以被動式採樣技術分析空氣中有害揮發性有機化合物

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徐珮瑄(Pei-Hsuan Hsu) 查詢紙本館藏

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化學學系

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以被動式採樣技術分析空氣中有害揮發性有機化合物

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至系統瀏覽論文 (2025-1-1以後開放)

摘要(中)

有害空氣污染物 (Hazardous Air Pollutants, HAPs) 隨著工業發展被大量排放，其中包括若干具毒性之揮發性有機化合物 (Toxic VOCs)。為求取空氣中 Toxic VOCs 平均濃度以評估長時間暴露下之健康風險，美國環保署已公告一標準方法 U.S. EPA Method 325A/B，利用化學吸附劑以氣體擴散原理吸附空氣中 VOCs，再利用不同吸附材料對於不同化合物之吸取速率 (Uptake Rate) 求出在採樣時期間各目標物的平均濃度。在樣品分析上採用自動化熱脫附儀 (Automated Thermal Desorption, ATD) 搭配氣相層析質譜儀 (Gas Chromatography- Mass Spectrometer, GC-MS) 作為分析系統以更簡易的採樣方法長時間監測周界 HAPs 濃度。
首先，本研究之目的是擬將可分析的HAPs物質數目增加，故合併數種不同化學吸附材料之優勢複合成單一採樣管，以達到廣泛應用之目的。研究重點之一是進行複合式材料之條件優化、測試及採樣的應用，其中包含檢量線之相關係數 (R2)、方法偵測極限 (MDL)、精密度 (Accuracy)、準確度 (Precision) 之儲存穩定性(Storage stability)，以達到嚴格的品保品管 (Quality Assurance/Quality Control, QA/QC) 要求，排除未通過 QA/QC 的物種。研究重點之二是利用自製暴露腔在不同溫度、濕度條件下求取個別目標物之專屬吸取速率用於計算周界HAPs濃度。
本研究考量吸附材料的選擇性，在最佳的複合方式下，結果顯示共可針對69項 HAPs 進行被動式採樣，比起單一吸附材料 Carbopack X 與 Carboxen 569 僅可針對50項及37項 HAPs 高出近30項目標物種。複合式材料檢量線相關係數介於0.990~1.000，方法偵測極限濃度介於0.04 ppbv~0.99 ppbv，精密度相對標準偏差介於0.32%~10.43%，準確度之樣品保存回收率介於74.28%~121.61%，而被動式採樣後之採樣管樣品須保存於4℃環境中，並於14天內分析完畢，以確保樣品品質。
在實驗室內進行實驗評估完成後，分別於各化學實驗室(有機、分析、生化實驗室)、台北中研院、桃園觀音工業區及大園工業區、彰化和美國中及埔心高中、雲林崙背國中、高雄仁大工業區等地進行實場採樣。以上採樣方式包含主動式採樣及被動式採樣，而於本研究當中，利用採樣管採樣有以下四種應用，第一：進行被動式採樣用於長時間的環境評估；第二：被動式採樣與線上熱脫附氣相層析質譜法 (Online TD-GC-MS) 或線上熱脫附氣相層析火焰離子偵測器 (Online TD-GC-FID) 進行比較；第三：利用被動式採樣以佈點的方式追朔排放源；第四：平行比對驗證，將被動式採樣與上述之線上GC分析方法置於同一地點平行採樣分析以驗證彼此可靠性。實場測試結果顯示被動式採樣與 online TD-GC-MS 分析方法的平均值接近，獲得極佳之驗證效果。日後監測目的是為了獲取各 Toxic VOCs 的平均濃度，而非瞬間濃度變化，則可以利用實施簡易之被動式採樣法評估相對較長時間之目標物的平均濃度，擴大對於這類有害物質的環境調查能力。

摘要(英)

