以NCLA9K4活性碳作為VOC濃縮介質與熱脫附方法之改良

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陳彥呈(Yan-cheng Chen) 查詢紙本館藏

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化學學系

論文名稱

以NCLA9K4活性碳作為VOC濃縮介質與熱脫附方法之改良
(Activated charcoal NCLA9K4 as VOC condensed medium and improvment of thermal desorption method)

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摘要(中)

揮發性有機化合物(volatile organic compound, VOC)，本身為空氣中之汙染物，也是臭氧以及二級有機氣溶膠之前驅物。臭氧、VOC以及有機氣溶膠濃度的上升會造成人們健康的危害。因此對於大氣中VOC的組成有事先的瞭解，將有助於掌握臭氧的形成機構。然而在全範圍的VOC分析中，對於高揮發性的物種量測在現今的技術中仍具相當挑戰。
本次研究中運用一多孔洞新材料活性碳NCLA9K4搭配自製不須冷劑補給之熱脫附裝置，將對大氣中之VOC具好的吸附能力且定量良好。值得注意的是VOC中含豐富的乙烷、乙烯、丙烷、丙烯等皆是容易破出之物質。NCLA9K4具微孔的特質(孔徑範圍在0.5 nm ~ 30 nm，平均孔徑1.85 nm)且高比表面積(~3500m2g-1)具良好的VOC吸附特性，並與孔徑材料MCM-48與商品化多重床碳吸附劑進行吸附比較。
透過皮爾特晶片的降溫，先將捕捉管之吸附溫度降至-10以及-30℃進行測試，最後針對皮爾特晶片之散熱部分，改用更高效能散熱模組，而能將溫度降至-40℃，利用降溫的輔助提高材料在高揮發性物種的捕捉。
利用A9K4搭配Carbosieve SIII所組合之二重床，發現在-40℃下能將C2以及C3物種捕捉效果良好，線性達0.999以上，C2~C11的RSD皆小於3%，偵測極限都在數百個pptv以下。

摘要(英)

Ambient volatile organic compounds (VOCs) are air pollutants, and also act as precursors of ozone and secondary organic aerosol (SOA). Elevated VOCs, ozone, and fine aerosol levels cause adverse effects on human health.
Knowing the composition of ambient VOCs is the prerequisite of understanding ozone formation and thus its containment strategy. However, the full-range analysis of ambient VOCs in the field is technically challenging, particularly for the more volatile compounds. In this study, a new porous material - activated charcoal NCLA9K4 - will be studied to quantitative enrich ambient level VOCs by a self-built cryogen-free thermal desorption device.
Special attention is given to the enrichment efficiency of the most volatile compounds, namely ethane, ethylene, propane, and propylene, since they are more easily to breakthrough. NCLA9K4, which has micropores (pore range = 0.5 nm ~ 30 nm, average pore size = 1.8 nm) and high specific surface area (3500 m2s-1), was compared with MCM-48 and commercial multi-carbon sorbents for their VOC enrichment capability.
Test of trapping was first performed by cooling the sorbent trap at -10 and -30℃. Further improvement in the Peltier cooling using a better heat-sink allowed a lower temperature of -40℃and; thus, better trapping efficiency for high boiling compounds.
The combination of using A9K4 and Carbosieve III to form a dual-sorbent bed and cooling at -40℃ was able to quantitatively analyze ambient C2-C3 compounds with R2 close to 0.999, RSD better than 3%, and detection limit at sub-ppbv level.

關鍵字(中)

★ 致冷晶片
★ 活性碳
★ 有機揮發性氣體

關鍵字(英)

