TATB制備廢水中污染物成分的分離分析研究
本文選題:TATB廢水 切入點(diǎn):液相色譜-質(zhì)譜聯(lián)用 出處:《南京理工大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
【摘要】:1,3,5-三氨基-2,4,6-三硝基苯(TATB)是一種高能鈍感炸藥,也是最早的耐熱炸藥之一,廣泛應(yīng)用于軍事民用等各個(gè)領(lǐng)域,其合成過(guò)程中三個(gè)階段產(chǎn)生大量有機(jī)廢水,色譜法是目前應(yīng)用最廣泛的廢水分析方法。本文采用液質(zhì)聯(lián)用(LC-MS)、高效液相色譜(HPLC)、氣相色譜(GC)等色譜儀器對(duì)TATB制備廢水中有機(jī)污染物成分進(jìn)行分析鑒定,采用液液萃取、固相萃取等前處理手段對(duì)廢水進(jìn)行處理得到固體物質(zhì),采用紅外(IR)、核磁(NMR)以及高分辨質(zhì)譜(HRMS)等分析儀器對(duì)其進(jìn)行表征,建立相應(yīng)的分析方法。采用液相色譜-質(zhì)譜聯(lián)用(LC-MS)對(duì)廢水中的難揮發(fā)性物質(zhì)進(jìn)行分析鑒定,結(jié)合線性離子阱-傅里葉變換質(zhì)譜(LTQ-FT-MS)對(duì)組分進(jìn)行定性分析,確定了廢水中熱不穩(wěn)定及難揮發(fā)性組分的成分組成;對(duì)廢水進(jìn)行處理得到固體物質(zhì),采用紅外、核磁以及高分辨質(zhì)譜進(jìn)行表征確定其結(jié)構(gòu),從硝化廢水中得到1,3,5-三羥基-2,4,6-三硝基苯(TNPG)固體,對(duì)胺化廢水進(jìn)行過(guò)柱重結(jié)晶分得到1,3,5-三乙氧基-2,4,6-三硝基苯(TETNB)和1-氨基-3,5-二乙氧基-2,4,6-三硝基苯;采用HPLC對(duì)TATB廢水中4種苯類衍生物進(jìn)行分析,得出了各階段廢水中四種苯類衍生物的含量,建立了 TATB廢水中4種物質(zhì)的HPLC分析方法;采用氣相色譜對(duì)廢水中的乙醇、丙酮、原甲酸三乙酯等小分子物質(zhì)的含量進(jìn)行測(cè)定,得出了各廢水中小分子的含量,建立了相應(yīng)的氣相色譜分析方法,適用于工業(yè)廢水體系中小分子殘留的分析。
[Abstract]:1,3,5- -2,4,6- three amino three nitrobenzene (TATB) is a kind of insensitive high explosives, one of heat-resistant explosives is also one of the earliest and widely used in military and civil fields, a large number of organic wastewater from the three stages of the synthesis process, wastewater chromatography is currently the most widely used analytical method. By using liquid chromatography-mass spectrometry (LC-MS), high performance liquid chromatography (HPLC), gas chromatography (GC) and other chromatographic instruments on the preparation of TATB organic pollutants in wastewater were analyzed and identified, using liquid-liquid extraction, solid phase extraction pretreatment method for processing the solid matter of wastewater, using infrared (IR), nuclear magnetic resonance (NMR) and high resolution mass spectrometry (HRMS) was characterized as analytic instrument, establish corresponding analysis method. By using liquid chromatography-mass spectrometry (LC-MS) were identified in the wastewater to volatile substances, combined with linear ion trap Fourier transform mass spectrometry (LTQ- FT-MS) were divided to group qualitative analysis, composition of wastewater heat labile and difficult volatile ingredients were determined; processing of solid material for wastewater by IR, NMR and high resolution mass spectrometry to determine its structure was characterized by 1,3,5-, -2,4,6- three hydroxy three nitrobenzene from nitrification in wastewater (TNPG) on solid. A column of amination wastewater recrystallization points 1,3,5- triethoxy -2,4,6- three nitrobenzene (TETNB) and 1- -3,5- two amino ethoxy -2,4,6- three nitrobenzene; using HPLC analysis of 4 kinds of benzene derivatives in TATB wastewater, the contents of four kinds of benzene derivatives in various stages of wastewater, set up 4 kinds of material TATB HPLC in the wastewater analysis method; chromatography in the wastewater by gas ethanol, acetone, ethyl formate content of three molecules were determined, the content of the wastewater of small molecules, established the corresponding The analytical method of gas chromatography is suitable for the analysis of small and medium molecular residues in industrial wastewater.
【學(xué)位授予單位】:南京理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:O657.63;X832
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