苯胺快速检测方法研究

发布时间：2019-05-08 12:15

【摘要】：近年来,危化品泄露的事故时有发生,及时的环境监测对环境保护和人类的健康非常重要。苯胺作为常见的一种危化品,泄漏后易对周围环境造成危害,影响生物体健康。因此,本研究旨在找出一种能够快速、灵敏检测水中苯胺的分析方法。本研究建立了顶空-气相色谱/质谱法和分光光度法测定苯胺的方法,并对拉曼法测定苯胺进行了探讨。利用顶空-气相色谱/质谱联用技术研究水环境中苯胺,讨论了色谱柱种类、柱温、分流比、平衡温度、平衡时间等因素对测定结果的影响。在优化的实验条件下,做出了苯胺的标准工作曲线(线性回归方程为y=31.865x+5.4729,相关系数r2=0.9993,线性范围是10～1000μg/L。苯胺的最低检出限为4.3μg/L。测定环境中的两种实际水样时苯胺的回收率为96.99%～99.98%、89.28%～97.97%。结果表明,顶空-气相色谱/质谱法适合测定泄漏到水环境中的苯胺。用分光光度法测定水中的苯胺时,利用苯胺产生的重氮化合物与显色剂反应,其显色物在450 nm处具有最大吸收波长。对重氮化反应的时间、各物料加入量、pH以及显色时间进行了实验讨论,得出了最佳的实验条件,并在最佳条件下做出了苯胺的标准工作曲线(线性回归方程为y=0.1338x+0.0008,r2=0.9994,线性范围是0～10mg/L)。苯胺的最低检出限是13.5μg/L。测定环境中的两种实际水样时苯胺的回收率为96.46%～101.53%、95.13%～99.33%,且水样本底值与顶空-气相色谱质谱法得出的结果相吻合。从分析成本和方法学的角度比较了顶空-气相色谱质谱法和分光光度法。成本上:从仪器成本和时间成本来看,分光光度法更加容易实现快速检测的目的,从处理手段的便捷化来看,顶空-气相色谱/质谱法却更胜一筹。方法学上:两种方法的相关系数、精密度都在化学分析的正常范畴内,其中顶空-气相色谱质谱法较分光光度法的最低检出限更加低一些,更加适合测定水中痕量的苯胺。
[Abstract]:In recent years, accidents of leakage of dangerous chemicals occur frequently. Timely environmental monitoring is very important for environmental protection and human health. Aniline, as a common dangerous chemical, is easy to cause harm to the surrounding environment and affect the health of organisms after leakage. Therefore, the purpose of this study is to find a rapid and sensitive analytical method for the determination of aniline in water. A headspace-gas chromatography / mass spectrometry method and spectrophotometric method for the determination of aniline were established, and the Raman method for the determination of aniline was discussed. Headspace-gas chromatography / mass spectrometry was used to study aniline in water environment. The effects of column type, column temperature, shunt ratio, equilibrium temperature, equilibrium time and other factors on the determination results were discussed. Under the optimized experimental conditions, the standard working curve of aniline was obtained. The linear regression equation was ya 31.865 x 5.4729, the correlation coefficient r 2 was 0.9993, and the linear range was 10 ~ 1000 渭 g / L. The minimum detection limit of aniline was 4.3 渭 g / L. The recovery of aniline was 96.99% ~ 99.98% and 89.28% ~ 97.97% respectively. The results show that headspace-gas chromatography / mass spectrometry is suitable for the determination of aniline leaking into water environment. In the determination of aniline in water by spectrophotometry, the diazocompound produced by aniline reacts with the chromogenic agent, and the chromogenic substance has the maximum absorption wavelength at 450 nm. The time of diazotization reaction, the amount of various materials, pH and color time were discussed experimentally. The optimum experimental conditions were obtained, and the standard working curve of aniline was obtained under the optimum conditions (the linear regression equation was y = 0.1338 x 0.0008, P < 0.01). The linear range is 0~10mg/L). The minimum detection limit of aniline is 13.5 渭 g / L. The recoveries of aniline were 96.46% ~ 101.53% and 95.13% ~ 99.33%, respectively. The bottom values of water samples were in good agreement with those obtained by headspace-gas chromatography mass spectrometry (HGC-MS). Headspace-gas chromatography mass spectrometry and spectrophotometry were compared in terms of analytical cost and methodology. Cost: spectrophotometry is easier to achieve rapid detection in terms of instrument cost and time cost, but headspace-gas chromatography / mass spectrometry is superior in terms of ease of processing. In methodology, the correlation coefficient and precision of the two methods are in the normal range of chemical analysis, and the detection limit of headspace-gas chromatography mass spectrometry is lower than that of spectrophotometry, which is more suitable for the determination of trace aniline in water.
【学位授予单位】：大连海事大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X832

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