污染土壤中二苯醚类残留物质的检测方法研究

发布时间：2018-04-23 03:09

  本文选题：前处理方法 + 二苯醚类　； 参考：《苏州科技学院》2015年硕士论文

【摘要】：有机物对土壤的污染已经得到了人们的普遍关注,许多化工厂在搬迁之后留下了污染严重的土地,这些地区的土壤无法再次投入农耕,也已经不能作为居住用地,导致大量的土地荒废。所以对于这些土壤中污染物质的含量测定与分析可以及时让人们了解土壤的污染状况,从而提出相应的解决方案。土壤样品的分析测定一般要经过前处理之后,才能利用测定仪器如气相色谱仪、液相色谱仪等进行上机分析。其中,前处理的过程普遍耗时较长,误差较大,对于整个样品处理过程的影响最大,也是制约当今分析方法发展的主要因素。本文将针对某化工厂污染土壤中的二苯醚类物质的残留进行前处理方法的研究,主要包括以下几个方面:(1)建立了一种简单便捷的处理土壤中二苯醚类物质残留的的前处理方法。实验对比研究了超声萃取、索式提取以及加速溶剂萃取3种前处理方法的实验条件,最终建立了体积比V(正己烷):V(二氯甲烷)=1:1为提取剂的ASE法提取,气相色谱质谱法(GC-MS)测定的方法。在添加浓度为50μg/kg、200μg/kg下,空白土壤的加标回收率为81%~106%,相对标准偏差在5.8%~10.4%,方法检出限为5.3μg/kg~11.5μg/kg,可以满足对残留分析的要求。(2)为了对污染土壤中二苯醚类物质的处理方法进行研究,对比了单独ASE与ASE-分散液相微萃取法的效果,采用ASE-分散液相微萃取-GC-MS的方法分析测定土壤中二苯醚类物质残留。研究用丙酮溶剂在140℃下对土壤样品进行ASE萃取,萃取液氮吹至1mL后加入40μL四氯化碳和纯水形成乳浊液,静置2min离心,吸取1μL底部有机相,气相色谱质谱法测定。结果表明5种二苯醚类物质在添加浓度为10μg/kg、50μg/kg、200μg/kg下的加标回收率达到83.5%~103.3%,相对标准偏差为4.2%~8.8%之间,方法检出限在0.43~14.83μg/kg。(3)在前文前处理方法研究的基础上,探讨了结合提取与净化为一体的分散固相萃取法处理土壤中二苯醚类残留物质的方法,讨论了吸附剂对目标物质的影响。(4)总结并对土壤中二苯醚类物质的前处理方法进行展望。
[Abstract]:The contamination of soil by organic matter has received widespread concern. Many chemical plants have left heavily polluted land after their relocation, and the soil in these areas cannot be reinvested in farming and can no longer be used as a living land. Resulting in a great deal of wasteland. Therefore, the determination and analysis of the contaminants in these soils can help people to understand the pollution situation in time and put forward the corresponding solutions. The analysis and determination of soil samples usually have to go through pretreatment before they can be analyzed by means of measuring instruments such as gas chromatograph liquid chromatograph and so on. Among them, the process of pretreatment generally takes longer time and larger error, which has the greatest influence on the whole process of sample treatment, and is also the main factor that restricts the development of analytical methods nowadays. In this paper, the pretreatment method of diphenyl ether residues in contaminated soil of a chemical plant is studied, including the following aspects: 1) A simple and convenient pretreatment method is established for the treatment of diphenyl ether residues in soil. The experimental conditions of ultrasonic extraction, cable extraction and accelerated solvent extraction were compared and studied. Finally, the ASE method with volume ratio V (n-hexane 1: 1) was established. Gas chromatography-mass spectrometry (GC-MS). At a concentration of 50 渭 g / kg ~ (2) 渭 g/kg, the standard recovery of blank soil was 81 ~ 106 and the relative standard deviation was 5.8 ~ 10.4. The detection limit of the method was 5.3 渭 g/kg~11.5 ~ (2) 渭 g 路kg ~ (-1), which could satisfy the requirement of residue analysis.) in order to study the treatment of diphenyl ether in contaminated soil, The effects of ASE and ASE- disperse liquid phase microextraction were compared, and the residual diphenyl ethers in soil were determined by GC-MS with ASE- dispersive liquid phase microextraction. Soil samples were extracted by ASE at 140 鈩，

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