本文選題：(?)量二級胺 + 氣相色譜�。� 參考：《中南林業(yè)科技大學》2012年碩士論文

【摘要】：二級胺是一類低沸點、易揮發(fā)、易轉化生成強致癌物質的有機胺類化合物,對于生態(tài)環(huán)境和人體健康都有很大的影響。快速、準確地檢測痕量二級胺的分析方法對于保護環(huán)境和人類健康至關重要。本文以二甲胺、甲乙胺、二乙胺、嗎啉和N-甲基芐胺物質代表物質為例,建立了使用氣相色譜-氫火焰檢測器和氣相色譜-質譜檢測器來測定飲用水源中痕量二級胺的方法,對保護環(huán)境和保障人體健康具有重要意義。 使用苯磺酰氯衍生的方法,將二級胺與苯磺酰氯反應生成性質穩(wěn)定的磺酰胺,通過氣相色譜法測定磺酰胺的含量,間接測定二級胺的含量。并對影響衍生反應的溫度、pH和攪拌時間等條件進行優(yōu)化,探索出最適合衍生反應的前處理條件。 使用優(yōu)化后的條件進行衍生反應,再經氣相色譜-氫火焰檢測器(GC-FID)分析水環(huán)境中二級胺含量,色譜柱HP-5型毛細管柱(30m×0.32mm×0.25μ m)；進樣口溫度：280℃；檢測器溫度：300℃；進樣量：1μL；進樣模式：分流進樣；分流比：1：1；載氣為氮氣,柱流量2mL/min,分流出口吹掃流量為3mL/min,柱前壓力為79kPa；氫氣和空氣流量分別為45、450mL/min,升溫程序：初始溫度為120℃,保持3分鐘；以5℃/min的速率從120℃上升至220℃,然后以10℃/分鐘的速率從220℃上升至290℃,保持5分鐘。結果表明：五種二級胺線性關系良好,相關系數為0.9997、0.9996、0.9996、0.9989、0.9995,相對標準偏差分別為0.46%、0.45%、0.38%、0.24%、0.16%,回收率為91%-133%。 使用優(yōu)化后的條件進行衍生反應,經過氣相色譜-質譜檢測器(GC-MS)分析水環(huán)境中的二級胺含量,使用DB-5MS型毛細管柱(30m×0.32mm×0.25μ m)；柱前壓力為80kPa；氮氣純度99.99%,氮氣流速1ml/min,MS檢測器電離電壓為70eV。升溫程序：初始溫度為140℃,以3℃/min的速率從140℃上升至210℃,然后以10℃/分鐘的速率從210℃上升至290℃,保持5分鐘。質譜檢測采用離子選擇模式(SIM),選擇離子為77,141,185。結果表明：五種二級胺線性關系良好,相關系數為0.9987、0.9977、0.9969、0.9956、0.9969,相對標準偏差分別為0.34%、0.43%、0.46%、0.41%、0.19%,回收率為74%-136%。 通過對線性關系、精密度、檢出限和準確度等方法學比較,使用GC-FID比GC-MS在以上指標中有有好的表現(xiàn),同時,GC-FID所需要的運行、維護成本較GC-MS也要低,更適合快速、準確測定飲用水源中二級胺的含量。 使用GC-FID對某地飲用水源進行檢測,使用主成分分析法對當地的二級胺污染狀況進行評價,結果表明：少數地區(qū)檢測出二甲胺、二乙胺,部分地區(qū)檢測出甲乙胺、嗎啉,大部分地區(qū)檢測出N-甲基芐胺,說明該地飲用水源已受到輕微污染。
[Abstract]:Two class amine is a kind of low boiling point, volatile and easily converted to produce strong carcinogen organic amines. It has a great influence on the ecological environment and human health. Rapid, accurate detection of trace amounts of two levels of amines is essential for the protection of the environment and human health. This article is two methylamine, methylamine, two ethylamine, morpholine and N- a. A method for the determination of trace amounts of two grade amine in drinking water source by gas chromatography hydrogen flame detector and gas chromatography-mass spectrometry is established, which is of great significance in protecting the environment and protecting human health by using gas chromatography hydrogen flame detector and gas chromatography mass spectrometry detector.
Using benzsulfonyl chloride, two grade amines are reacted with benzsulfonyl chloride to produce sulfonamide with stable properties. The content of sulfonamide is determined by gas chromatography and the content of two grade amine is indirectly determined. The conditions of temperature, pH and stirring time which affect the derivative reaction are optimized, and the best preconditioning conditions for the derivative reaction are explored.
Using the optimized conditions to derive the reaction, then the gas chromatography hydrogen flame detector (GC-FID) was used to analyze the content of two grade amine in the water environment, the HP-5 capillary column of the column (30M x 0.32mm x 0.25 mu m), the inlet temperature of 280, the detector temperature, 300, 1 Mu L, the sampling mode, the diversion pattern, the shunt ratio: 1:1; The gas carrying capacity is nitrogen, the flow rate of the column flow is 2mL/min, the flow discharge flow is 3mL/min, the pre column pressure is 79kPa, and the hydrogen and air flow are 45450mL/min respectively. The initial temperature is 120 centigrade, keeping 3 minutes; at the rate of /min of 5 degrees C, it rises from 120 to 220, and then rises from 220 to 290 C at 10 C / min, keeping 5 points. The results show that the linear relationship between five kinds of two grade amines is good, the correlation coefficient is 0.9997,0.9996,0.9996,0.9989,0.9995, the relative standard deviation is 0.46%, 0.45%, 0.38%, 0.24%, 0.16%, and the recovery rate is 91%-133%.
Based on the optimized conditions, the two grade amine content in water environment was analyzed by gas chromatography-mass spectrometry (GC-MS), DB-5MS capillary column (30M x 0.32mm x 0.25 mu m), pre column pressure was 80kPa, nitrogen purity was 99.99%, nitrogen flow rate 1ml/min, MS detector ionization voltage was 70eV. heating program: initial temperature was 14. At 0 C, the rate of 3 C /min rose from 140 to 210, and then increased from 210 to 290 C at 10 C / min for 5 minutes. The ion selection mode (SIM) was used for mass spectrometry. The selection ion was 77141185., and the linear relationship of five two amines was good, the correlation coefficient was 0.9987,0.9977,0.9969,0.9956,0.9969, relative standard. The deviations were 0.34%, 0.43%, 0.46%, 0.41%, 0.19%, respectively, and the recovery rate was 74%-136%.
By comparing the linear relation, the precision, the detection limit and the accuracy, the GC-FID is better than the GC-MS in the above indexes. At the same time, the operation and maintenance cost of GC-FID are lower than that of GC-MS. It is more suitable for rapid and accurate determination of the content of two grade amine in the drinking water source.
GC-FID was used to test a drinking water source in a certain area. The status of two grade amine pollution was evaluated by principal component analysis. The results showed that two methylamine, two ethylamine were detected in a few areas, methylamine and morpholine were detected in some areas, and N- methyl benzylamine was detected in most areas, indicating that the drinking water source had been slightly polluted.

【學位授予單位】：中南林業(yè)科技大學
【學位級別】：碩士
【學位授予年份】：2012
【分類號】：R123.1

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