【摘要】：印染行業(yè)是國民經(jīng)濟重要支柱產(chǎn)業(yè)之一,行業(yè)所需的原料——染料是工業(yè)和生活中必不可少的原材料。染料的種類繁多,其中一些染料中含有對環(huán)境和人體有害的物質,許多國家和相關組織對這些染料的使用作出嚴格的限制。部分分散染料和酸性染料對人體有致敏作用,能引起人體皮膚、黏膜或呼吸道過敏,有的還具有致癌性、致突變等毒性作用。生產(chǎn)排放的染料類污染物通過印染廢水積聚到印染污泥中,往往成為很難處理的一類污染物。染料中的有害成分通過污泥的循環(huán)利用轉移到環(huán)境中,使得人體和動植物的健康受到潛在的威脅。因此,對于印染污泥中染料類污染物的檢測顯得尤為重要,但是印染污泥成分復雜,要分析其中的染料類污染物存在相當大的難度,所以選擇符合要求的樣品前處理方法和檢測方法很關鍵。基質固相分散(Matrix Solid-Phase Dispersion,MSPD)技術操作快速簡便,所需溶劑和樣品量少,特別適合于粘性樣品(例如生物組織)、固體、半固體的處理。MSPD技術自發(fā)明以來,其與GC-MS、HPLC-MS等相結合,在環(huán)境、醫(yī)藥衛(wèi)生、食品等方面得到了廣泛的應用。本文將MSPD技術應用于萃取污泥樣品中的染料類污染物,提取液進入高效液相色譜-質譜聯(lián)用(HPLC-MS/MS)檢測,進行研究。本文主要有以下幾點:1.介紹了染料類污染物的基本情況、常用于污泥樣品的前處理方法及各自特點,著重說明基質固相分散萃取技術在各類樣品中的應用。2.建立了基質固相分散-高效液相色譜-串聯(lián)質譜法測定印染污泥中三種分散染料(分散藍35、分散紅1、分散橙37)的分析方法。優(yōu)化了萃取劑的選擇及用量、洗脫劑的選擇及用量、研磨條件、凈化劑條件等萃取效果的影響因素。三種分散染料在最優(yōu)條件下,2～100μg/kg范圍內線性關系良好(r20.998),檢出限為0.01～0.14μg/kg。相對標準偏差2.9%～8.2%,加標回收率86.4%～106.4%,能滿足印染污泥中痕量分散染料的同時檢測。3.對MSPD萃取方法進行再次的試驗,仍運用基質固相分散-高效液相色譜-串聯(lián)質譜法測定印染污泥中四種酸性染料(酸性紅1、酸性紅87、酸性橙7和酸性藍83)。四種酸性染料在最優(yōu)條件下在5～100μg/kg范圍內線性關系良好(r20.996),檢出限為0.19～0.75μg/kg。加標回收率在81.7%～103.1%之間,相對標準偏差在1.3%～8.9%之間,能夠同時滿足污泥中酸性染料類污染物的分析測定。4.最后對實驗進行總結,基質固相分散萃取設備簡單,成本低廉,所需時間短,將其應用于污泥這種基質中的樣品提取,發(fā)展?jié)摿α己谩?br/>[Abstract]:Printing and dyeing industry is one of the important pillar industries of national economy. There are many kinds of dyes, some of which contain harmful substances to the environment and human body. Many countries and related organizations impose strict restrictions on the use of these dyes. Some disperse dyes and acid dyes can sensitize human body and cause skin, mucosal or respiratory allergies. Some of them have carcinogenic and mutagenic effects. The dye pollutants discharged from production are accumulated into the printing and dyeing sludge through printing and dyeing wastewater, which often become a class of pollutants that are difficult to deal with. The harmful components of dyes are transferred to the environment through the recycling of sludge, which makes the health of human body, animal and plant under potential threat. Therefore, the detection of dye pollutants in printing and dyeing sludge is particularly important, but the composition of printing and dyeing sludge is very complex, so it is very difficult to analyze the dye pollutants in printing and dyeing sludge. Therefore, it is very important to select sample pretreatment and detection methods that meet the requirements. Matrix solid dispersion (Matrix Solid-Phase Dispersion,MSPD) is a rapid and simple technique with less solvent and sample quantity. It is especially suitable for the treatment of viscous samples (such as biological tissue), solids and semisolids. Since the invention of MSPD technology, it has been combined with GC-MS,. HPLC-MS has been widely used in environment, medicine, food and so on. In this paper, MSPD technique was applied to extract dye pollutants from sludge samples, and the extract was detected by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). This paper has the following main points: 1. This paper introduces the basic situation of dye pollutants, the pretreatment methods and their characteristics of sludge samples, and emphatically explains the application of matrix solid phase dispersion extraction technology in all kinds of samples. 2. A method for the determination of three disperse dyes (disperse blue 35, disperse red 1, disperse orange 37) in printing and dyeing sludge by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry was established. The factors affecting the extraction effect were optimized, such as the selection and dosage of extractant, the selection and dosage of eluent, the grinding condition and the condition of purifying agent. Under the optimum conditions, the linear relationship between the three disperse dyes was good in the range of 100 渭 g/kg (r20.998), and the detection limit was 0.01 渭 g / kg. The relative standard deviation of 2.9and 8.2and the recovery rate of 86.4and 106.4can meet the requirement of simultaneous determination of trace disperse dyes in printing and dyeing sludge. The extraction method of MSPD was tested again, and four kinds of acid dyes (acid red 1, acid red 87, acid orange 7 and acid blue 83) in printing and dyeing sludge were determined by matrix solid-phase dispersion-high performance liquid chromatography-tandem mass spectrometry. The linear range of the four acid dyes is 5 渭 g/kg (r20.996), and the detection limit is 0.19 ~ 0.75 渭 g / kg 路kg ~ (-1) 路min ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1) ~ (-1). The recovery rate was between 81.7% and 103.1%, and the relative standard deviation was between 1.3% and 8.9%. Finally, the experimental results show that the matrix solid phase dispersion extraction equipment is simple, low cost and short time. It has a good development potential when it is applied to the sample extraction of sludge.
【學位授予單位】：蘇州科技學院
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：X832;O657.63

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本文編號：2349635