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采用气相色谱法和气相色谱-质谱联用法分析有机水污染物。

The analysis of organic water pollutants by gas chromatography and gas chromatography-mass spectrometry.

作者信息

Hites R A

出版信息

Adv Chromatogr. 1977;15:69-112.

PMID:14483
Abstract

Four methods for the analysis of trace levels or organic compounds in water have been discussed: direct aqueous injection, vapor stripping, solvent extraction, and lipophilic adsorption. Table 6 presents a comparison of these techniques. Direct injection is applicable to compounds having a wide range of polarities and volatilities, but it is not a very sensitive technique. For applications in which low sensitivity is acceptable, direct injection offers a very rapid and potentially accurate means of measuring organics in water. Vapor stripping is a factor of 10(6) more sensitive than direct injection, but this is achieved at the expense of simplicity. This method is applicable to compounds of volatilities less than that of eicosane. A subtle operational problem with most vapor stripping techniques is that the contents of the trap are consumed with one analysis; if anything goes awry, the analysis of that trapped sample cannot be repeated. Solvent extraction has a respectable sensitivity (about 0.5 ppb) and operationally it is very simple. Furthermore, aliquots of the resulting extract can be analyzed many times with different techniques if necessary. Because of the evaporation step, very volatile compounds (greater than that of decane) cannot be measured effectively with solvent extraction. The introduction of a solvent into the water carries with it the potential for contamination. Thus, ultrapure solvents must be used and all glassware should be carefully cleaned [96]. Lipophilic adsorption has the unique property of sampling many hundreds of liters of water. Thus, the method is quite sensitive (potentially in the ppt range) and, in addition, it can provide several milligrams of an isolated component. This latter feature is of considerable advantage if one wants to complement GC-MS analyses with infrared or NMR for difficult structural identifications. As a solvent extraction, the evaporation of the final solvent limits the applicability of adsorption methods to compounds with volatilities greater than that of decane. Finally, the importance of avoiding contamination should be emphasized. Many of the compounds encountered in environmental samples are also common laboratory artifacts, for example plasticizers and antioxidants. When one finds such compounds in a water sample, it is absolutely essential to demonstrate that they are indeed present in the water and are not the result of laboratory contamination. The best such demonstration is procedural blank analyses that are indeed blank.

摘要

本文讨论了分析水中痕量有机化合物的四种方法

直接水相进样、气相吹扫、溶剂萃取和亲脂吸附。表6对这些技术进行了比较。直接进样适用于极性和挥发性范围较广的化合物,但它不是一种非常灵敏的技术。对于灵敏度要求不高的应用,直接进样提供了一种非常快速且可能准确的测量水中有机物的方法。气相吹扫比直接进样灵敏10(6)倍,但这是以牺牲方法的简单性为代价的。该方法适用于挥发性低于二十烷的化合物。大多数气相吹扫技术存在一个微妙的操作问题,即捕集阱中的物质在一次分析中就会被消耗掉;如果出现任何问题,就无法重复对该捕集样品进行分析。溶剂萃取具有可观的灵敏度(约0.5 ppb),并且操作非常简单。此外,如果需要,所得萃取液的等分试样可以用不同技术进行多次分析。由于存在蒸发步骤,挥发性很强的化合物(高于癸烷)无法用溶剂萃取有效地测量。将溶剂引入水中会带来污染的可能性。因此,必须使用超纯溶剂,并且所有玻璃器皿都应仔细清洗[96]。亲脂吸附具有采集数百升水样的独特性质。因此,该方法相当灵敏(潜在可达ppt范围),此外,它可以提供几毫克的分离组分。如果想用红外或核磁共振对难以进行结构鉴定的化合物补充气相色谱 - 质谱分析,后一个特点具有相当大的优势。与溶剂萃取一样,最终溶剂的蒸发限制了吸附方法对挥发性高于癸烷的化合物的适用性。最后,应强调避免污染的重要性。环境样品中遇到的许多化合物也是常见的实验室污染物,例如增塑剂和抗氧化剂。当在水样中发现此类化合物时,绝对有必要证明它们确实存在于水中,而不是实验室污染的结果。最好的证明是进行确实空白的程序空白分析。

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