努尔古丽·拉提莆 宋琪

摘 要：针对工业废水中部分有机类化合物易挥发、难测定的问题，研究提出顶空和气相色谱-质谱法，测定了工业废水中的55种挥发性有机物含量。研究氟苯和1，2-二氯苯-D4为内标物，在顶空平衡温度为65℃、平衡时间为50min时，分别采用全扫描和离子扫描对工业废水中有机类化合物含量进行测定，得到废水中10种挥发性有机物的线性范围在10～300μg/L。当采用全扫描时，其检出限范围0.8～6.8μg/L，加标回收率在81%～116%，相对标准偏差在0.38%～15.25%;当采用离子扫描时，检出限在0.2～1.1μg/L，加标回收率在81%～118%，相对标准偏差在0.38%～7%。

关键词：工业废水;顶空;气相色谱-质谱法;挥发性有机化合物

中图分类号：X703 文献标识码：A     文章编号：1001-5922（2021）10-0029-04

Determination of Organic Compounds in Industrial Wastewater

Nuerguli·Latipu， Song Qi

（China University of Petroleum （Beijing）， Karamay 834000， China ）

Abstract：In view of the problem that some organic compounds in industrial wastewater are easy to volatilize and difficult to determine， headspace and gas chromatography-mass spectrometry （GC-MS） were proposed to determine 55 volatile organic compounds in industrial wastewater. In this paper， fluorobenzene and 1，2-dichlorobenzene-d4 were used as internal standards. When the headspace equilibrium temperature was 65℃ and the equilibrium time was 50 minutes， the contents of organic compounds in industrial wastewater were determined by full scanning and ion scanning respectively. The measurement shows that the linear range of 10 volatile organic compounds in wastewater is between 10μg/L and 300μg/L. When using full scan， the detection limit range is 0.8～6.8μg/L， the recovery of standard addition is between 81%～116%， and the relative standard deviation is between 0.38%～15.25%; when using ion scanning， the detection limit is between 0.2～1.1μg/L， the recovery rate of standard addition is between 81%～118%， and the relative standard deviation is between 0.38%～7%.

Key words：industrial wastewater; headspace; gas chromatography-mass spectrometry; volatile organic compounds

工業废水中存在大量的挥发性有机化合物，这类物质大多数对人体有毒有害，因此中国制定了相关的规定和标准以严格控制含有这类物质的工业废水的排放。目前，测定工业废水中挥发性有机化合物的方法主要是通过吹扫捕集法或固相微萃取法对水中挥发性有化合物进行前处理，然后利用气相色谱-质谱法进行分析。如崔永学、李新伟、崔亮亮等采用吹扫捕集法和气相色谱-质谱联合法对工业基地附近居民内挥发性有机物暴露情况进行了检测与分析[1]。皮立、李玉林、谭亮等，采用顶空固相微萃取-气质联用技术，分析青海省不同产地牦牛肉中挥发性风味成分[2]。虽然吹扫捕集法对工业废水中挥发性有机化合物的富集效率较高，但对于含挥发性有机化合物浓度高的工业废水，该方法容易导致吹扫捕集吸附管吸附过饱和，进而交叉污染连续分析的样品。……