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采用吹扫捕集、毛细管气相色谱法和选择性检测器分析水中有机化合物的十亿分比水平。

Analysis of ppb levels of organics in water by means of purge-and-trap, capillary gas chromatography and selective detectors.

作者信息

Duffy M, Driscoll J N, Pappas S, Sanford W

机构信息

HNU Systems Inc., Newton, MA 02161.

出版信息

J Chromatogr. 1988 May 27;441(1):73-80. doi: 10.1016/s0021-9673(01)84655-0.

Abstract

The Environmental Protection Agency (EPA) has issued a series of methods (500 and 600 series) for the analysis of organics in drinking water and industrial discharges. Methods 601 and 602 employ packed-column gas chromatography (GC) with electrolytic conductivity (E1CD) and photoionization detection (PID), respectively. A purge-and-trap system is used for concentration of volatiles. The EPA is in the process of converting methods 601 and 602 and certain 500-series methods to capillary column analysis. We have also initiated the conversion of a number of these methods, using E1CD and PID and have described them in detail in this paper. We have evaluated both 0.32- and 0.53-mm diameter capillary columns, using helium and nitrogen as carrier gases with each detector. We found that with nitrogen optimum results are obtained at a flow-rate of 15 ml/min, and with helium at 6-8 ml/min. As a result of system optimization, including operation of the two detectors in series, and converting from packed to capillary columns, we found that analysis time could be reduced from 80 min (for two methods separately) to ca. 30 min. In addition, the elution of more than five components in one peak, observed when the packed column specified in method 601 are used, was eliminated.

摘要

美国环境保护局(EPA)发布了一系列用于分析饮用水和工业排放物中有机物的方法(500系列和600系列)。方法601和602分别采用填充柱气相色谱法(GC),配备电解电导检测器(ELCD)和光离子化检测器(PID)。吹扫捕集系统用于浓缩挥发性物质。EPA正在将方法601和602以及某些500系列方法转换为毛细管柱分析。我们也已开始对其中一些方法进行转换,采用ELCD和PID,并在本文中进行了详细描述。我们使用氦气和氮气作为每种检测器的载气,评估了直径为0.32毫米和0.53毫米的毛细管柱。我们发现,使用氮气时,流速为15毫升/分钟可获得最佳结果,使用氦气时,流速为6至8毫升/分钟可获得最佳结果。通过系统优化,包括串联操作两个检测器以及从填充柱转换为毛细管柱,我们发现分析时间可以从80分钟(分别针对两种方法)减少到约30分钟。此外,使用方法601中规定的填充柱时观察到的一个峰中洗脱超过五种成分的情况也消除了。

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