博碩士論文 103223019 詳細資訊




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姓名 陳宥璇(Yu-Hsuan Chen)  查詢紙本館藏   畢業系所 化學學系
論文名稱 利用基質固相分散萃取法檢測室內灰塵中的短鏈氯化石蠟
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摘要(中) 短鏈氯化石蠟 (Short chain chlorinated paraffins, SCCPs) 由碳數為10-13的直鏈多氯化烷烴 (Polychlorinated alkanes, PCAs) 所組成,含氯量在30-72%之間。短鏈氯化石蠟自從1930年以來,因其具有價格低廉、揮發性低、絕緣性和阻燃性良好的特性,多用於金屬切削液 (Metal cutting fluid)、橡膠的阻燃劑 (Flame retardant) 以及油漆與紡織品中的阻燃劑和塑化劑 (Plasticizer) 等。短鏈氯化石蠟具有持久性、生物累積性及透過大氣進行遠距離遷移的能力,斯德哥爾摩公約 (Stockholm convention) 目前也擬將短鏈氯化石蠟增列為優先控制之持久性有機物染物 (Persistent organic pollutants, POPs)。因此開發一套簡單且穩固的方法來檢測環境中的短鏈氯化石蠟是非常重要的。
本研究使用基質固相分散萃取法 (Matrix solid-phase dispersion, MSPD) 作為樣品前處理方法,並搭配氣相層析電子捕捉負離子質譜儀 (GC/ECNI-MS),快速且有效檢測灰塵中的短鏈氯化石蠟。
基質固相分散萃取法最佳化條件為取0.1 g灰塵與0.1 g的矽膠置於震盪器中均勻混合,再將其置入含有3.0 g酸性矽膠 (44% H2SO4) 、2.0 g鹼性矽膠 (33% NaOH) 及2.0 g中性矽膠 (3% H2O) 的玻璃管柱中,並依序使用7 mL正己烷及7 mL正己烷:二氯甲烷= 2:1 (v:v) 進行沖提 (不收集),接著加入5 mL正己烷:二氯甲烷= 2:1 進行沖提並收集,將萃取液旋濃乾燥,再以內標準品回溶至10 μL,取1 μL進樣GC/ECNI-MS進行檢測分析。偵測極限為0.2 μg/g;Inter-days及Intra-day的測試所得相對標準偏差 (RSDs) 皆小於5 %,顯示本方法具有良好的穩定性與再現性。在國內室內灰塵中所測得的短鏈氯化石蠟濃度為1.2至31 μg/g。
摘要(英) Short chain chlorinated paraffins (SCCPs) are complex mixtures of polychlorinated n-alkanes with carbon chain lengths from 10 to 13 and a chlorination degree between 30% and 72% by weight. Because of their low price, low volatility, good insulation and flame resistance properties, SCCPs have been used for metal cutting fluids, plasticisers and flame retardants since 1930. SCCPs are persistent, bioaccumulation and potential for long-range transport. Owing to that, they were under reviewed by the Stockholm Convention on Persistent Organic Pollutants. Therefore, it is important to develop a simple and robust method to monitor SCCPs in the environment.
In this study, vortex-homogenization matrix solid-phase dispersant (VHMSPD) coupled with gas chromatography electron capture negative ion mass spectrometry (GC/ECNI-MS) was developed and used to determine SCCPs in indoor dust samples. The optimized procedure of VHMSPD were 0.1 g dust dispersing with 0.1 g silica gel by a vigorous shaking to obtain a homogenous mixture. The mixture was transferred to a glass column packing with 3.0 g acidic silica gel (44% H2SO4) plus 2.0 g basic silica gel (33% NaOH) and 2.0 g of silica (3% H2O) gel, then the target analytes were eluted with last 5 mL of the mixture of n-hexane and dichloromethane (2:1, v:v). After rotary evaporation to dryness, the residue was redissolved in 10 μL of acetone containing internal standard and 1 μL sample was injected into GC/ECNI-MS for analysis.
The limit of detection (LOD) for SCCPs in indoor dust samples were determined to be 0.2 μg/g. The relative standard deviations (RSDs) of inter-days and intraday tests were lower than 5%, and the SCCPs levels in indoor dust samples ranged from 1.2 to 31 μg/g.
關鍵字(中) ★ 短鏈氯化石蠟
★ 基質固相分散萃取法
★ 氣相層析電子捕捉負離子質譜儀
關鍵字(英) ★ SCCPs
★ MSPD
★ GC/ECNI/MS
論文目次 摘要 I
Abstract III
謝誌 V
目錄 VI
圖目錄 X
表目錄 XII

第一章 前言 1
1-1研究緣起 1
1-2研究目標 3

第二章 文獻回顧 5
2-1室內灰塵 5
2-2氯化石蠟 7
2-2-1 性質 7
2-2-2 毒性研究 9
2-2-3 產量與規範 10
2-2-4 用途 11
2-2-5 環境影響 12
2-3 國內外相關研究 15
2-4 氣相層析質譜儀 23
2-4-1 四級矩質譜儀 25
2-4-2 電子捕捉負離子游離法 27
2-4-3 選擇離子偵測模式 29
2-5 基質固相分散萃取法 30
2-5-1 前言 30
2-5-2 原理 31
2-5-3萃取流程 32
2-5-4 影響因素 34
2-6 線性回歸 36
2-6-1 Mandel Test 36
2-6-2 The lack-of-fit test by ANOVA 38
2-7 基質效應 40

第三章 實驗步驟與樣品分析 43
3-1實驗藥品與設備 43
3-1-1 實驗藥品 43
3-1-2 儀器設備 45
3-2 實驗步驟 47
3-2-1 標準品配製 47
3-2-2 氣相層析質譜儀的參數設定 48
3-2-3 空白灰塵的前處理 50
3-2-4 樣品添加的步驟 50
3-2-5基質固相分散萃取法實驗步驟 51
3-3 灰塵採集 53

第四章 結果與討論 55
4-1 氣相層析質譜儀對短鏈氯化石蠟的測定 55
4-1-1 短鏈氯化石蠟的分析 55
4-1-2 短鏈氯化石蠟的定性與定量 59
4-1-3 檢量線與偵測極限 59
4-2 震盪 (Vortex) 與研磨的比較 61
4-3 基質固相分散萃取法之最佳化探討 62
4-3-1 分散劑種類探討 63
4-3-2 吸附劑種類探討 64
4-3-3 萃取溶劑種類探討 65
4-3-4 分散劑添加量探討 66
4-3-5 酸性矽膠添加量探討 67
4-3-6 中性與鹼性矽膠添加量探討 68
4-3-7 萃取溶劑比例探討 69
4-3-8 萃取溶劑體積探討 70
4-3-9 基質固相分散萃取法之最佳化結果 72
4-4 線性方程式的適用性 73
4-4-1 Mandel Test 73
4-4-2 The lack-of-fit test by ANOVA 74
4-5 真實樣品的檢測 75
4-5-1 室內灰塵樣品檢測結果 75
4-5-2 檢測結果比較 86
4-5-3 基質效應 88
4-5-4 方法的精密度及準確性 89

第五章 結論 91

第六章 參考文獻 93

附錄 111
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指導教授 丁望賢(Wang-Hsien Ding) 審核日期 2016-6-20
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