本文選題：揮發(fā)性有機物 + 標準樣品��； 參考：《北京化工大學》2016年碩士論文

【摘要】：揮發(fā)性有機物(Volatile Organic Compounds, VOCs)作為重要的水質(zhì)評價指標之一,在多項環(huán)境標準中明確規(guī)定了限值。但是,水體中VOCs的含量少且種類多,因而如何保證水中VOCs測試數(shù)據(jù)的準確及可靠成為水質(zhì)分析質(zhì)量控制的難點。標準樣品是環(huán)境監(jiān)測質(zhì)量控制手段之一,近年來環(huán)境保護的壓力和分析方法的更新對水體VOCs標準樣品的需求不斷提高。目前市售的VOCs標準樣品多來自國外,其種類和濃度范圍不能滿足我國實際監(jiān)測的需求。為此,本文研制了一種涵蓋我國環(huán)境水標準中涉及的29種VOCs混合標準樣品溶液,解決了研制過程中的關鍵技術問題,并對標樣的均勻性和穩(wěn)定性進行了評價。主要研究內(nèi)容如下：1、首先采用氣密注射預先配制氯乙烯甲醇溶液,然后標準稱量其余組分并混勻,按照標準樣品工作導則將配制好的溶液進行灌封、分裝。對制備好的VOCs混合標樣進行均勻性檢驗,F檢驗統(tǒng)計結果表明均勻性合格。2、對所制備的VOCs甲醇標樣進行穩(wěn)定性研究。長期穩(wěn)定性檢驗結果表明標準樣品可以在-18℃的條件穩(wěn)定保存18個月；然而由于在室溫及4℃保存條件下,環(huán)氧氯丙烷易分解影響量值的準確,因此進一步對其進行了短期穩(wěn)定性檢驗,結果表明環(huán)氧氯丙烷的濃度受溫度影響較大,建議該VOCs混合標樣在運輸過程中控制低溫環(huán)境；轉(zhuǎn)移至實驗室時,可短期保存于4℃或室溫環(huán)境,并盡快完成測量以保證結果的準確性。3、建立了吹掃捕集-氣質(zhì)聯(lián)用法檢測水體中VOCs的檢測條件：吹掃(時間11 min,流速40 mL/min)-干吹掃時間1 min-預脫附(溫度180℃)-吹掃(溫度30℃,時間11 min)-解吸附(溫度190℃,時間2 min)-烘烤(時間8 min,溫度230℃)。將研制的29種VOCs混合標樣采用此方法進行定值分析,并將數(shù)據(jù)結果與6家實驗室進行統(tǒng)計,依次進行Dixon檢驗、Grubbs檢驗、Cochran檢驗,剔除離群值,計算出標準樣品的標準值,并整合配制過程、均勻性檢驗、穩(wěn)定性研究、定值過程各步的不確定度分量,計算標準樣品的擴展不確定度。4、將建立的檢測方法應用于環(huán)境不同水體中VOCs檢測,用研制的質(zhì)控用29種VOCs標準樣品進行加標回收試驗,方法線性良好,加標回收率在60%～130%之間,檢測限達到0.04～2.82μg·L-1,精密度在0.7%-7.5%之間。本論文研制的水質(zhì)分析質(zhì)量控制用29種VOCs標準樣品符合實際水體中VOCs的監(jiān)測需求,完善了我國VOCs昆合標準樣品體系,為監(jiān)測實際水體中的VOCs提供了一種質(zhì)量控制手段。
[Abstract]:Volatile Organic components (VOCs), as one of the important water quality evaluation indexes, has specified the limit value in many environmental standards. However, the content of VOCs in water is small and there are many kinds, so how to ensure the accuracy and reliability of VOCs test data in water becomes the difficulty of quality control of water quality analysis. Standard samples are one of the quality control methods for environmental monitoring. In recent years, the pressure of environmental protection and the updating of analytical methods have increased the demand for VOCs standard samples of water body. At present, most of the VOCs standard samples on the market come from abroad, and their types and concentration range can not meet the needs of China's actual monitoring. In this paper, a mixture of 29 kinds of VOCs sample solution which covers the environmental water standard in China is developed. The key technical problems in the process are solved, and the uniformity and stability of the standard sample are evaluated. The main research contents are as follows: firstly, the solution of vinyl chloride was pre-prepared by air-tight injection, then the remaining components of the standard weighing were mixed and mixed, and the prepared solution was sealed and divided according to the work guidelines of the standard sample. The uniformity test of the prepared VOCs mixed standard samples was carried out. The F test results showed that the uniformity was qualified. The stability of the prepared VOCs methanol standard samples was studied. The results of long-term stability test showed that the standard samples could be stably preserved at -18 鈩，

本文編號：1793481