★ VOC
★ peltier cooler
★ activated charcoal

論文目次

中文摘要.............................................................................................................I
英文摘要............................................................................................................II
謝誌..................................................................................................................IV
目錄..................................................................................................................VI
圖目錄..............................................................................................................IX
表目錄.......................................................................................................... XIII
第一章、前言....................................................................................................1
1-1 VOC之來源.................................................................................................1
1-2 VOC的為害.................................................................................................4
1-3 光化測站與監測網.....................................................................................5
1-4 VOC之分析方法.......................................................................................10
1-5 前濃縮方法...............................................................................................13
第二章、文獻回顧............................................................................................19
2-1 活性碳吸附劑...........................................................................................20
2-2 石墨碳黑吸附劑.......................................................................................21
2-3 多孔聚合物吸附劑...................................................................................22
2-4 碳分子篩吸附劑.......................................................................................23
2-5 中孔洞矽分子篩.......................................................................................24
2-6 活性碳NCLA9K4.....................................................................................30
2-6-1 水熱碳化法............................................................................................30
2-6-2 合成配方................................................................................................32
2-6-3 表面形貌觀察........................................................................................34
2-7 實驗動機...................................................................................................36
第三章、實驗原理及分析方法......................................................................37
3-1 前濃縮儀裝置...........................................................................................37
3-1-1 捕捉管改良與製作................................................................................38
3-1-2 致冷裝置設計........................................................................................40
3-1-3 致冷裝置改良........................................................................................43
3-1-4 致冷裝置再改良....................................................................................45
3-1-5 自動化程序控制....................................................................................46
3-2 實驗架構與流程.......................................................................................47
3-3 層析系統架構...........................................................................................51
3-3-1 層析管柱原理........................................................................................51
3-3-2 Heart-cut 原理........................................................................................52
3-4 偵測器.......................................................................................................56
3-5 除水裝置...................................................................................................57
3-6 標準氣體...................................................................................................58
第四章、結果與討論........................................................................................60
4-1 常溫下不同材料間比較...........................................................................60
4-2 負溫捕捉探討...........................................................................................64
4-2-1 A9K4在-10℃捕捉探討.........................................................................64
4-2-2 A9K4在-30℃捕捉探討.........................................................................67
4-2-3 A9K4搭配Carbosieve SIII於-30℃捕捉表現.......................................70
4-2-4 -40℃低溫下材料吸附比較...................................................................72
4-3 儀器偵測極限(LOD)................................................................................80
4-4 結論...........................................................................................................83
第五章、參考資料..........................................................................................84
圖目錄
圖1-1 NOx與VOC經光化反應形成O3與HNO3之二次汙染物示意圖.........5
圖1-2 1998年美國光化學評估監測站的分布.................................................6
圖1-3 我國2010年光化學評估監測站分布圖，其中包括兩個移動測站......8
圖1-4 自1999到2009年之全台臭氧月平均圖...............................................8
圖1-5 全球VOC監測網...................................................................................9
圖1-6 大氣中VOC量測方法分類.................................................................12
圖1-7 皮爾特晶片實圖，可依需求使用不同尺寸的晶片.............................17
圖1-8 降溫晶片示意圖...................................................................................17
圖2-1 活性碳表面結構示意圖.......................................................................20
圖2-2 poly(p-2,6-diphenylphenyleneoxide)結構圖.........................................23
