Main Influencing Factors and Solutions in the Analysis of Volatile Organic Compounds in Water
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摘要: 应用吹扫捕集-气相色谱-质谱法测定水中挥发性有机物，多种因素影响着定量分析的准确性，包括样品瓶的清洗及标准配制、样品和标准溶液的保存、载气气源的纯度、仪器状态检查及参数选择、分离度及积分方式。本文提出在分析过程中样品瓶必须清洗干净，以免污染样品；样品和标准溶液的保存时间过长会降低目标物的回收率；载气和吹扫气会带入杂质；分离度的大小将影响峰高和峰面积测量的准确度。针对分析中氯乙烯的回收、二氯甲烷的交叉污染、浑浊样品的处理等常见问题提供了解决方案，推荐采用选择扫描方式进行分析，并根据样品基体的情况来选择定量离子，将分析的初始温度降至40℃以下并保持2～3 min，以保证氯乙烯的回收率；实验室保持良好的通风环境，避免二氯甲烷交叉污染；色谱柱的最高温度升至220℃以上并保持2～3 min，可以排除萘及分子烷烃的干扰，保证分析的连续性；对于浑浊样品，推荐在野外取样时进行在线过滤或直接采用静态顶空方式进行测定。Abstract: Purge and Trapping-Gas Chromatography-Mass Spectrometry was used to determine volatile organic compounds in water. The accuracy of the quantitative analysis was affected by several factors, including standard preparation, preservation of samples and standard solution, and gas purity during analysis, sample bottles should be kept as clean as possible to avoid pollution. The preservation of samples and standard solution over long time can reduce the recoveries of target compounds. Impurities arise from the carrier gas and sweep gas and the separating degree affects the accuracy of the measurements of peak height and peak area, which consequently affects analysis precision. The solution to this problem is presented in this paper. Selected ion monitoring (SIM)was chosen generally, and a quantitative ion was selected according to the matrix. The initial temperature was dropped to 40℃, and maintained for 2-3 minutes, in order to assure the recovery of vinyl chloride. The laboratory should have a good ventilation environment to avoid cross contamination from methylene chloride. The highest temperature of the chromatographic column was increased to 220℃, and maintained for 2-3 minutes, in order to ensure the continuity of the analysis and eliminate interference from alkanes and naphthalene. For turbidity samples, an on-line filter in the field or using Static Headspace-Gas Chromatography technique directly is recommended.
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Key words:
- water sample /
- volatile organic compounds /
- analysis accuracy /
- influencing factors
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表 1 不同存放时间后标准溶液的回收率
Table 1. The recoveries of standard solutions after different storage time
化合物 回收率/% 1 2 3 4 5 6 氯乙烯 108.3 95.7 88.2 61.7 55.3 66.2 1，1-二氯乙烯 96.8 96.7 78.9 62.1 59.1 83.3 二氯甲烷 105.3 105.5 79.6 73.5 68.7 99.4 1，2-二氯乙烯 104.7 102.8 85.8 82.8 71.0 91.6 1，1-二氯乙烷 107.7 105.3 89.8 83.8 81.6 96.0 氯仿 109.9 104.8 93.9 82.1 76.8 101.5 1，1，1-三氯乙烷 99.4 92.1 89.7 86.2 80.7 86.2 四氯化碳 96.3 95.9 89.5 84.9 78.8 81.2 苯 108.5 96.5 89.1 85.5 80.9 96.6 1，2-二氯乙烷 107.9 104.0 84.4 80.9 75.7 102.5 三氯乙烯 101.6 93.2 87.4 83.2 75.1 91.7 1，2-二氯丙烷 104.0 92.7 82.1 79.8 77.5 95.5 溴二氯甲烷 105.1 92.5 89.2 87.8 77.0 96.8 反-1，3-二氯丙烯 99.4 91.2 89.5 73.3 58.7 91.2 甲苯 100.9 97.2 94.9 88.7 77.2 88.3 顺-1，3-二氯丙烯 101.1 93.3 81.4 74.3 62.7 91.7 1，1，2-三氯乙烷 103.3 91.7 87.8 86.7 77.0 94.2 四氯乙烯 94.5 95.3 85.2 87.2 64.0 83.4 氯二溴甲烷 101.0 96.5 89.3 91.1 76.6 93.0 氯苯 98.7 102.2 87.6 92.2 76.3 88.0 乙苯 100.0 96.7 93.2 92.2 78.4 85.7 间/对二甲苯 99.1 97.2 96.9 92.5 97.1 85.7 邻二甲苯 99.4 95.5 95.1 94.2 79.8 86.8 苯乙烯 99.4 90.5 88.5 80.9 64.4 87.1 溴仿 101.6 94.3 92.6 89.5 71.3 90.2 1，1，2，2-四氯乙烷 109.1 99.5 96.2 94.0 84.3 97.7 间二氯苯 104.6 95.3 96.3 93.1 78.4 88.8 对二氯苯 104.9 95.3 94.4 92.4 76.9 88.8 邻二氯苯 105.1 95.4 96.6 95.1 81.3 90.0 1，2，4-三氯苯 92.9 92.2 90.7 87.8 64.4 79.6 注：回收率1为分装浓标在4个月后测得，回收率2、3、4、5分别为配制于40 mL样品中的6.0 μg/L标准溶液在3天、7天、14天、21天后测得，回收率6为6.0 μg/L样品溶液经过定量滤纸过滤后测得。 
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