Hazardous Air Pollutants (HAPs) are emitted in large quantities with industrial development, and the threat to public health has been an issue of great concern in recent years. In the past, the passive sampling technique, similar to the U.S. EPA Method 325A/B, was developed, including the determination of uptake rates for different adsorbent materials for a variety of volatile organic compounds (VOCs) under different climatic conditions.
Firstly, to broaden the range of target compounds, dual commercial adsorbent materials were combined into a tandom adsorbent tube for the complementary benefits and easier deployement and logistics. After excluding the species not passing the QA/QC criteria, the specific experimental uptake rates of the remaining target species were experimentally obtained for calculating concentrations of target compounds after passive sampling. Therefore, another important aspect of this study is to determine the uptake rates with a self-designed exposure chamber under different temperature and humidity conditions. An Automated Thermal Desorption (ATD) with Gas Chromatography-Mass Spectrometer (GC-MS) was used to analze the sorption tubes of passive sampling collected from the field.
The results showed that the composite materials could be used for passive sampling of 69 HAPs, nearly 30 more than the single adsorbent material, e.g., Carbopack X and Carboxen 569, which can only target 50 and 37 HAPs, respectively. The correlation coefficients of the composite materials were between 0.990~1.000, the detection limits were between 0.04 ppbv~0.99 ppbv, the relative standard deviations representing precision were between 0.32%~17.57%, and the recoveries representing accuracy were between 74.28%~121.61%. The samples were stored at 4°C and analyzed within 14 days to ensure the sample and thus data quality.
After thorough preparation, the composite materials were tested in various environments, such as nearby laboratories (organic, analytical, and biochemical laboratories), Academia Sinica, Taoyuan Guanyin Industrial Park. Tayuan Industrial Park, Changhua, and U.S. High School, Puxin High School, Yunlin Lunbei National High School, and Kaohsiung Renda Industrial Park. At some of these sites, both active sampling and passive sampling methods were used. In this study, there are four applications of passive sampling. Firstly, for long-term environmental exposure assessment; secondly, passive sampling with online thermal desorption (TD)-GC-MS or TD-GC with flame ionization detection (FID); thirdly, for emission source investigation; and fourthly, mutual validation with the online TD-GC-MS measurements. Comparing with the online GC method, passive sampling can avoid the complications in operation and maintenance of an instrument in the field. The field tests also revealed comparable results between the two methods when the mean concentrations were compared. As a result, passive sampling can effectively evaluate average concentrations of the target species over a prolonged period at minimal cost and effort, thus adding another useful tool to enhance environmental monitoring capability.

關鍵字(中)

★ 有害空氣污染物
★ 揮發性有機化合物
★ 自動化熱脫附儀
★ 吸取速率
★ 複合式材料

關鍵字(英)

