本文選題：揮發(fā)性有機(jī)物 + 標(biāo)準(zhǔn)樣品��； 參考：《北京化工大學(xué)》2016年碩士論文

【摘要】：揮發(fā)性有機(jī)物(Volatile Organic Compounds, VOCs)作為重要的水質(zhì)評(píng)價(jià)指標(biāo)之一,在多項(xiàng)環(huán)境標(biāo)準(zhǔn)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(cè)試數(shù)據(jù)的準(zhǔn)確及可靠成為水質(zhì)分析質(zhì)量控制的難點(diǎn)。標(biāo)準(zhǔn)樣品是環(huán)境監(jiān)測(cè)質(zhì)量控制手段之一,近年來(lái)環(huán)境保護(hù)的壓力和分析方法的更新對(duì)水體VOCs標(biāo)準(zhǔn)樣品的需求不斷提高。目前市售的VOCs標(biāo)準(zhǔn)樣品多來(lái)自國(guó)外,其種類和濃度范圍不能滿足我國(guó)實(shí)際監(jiān)測(cè)的需求。為此,本文研制了一種涵蓋我國(guó)環(huán)境水標(biāo)準(zhǔn)中涉及的29種VOCs混合標(biāo)準(zhǔn)樣品溶液,解決了研制過(guò)程中的關(guān)鍵技術(shù)問(wèn)題,并對(duì)標(biāo)樣的均勻性和穩(wěn)定性進(jìn)行了評(píng)價(jià)。主要研究?jī)?nèi)容如下：1、首先采用氣密注射預(yù)先配制氯乙烯甲醇溶液,然后標(biāo)準(zhǔn)稱量其余組分并混勻,按照標(biāo)準(zhǔn)樣品工作導(dǎo)則將配制好的溶液進(jìn)行灌封、分裝。對(duì)制備好的VOCs混合標(biāo)樣進(jìn)行均勻性檢驗(yàn),F檢驗(yàn)統(tǒng)計(jì)結(jié)果表明均勻性合格。2、對(duì)所制備的VOCs甲醇標(biāo)樣進(jìn)行穩(wěn)定性研究。長(zhǎng)期穩(wěn)定性檢驗(yàn)結(jié)果表明標(biāo)準(zhǔn)樣品可以在-18℃的條件穩(wěn)定保存18個(gè)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(zhǔn)確,因此進(jìn)一步對(duì)其進(jìn)行了短期穩(wěn)定性檢驗(yàn),結(jié)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(biāo)樣在運(yùn)輸過(guò)程中控制低溫環(huán)境；轉(zhuǎn)移至實(shí)驗(yàn)室時(shí),可短期保存于4℃或室溫環(huán)境,并盡快完成測(cè)量以保證結(jié)果的準(zhǔn)確性。3、建立了吹掃捕集-氣質(zhì)聯(lián)用法檢測(cè)水體中VOCs的檢測(cè)條件：吹掃(時(shí)間11 min,流速40 mL/min)-干吹掃時(shí)間1 min-預(yù)脫附(溫度180℃)-吹掃(溫度30℃,時(shí)間11 min)-解吸附(溫度190℃,時(shí)間2 min)-烘烤(時(shí)間8 min,溫度230℃)。將研制的29種VOCs混合標(biāo)樣采用此方法進(jìn)行定值分析,并將數(shù)據(jù)結(jié)果與6家實(shí)驗(yàn)室進(jìn)行統(tǒng)計(jì),依次進(jìn)行Dixon檢驗(yàn)、Grubbs檢驗(yàn)、Cochran檢驗(yàn),剔除離群值,計(jì)算出標(biāo)準(zhǔn)樣品的標(biāo)準(zhǔn)值,并整合配制過(guò)程、均勻性檢驗(yàn)、穩(wěn)定性研究、定值過(guò)程各步的不確定度分量,計(jì)算標(biāo)準(zhǔn)樣品的擴(kuò)展不確定度。4、將建立的檢測(cè)方法應(yīng)用于環(huán)境不同水體中VOCs檢測(cè),用研制的質(zhì)控用29種VOCs標(biāo)準(zhǔn)樣品進(jìn)行加標(biāo)回收試驗(yàn),方法線性良好,加標(biāo)回收率在60%～130%之間,檢測(cè)限達(dá)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(biāo)準(zhǔn)樣品符合實(shí)際水體中VOCs的監(jiān)測(cè)需求,完善了我國(guó)VOCs昆合標(biāo)準(zhǔn)樣品體系,為監(jiān)測(cè)實(shí)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(hào)：1793481