圖2-3 矽酸及鋁酸四面體結構.......................................................................26
圖2-4 MCM-41之可能合成機制，(1)形成液晶化，(2)矽酸化.......................26
圖2-5 M41S系列示意圖.................................................................................26
圖2-6在250℃脫附溫度下，MCM-41與碳分子篩多重床
(multi-carbon: Carboxen 1003 + Carboxen 1000 + Carbotrap)之單位
碳感度比較..........................................................................................27
圖2-7 MCM-41與碳分子篩多重床對混合VOC C7-C12脫附溫度圖...........28
圖2-8 不同溫度下MCM-48對於VOC捕捉之層析圖，圖譜分為
PLOT(C2~C6)以及DB-1(C6~C12)呈現，(a)、(c)捕捉溫度30℃；(b)、
(d)捕捉溫度-20℃................................................................................29
圖2-9 (a) 5 μm解析度SEM圖；(b)高效能電子穿透顯微圖，掃描模式2 nm
..............................................................................................................31
圖2-10 推測硬碳球形成機制，A：為兩性結構形成；B：微胞形成；C：
堆疊成核............................................................................................31
圖2-10 (a) 不鏽鋼外罐； (b) 鐵氟龍內罐....................................................32
圖2-11 (a)尺標50 μm，粒子團聚大小1~25 μm； (b)尺標10 μm，單一粒
子大小~200 nm....................................................................................35
圖2-12 水熱產物活化前後SEM圖。(a)活化前的表面形貌；(b)活化後所得活性碳的表面形貌...................................................................................35
圖3-1 濃縮系統關鍵步驟(a)降溫捕捉；(b)高溫脫附...................................38
圖3-2 早期電阻式加熱裝置，捕捉管以不鏽鋼管為主，捕捉管中間焊有感
溫線來偵測捕捉管之溫度..................................................................39
圖3-3 以玻璃管填充之多重床吸附管...........................................................40
圖3-4 (a) Peltier致冷晶片實圖；(b)加熱線圈實圖........................................41
圖3-5致冷裝置示意圖：(a)透視圖(b)側視圖.................................................42
圖3-6致冷裝置示意圖(a)設計圖；(b)、(c)裝置實照圖..................................44
圖3-7 (a)散熱器實圖；(b) 改良之致冷裝置測試圖......................................45
圖3-8 自動化控制程序聯結示意圖...............................................................46
圖3-9 前濃縮系統示意圖，SSR為固態繼電器(solid state relay)；P-535為
溫度程序控制器；MFC質量流量控制器(mass flow control)............49
圖3-10 閥件切換狀態(a)預備狀態；(b)樣品捕捉；(c)進樣；(d)管路淨化，
pump為一負壓系統，透過MFC控制進樣的流量；STD表示56
種 VOC 混合氣體............................................................................50
圖3-11 Heart-Cut原理示意圖，DB-1無法分析良好之輕碳部分(C2~C5)切入
(a) PLOT管柱將輕碳分離；(b)重碳分離良好部分切入空管直接帶
出........................................................................................................53
圖3-12 層析系統Deans switch裝置..............................................................54
圖3-13 火焰離子偵測器(FID)結構圖...........................................................56
圖3-14 Nafion dryer示意圖............................................................................57
圖4-1 A9K4空白分析圖譜，(a)PLOT管柱層析圖譜；(b)DB-1管柱層析圖
譜..........................................................................................................62
圖4-2 (a)三合一多重床與(b)A9K4在30℃下對C2~C5的捕捉效果比較.....63
圖4-3 (a)三合一組合多重床與(b)A9K4在30℃下對C6~C12的捕捉效果比
較..........................................................................................................63
圖4-4 (a)三合一與(b)A9K4在-10℃捕捉下，於PLOT管柱之層析效果......65
圖4-5 (a)三合一與(b)A9K4在-10℃捕捉下，於DB-1管柱之層析效果.......66
圖4-6 吸附材料於-10℃捕捉之再現性(N=3)...............................................66
圖4-7 A9K4在-30℃下的層析效果(a)PLOT管柱層析圖；(b)DB-1管柱層
析圖，虛線部分為C2的層析峰............................................................67
圖4-8 A9K4於-30℃捕捉VOC之線性..........................................................68
圖4-9 A9K4 + Carbosieve III於-30℃捕捉之層析圖譜，(a)C2~C6在PLOT
管柱層析圖；(b)C6~C12在DB-1管柱層析圖......................................70
圖4-10多重床吸附劑之線性比較，(a)~(f)為A9K4+Carbosieve SIII；(g)~(l)
為三合一材料....................................................................................72
圖4-11 -40℃低溫下捕捉層析圖，(a)、(b)為C2~C5層析圖；(c)、(d)為C6~C12
層析圖，(a)、(c)為三合一材料；(b)、(d)為A9K4+Carbosieve SIII......74
圖4-12 -40℃下捕捉VOC線性比較，(a)~(m)為A9K4+Carbosieve III；(n)~(z)
為三合一材料......................................................................................77
圖4-13 吸附材料穩定性比較.........................................................................78
圖4-14 不同溫度下材料捕捉穩定性.............................................................78
圖4-15 校正曲線圖，斜率值m表校正靈敏度..............................................79
圖4-16 2010年1月至2011年5月各光化測站所測乙烯濃度值，取當月量
測濃度之最高值................................................................................82
圖4-17 吸附材料與降溫輔助捕捉VOC之整理...........................................84
表目錄
表1-1 估計全球VOC的排放(百萬噸/年).......................................................3
表1-2 美國標準方法(TO)與我國標準方法(NIEA)比較..............................15
表1-3 晶片致冷捕捉運用於即時量測之論文回顧.......................................18
表2-1 Tenax結構特性..................................................................................23
表3-1 氣流參數設定，Aux1用於將捕捉之VOC送至DB-1層析管柱；
Aux2用於切割樣品，將C2~C5送至PLOT管柱，C6~C12送至空
管..........................................................................................................55
表3-2 GC運作溫度時序.................................................................................55
表3-3 鋼瓶56種VOC標準氣體....................................................................59
表4-1 材料特性，Carboxen 1000、Carboxen 1003、Carbotrap組合成多重
床..........................................................................................................62
表4-2常溫下不同孔徑材料對於VOC吸附範圍比較...................................64
表4-3 吸附材料特性.......................................................................................69
表4-4 A9K4+Carbosieve SIII於-40℃捕捉下之偵測極限(σ = 3).................80

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59. www.sigmaaldrich.com/cataglog/ProductDetail.do

指導教授

王家麟(Jia-lin Wang)

審核日期

2011-7-26

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