論文目次

目次
摘要 i
Abstract iii
謝誌 v
目次 vii
圖目次 ix
表目次 xii
第一章前言 1
1.1 研究背景 1
1.2 研究目的 5
第二章文獻回顧與整理 7
2.1 有害空氣污染物 7
2.1.1 各國對於HAPs的重視 8
2.1.2 國內對於HAPs的重視 11
2.2 光化學評估監測站 14
2.3 揮發性有機化合物 (VOCs) 的監測 20
2.3.1 離線式採樣分析方法 (Off Line) 23
2.3.2 線上連續式自動監測方法 (On Line) 30
2.4 被動式採樣技術介紹 34
2.4.1 採樣管的介紹 36
2.4.2 擴散吸取速率 (Uptake rate, U) 的介紹 40
2.4.3 採樣管的建置及保存 43
2.4.4 實驗吸取速率之系統裝置 45
2.5 作業健康環境風險 50
第三章實驗設備與流程介紹 53
3.1 實驗儀器介紹 53
3.1.1 適化設備 (Condition Oven) 53
3.1.2 自動熱脫附系統 54
3.2.3 分析儀器 58
3.2 實驗流程 63
3.3 內標準品 (Internal Standard, IS) 65
3.4 標準氣體 (Standard gas) 67
3.5 暴露腔系統 (Exposure Chamber System) 70
3.5.1 溫控設備 70
3.5.2 稀釋系統 71
3.5.3 暴露腔系統 73
第四章實驗方法及條件優化 75
4.1 單一吸附材料 76
4.1.1 Carbopack X 及 Carboxen 569 質量控制標準 76
4.1.2 Carbopack X 及 Carboxen 569 之氣候條件測試 81
4.2 複合式吸附材料配置 85
4.2.1 吸附材料的配方 85
4.2.2 吸附材料的比例 86
4.2.3 重複測試採樣管 88
4.3 自動熱脫附系統參數優化 89
4.3.1 Dry Purge 89
4.3.2 熱脫附 91
4.4 品保品管 (Quality Assurance/Quality Control, QA/QC) 97
4.4.1 質譜儀調整 97
4.4.2 檢量線 (Calibration curve) 98
4.4.3 方法偵測極限 (Method Detection Limit, MDL) 102
4.4.4 精密度 (Accuracy) 105
4.4.5 準確度 (Precision) / 樣品保存 108
4.5 實驗吸取速率 111
4.5.1 計算方法 112
4.5.2 溫度及濕度調整 114
4.6 採樣管之適用性 117
第五章實場採樣及結果討論 119
5.1 實場監測準備 119
5.1.1 主動式採樣 119
5.1.2被動式採樣 120
5.2 監測結果 122
5.2.1 實驗室採樣 122
5.2.2 高雄仁武採樣 125
5.2.3 桃園大園觀音採樣 130
5.2.4 台北中研院採樣 133
5.2.5 彰化和美高中採樣 134
5.2.6 雲林崙背採樣 139
5.2.7 濾紙分析 142
第六章結論 147
參考文獻 151
圖目次
圖1 二次污染物的產生 2
圖2 大氣中主要反應性排放來源 3
圖3 對流層臭氧的生成機制 4
圖4 全臺灣石化及科學工業區分佈 14
圖5 光化學評估監測網設置原則 16
圖6 臺灣光化學評估監測站地理位置 17
圖7 VOCs監測的流程圖 23
圖8 不鏽鋼採樣筒示意圖 25
圖9 NIEA A715.16B標準方法系統圖 26
圖10 TO-15標準方法系統圖 26
圖11 TO-14標準方法系統圖 27
圖12 採樣袋示意圖 27
圖13 TO-18標準方法設備組裝示意圖 28
圖14 不鏽鋼採樣管示意圖 29
圖15 TO-17標準方法系統圖 29
圖16 NIEA A505.12B標準方法系統圖 31
圖17 GC-MS分析系統流路 33
圖18 採樣管剖面示意圖 36
圖19 U.S. EPA Method 325A採樣據點建議設置方法 43
圖20 被動式採樣廠區配置圖 44
圖21 採樣管之黃銅蓋、鐵氟龍蓋與擴散蓋 44
圖22 T.D.Ramos暴露腔體裝置圖 46
圖23 W.A.McClenny暴露腔體裝置圖 46
圖24 PerkinElmer TurboMatrix TC 220 Condition Oven 230 V 54
圖25 PerkinElmer Turbo Matrix 650 Automated Thermal Desorption 55
圖26 PerkinElmer之Air Monitoring Trap 56
圖27 PerkinElmer Clarus 690 GC 59
圖28 升溫梯度 59
圖29 PerkinElmer Clarus SQ 8T 60
圖30 實驗流程 64
圖31 內標準品層析圖譜 66
圖32 標準品圖譜 69
圖33 暴露腔系統示意圖 70
圖34 溫控設備實際圖 (a)上層 (b)下層 71
圖35 (a)MFC控制設備 (b)加濕設備 (c)標準氣體鋼瓶 71
圖36 (a)止逆閥 (b)浮子流量計及針閥 (c)Arduino模組 73
圖37 (a)進氣口 (b)出氣口 (c)Arduino模偵測器 (d)採樣管架 74
圖38 (a) Carbopack X BD 柱狀圖 (b) Carboxen 569 BD 柱狀圖 80
圖39 (a)分層配置 (b)混層配置示意圖 85
圖40 調整複合式材料配置含量之層析圖 86
圖41 調整複合式材料比例之層析圖 87
圖42 調整複合式材料比例之二次脫附層析圖 87
圖43 不同支複合式材料之濃度差 88
圖44 ATD Dry Purge步驟示意圖 89
圖45 Dry Purge流速優化 90
圖46 Dry Purge時間優化 91
圖47 ATD熱脫附步驟示意圖 92
圖48 脫附溫度優化 93
圖49 複合式材料分層殘留比 93
圖50 複合式材料混層殘留比 93
圖51 脫附時間優化層析圖 94
圖52 脫附時間優化柱狀圖 94
圖53 Air Monitoring Trap材料崩解 95
圖54 更換Trap管前後層析圖譜比較 95
圖55 更換Trap管前內標層析疊圖 96
圖56 全氟三丁胺 (PFTBA) 實際圖 97
圖57 吸取速率計算流程 113
圖58 溫度及濕度影響之實驗設計 114
圖59 Markes MTS-32 (multiple-tube sampler) 120
圖60 PerkinElmer STS-25 (sequential tube sampler) 120
圖61 採樣遮罩實際架設圖 121
圖62 本研究採樣地點 (藍色：主動式；紅色：被動式) 122
圖63 火災後有機化學實驗室 123
圖64 事件日與平常日之層析圖譜疊圖 123
圖65 (a)有機實驗室 (b)氣體分析實驗室 (c)液體分析實驗室 (d)生化實驗室 124
圖66 實驗室被動式採樣疊圖 125
圖67 (a) 高雄測站外觀 (b)採樣遮罩架設 (c)現地質譜採樣口 126
圖68 2021年被動式採樣與現地質譜之氯乙烯濃度結果 127
圖69 2021年被動式採樣與現地質譜之四氯化碳濃度結果 127
圖70 2021年被動式採樣與現地質譜之氯仿濃度結果 128
圖71 2022年被動式採樣與現地質譜之氯乙烯濃度結果 128
圖72 2022年被動式採樣與現地質譜之四氯化碳濃度結果 129
圖73 2022年被動式採樣與現地質譜之氯仿濃度結果 129
圖74 Canister與現地質譜之氯仿濃度結果 130
圖75 氯仿數據後推軌跡 130
圖76 大園工業區採樣佈點圖 131
圖77 Chloroform離子碎片層析圖 132
圖78 含氯化物之全圖譜 132
圖79 83, 62, 117離子碎片層析圖 132
圖80 (a)環境變遷研究中心 (b)地球科學研究所 (c)STS-25架設 133
圖81 中研院主要出現物種濃度 134
圖82 彰化和美高中及光化測站相對位置 134
圖83 (a) PM2.5及VOCs採樣設備 (b)MTS-32內部 135
圖84 苯每小時濃度比較及柱狀圖 136
圖85 甲苯每小時濃度比較 136
圖86 物種之同源性 137
圖87 和美高中與光化測站物種出現頻率之濃度 137
圖88 光化測站物種出現頻率之濃度 138
圖89 和美高中每天平均濃度高值物種呈現 138
圖90 (a)崙背測站地點 (b)測站鄰近工廠相對距離 139
圖91 光化測站高值圖譜 140
圖92 (a)崙背測站外觀 (b)STS-25架設位置 (c)光化ATD-GC-FID 140
圖93 光化測站圖譜 141
圖94 崙背層析圖譜 141
圖95 甲苯比對 142
圖96 採樣空管實際圖 143
圖97 濾紙填充示意圖 143
圖98 濾紙脫附溫度層析圖 145
圖99 (a)濾紙空白 (b)濾紙樣品 145
圖100 濾紙樣品層析圖 146

