【摘要】：近年來,�；沸孤兜氖鹿蕰r有發(fā)生,及時的環(huán)境監(jiān)測對環(huán)境保護和人類的健康非常重要。苯胺作為常見的一種�；�,泄漏后易對周圍環(huán)境造成危害,影響生物體健康。因此,本研究旨在找出一種能夠快速、靈敏檢測水中苯胺的分析方法。本研究建立了頂空-氣相色譜/質(zhì)譜法和分光光度法測定苯胺的方法,并對拉曼法測定苯胺進行了探討。利用頂空-氣相色譜/質(zhì)譜聯(lián)用技術(shù)研究水環(huán)境中苯胺,討論了色譜柱種類、柱溫、分流比、平衡溫度、平衡時間等因素對測定結(jié)果的影響。在優(yōu)化的實驗條件下,做出了苯胺的標(biāo)準(zhǔn)工作曲線(線性回歸方程為y=31.865x+5.4729,相關(guān)系數(shù)r2=0.9993,線性范圍是10～1000μg/L。苯胺的最低檢出限為4.3μg/L。測定環(huán)境中的兩種實際水樣時苯胺的回收率為96.99%～99.98%、89.28%～97.97%。結(jié)果表明,頂空-氣相色譜/質(zhì)譜法適合測定泄漏到水環(huán)境中的苯胺。用分光光度法測定水中的苯胺時,利用苯胺產(chǎn)生的重氮化合物與顯色劑反應(yīng),其顯色物在450 nm處具有最大吸收波長。對重氮化反應(yīng)的時間、各物料加入量、pH以及顯色時間進行了實驗討論,得出了最佳的實驗條件,并在最佳條件下做出了苯胺的標(biāo)準(zhǔn)工作曲線(線性回歸方程為y=0.1338x+0.0008,r2=0.9994,線性范圍是0～10mg/L)。苯胺的最低檢出限是13.5μg/L。測定環(huán)境中的兩種實際水樣時苯胺的回收率為96.46%～101.53%、95.13%～99.33%,且水樣本底值與頂空-氣相色譜質(zhì)譜法得出的結(jié)果相吻合。從分析成本和方法學(xué)的角度比較了頂空-氣相色譜質(zhì)譜法和分光光度法。成本上:從儀器成本和時間成本來看,分光光度法更加容易實現(xiàn)快速檢測的目的,從處理手段的便捷化來看,頂空-氣相色譜/質(zhì)譜法卻更勝一籌。方法學(xué)上:兩種方法的相關(guān)系數(shù)、精密度都在化學(xué)分析的正常范疇內(nèi),其中頂空-氣相色譜質(zhì)譜法較分光光度法的最低檢出限更加低一些,更加適合測定水中痕量的苯胺。
[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.
【學(xué)位授予單位】：大連海事大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X832

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