significant point source pollution to Malaysian drinking water.     

吹扫捕集与气相色谱-质谱联用测定饮用水和地表水中挥发性有机污染物

报道了Trap I(VOCARB 4000)柱捕集水中挥发性有机污染物的性能和条件,建立了吹扫捕集和气相色谱-质谱联用测定饮用水和地表水样中25种挥发性有机污染物的分析方法.水样的加标回收率在90%～110%之间,最低检测限在0.04～0.85μg/L之间,20μg/L的挥发性有机物标准溶液经重复6次测定,其相对标准偏差基本小于5.0%.该方法已成功地运用于饮用水和地表水中挥发性有机污染物的测定,结果令人满意.     

Investigation and assessment of volatile organic compounds in water sources in China

456 water samples collected from 152 water sources in 2006 were analyzed for 21 volatile organic compounds (VOCs). Concentrations of 21 VOCs ranged from below method detection limits of the laboratory to 7.65 ??g/L (toluene), but seldom exceeded the concentration limits set in the National Drinking Water Quality Standards (GB5749-2006) or the National Environmental Quality Standards for Surface Water (GB3838-2002) of China. Of the 21 individual VOCs analyzed, 11 VOCs were detected in at least one sample at or above 1.0 ??g/L; 6.6% of the water samples had a detection of at least one VOC at or above 1.0 ??g/L, and 2.6% had a detection of at least two VOCs at or above 1.0 ??g/L. Based on the statistical data of detection frequencies above the method detection limits, 75% of the samples detected at least one VOC, and 65% of the samples detected at least two VOCs. Chloroform, toluene, and 1,2-dichloroethene were the three most frequently detected VOCs, with detection frequencies of 76.97%, 68.42%, and 44.08%, respectively. Volatile halogenated hydrocarbons and gasoline components were the two most frequently detected VOC groups.     

Determination of organophosphorus pesticides and related compounds in water samples by membrane extraction and gas chromatography

A membrane extraction-gas chromatography method was developed fordetermination of organophosphorus pesticides and related compounds including methamidophos, DDVP, dimethoate, methyl parathion, parathion, thiophosphoric acid trimethyl ester, and thiophosphoramidic acid dimethyl ester in water samples. In thismethod, surface-modified acetic cellulose membranes were used to extract the target analytes in water samples, the extracted analytes were back-extracted into a small amount of methanol, andgas chromatography with pulsed flame photometric detector (GC-PFPD) was used to determine the concentrations of targetanalytes in the extracts. The recoveries obtained for thetarget analytes spiked into the water samples ranged from 66to 94%. The method detection limit for each target analyte was 0.05 g L^-1. The method developed in this study had shown the advantages of being cheap, simple, fast, and reliable. It had been used successfully to determine the concentrations of target analytes in river water samples.     

环境空气中痕量挥发性有机硫监测分析方法研究

采用预浓缩系统与GC MS联用,建立了环境空气中痕量挥发性有机硫的分析方法,该法用苏玛罐或Tedlar袋采集空气样品在预浓缩系统中经液氮于-160℃冷冻浓缩后,进入GC MS进行分析。甲硫醇、乙硫醇、甲硫醚、乙硫醚、二甲二硫的最低检出限分别为2 0、1 0、1 0、1 0、0 5μg m3。经6次的重复测定,其相对标准偏差小于9 0%。该方法已用于环境空气的测定,取得了令人满意的结果。     

毛细管气相色谱法快速测定化妆品中4种对羟基苯甲酸酯防腐剂

用乙醇萃取了化妆品中的4种防腐剂(对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯),用毛细管气相色谱法实现了快速分离测定,并用色谱-气相质谱联用技术进行了峰鉴定。分析时间为4min,方法回收率为90 8%～104 6%,检出限为0 5mg/L,线性范围为2～80mg/L,线性相关系数>0 999。     

吹扫—捕集/气相色谱法测定水中挥发性卤代烃

建立了吹扫—捕集 /气相色谱 /电子捕获检测器联用测定水中 5种挥发性卤代烃分析方法 ,且按国家水质分析标准方法 (GB/T 1 71 3 0 -1 997)所确定的三氯甲烷、四氯化碳、三氯乙烯、四氯乙烯、三溴甲烷 5种挥发性卤代烃进行实验 ,采用 Supelcoport担体层析柱对去离子水处理 ,所获得的纯水无色谱干扰峰 ,本法按国家水质分析标准方法列出的 5种挥发性卤代烃进行测定在国内尚未见报导。当纯水的进样体积为 5 .0 ml时 ,其最低检出浓度为 1× 1 0 - 2～ 6× 1 0 - 4(μg/L)之间 ;相对误差在 1 .1 %～ 2 .4%之间 ;加标回收率在 82 .5 %～ 1 0 8%之间 ;相关系数在 0 .9980～ 0 .9999之间。可快速、高灵敏度、简便、准确、精密地测定水中 5种挥发性卤代烃 ,本法适用于饮用水和地表水中挥发性卤代烃的测定     

气相色谱法测定地下水中氯化苄

建立了气相色谱法测定地下水中氯化苄的方法。选用ＧＤＸ５０２大孔树脂或Ｃ１８小预处理柱吸附浓缩地下水中氯化苄,用苯洗脱,洗脱液注入色谱仪进行分析。方法回收率为８６４９８１％,变异系数＜８％。