表目次
表1 VOCs的定義 7
表2 各國HAPs管制相關法規 10
表3 臺灣及美國HAPs排放管制及相關標準方法檢測物種清單 12
表4 特殊性工業區管制之特殊性工業 15
表5 特殊性工業區依區內容納工業需個別監測之其他空氣污染物 17
表6 特殊性工業區應監測之有機光化前驅物 18
表7 特殊性工業區應監測之有害空氣污染物 19
表8 周界VOCs國內外監測方法比較 22
表9 採樣分析方法優缺點比較 24
表10 離線式採樣分析方法統計 24
表11 NIEA A715.16B標準方法及文獻的比較 32
表12 U.S. EPA Method 325B中提及物種之吸取速率 35
表13 吸附劑的種類及性質比較 39
表14 物種之溫度、濕度與反擴散的差異a 48
表15 採樣管之適化參數 54
表16 常見系統彙整 56
表17 常用之吸附劑種類 57
表18 除水方式之比較 58
表19 目標物種相關資訊 61
表20 內標準品基本資料 65
表21 目標物種對照表 67
表22 多重床吸附材料的配置 75
表23 Carbopack X 之 R2、MDL、樣品儲存回收率、BD 76
表24 Carboxen 569 之 R2、MDL、樣品儲存回收率、BD 78
表25 Carbopack X 實驗吸取速率之溫度及相對濕度變化影響 81
表26 Carboxen 569 實驗吸取速率之溫度及相對濕度變化影響 83
表27 複合式材料配置含量 86
表28 複合式材料配置比例 87
表29 分層配置比例 88
表30 混層配置比例 88
表31 自動化熱脫附儀條件 95
表32 更換Trap之相對標準偏差比較 96
表33 檢量線相關係數 100
表34 採樣管之方法偵測極限 (ppbv) 104
表35 採樣管之精密度 106
表36 採樣管之準確度 109
表37 與文獻實驗吸取速率 112
表38 採樣管之實驗吸取速率 115
表39 採樣管之適合採集目標物種 117
表40 實驗室內之物種 124
表41 濾紙Condition最適溫度 144
表42 濾紙脫附最適溫度 144

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指導教授

王家麟(Jia-Lin Wang)

審核日期

2023-7-4

推文