環保專案成果報告查詢系統

專案計畫編號	EPA-154109012
經費年度	109
計畫經費	3,200 千元
預算科目	固定污染源管制
專案開始日期	2020/01/20
專案結束日期	2020/12/31
專案主持人	許逸群
主辦單位	環檢所
承辦人	方建翔
執行單位	崑山科技大學
專案分類	環境監測及檢測
中文關鍵字	有害空氣污染物，周界空氣，串聯質譜儀
英文關鍵字	Hazardous Air Pollutants, ambient air, The tandem mass spectrometer
協同主持人	鄭景智
共同主持人
計畫聯絡人	蘇珮甄
計畫聯絡電話	06-2055952#
計畫聯絡信箱	kksn5488@gmail.com

中文摘要	環保署於民國108年預告「固定污染源有害空氣污染物排放標準」(草案)，其中針對72項重要有害空氣污染物，擬依三階段期程制定其固定污染源排放標準，故本計畫乃參考NIEA A801、method 10、method 8270E、CLA2101與前期「排放管道中硝苯等半揮發性有機物調查技術開發」之採樣與分析技術，針對硝苯、鄰苯二甲酸二(2-乙基己基)酯、六氯乙烷、聯苯胺、4,4'-亞甲雙(2-氯苯胺)、六氯苯、多氯聯苯及多環芳香烴等空氣污染物進行GC/MS/MS與LC/MS/MS調查技術之研究開發。本計畫規劃探討前述污染物相關採集效率、層析儀器最佳化分析條件、適用濃度範圍、保存條件及可能造成之干擾及去除方法等，建立合宜之調查技術作業程序。並依循環檢所所訂之「環境檢測標準方法驗證程序準則」針對所建立的調查技術進行評估，包括檢量線建立、方法偵測極限測定、品保品管規範（如準確度及精密度）建立及真實樣品採樣、樣品前處理及分析測定等。最後根據計畫執行調查技術建立成效，於期末報告須提出符合環檢所方法格式規範之空氣中前述空氣污染物調查技術草案。在GC/MS/MS部分，針對檢量線測試為依據NIEA M731 方法以內標準品進行校正 (感應因子校正法)所得結果，各待測物相對標準偏差RSD(%)結果皆能符合方法技術上可接受之規定(< 30%)。在方法偵測極限結果，六氯乙烷偵測極限為2.506 ng/mL、硝苯偵測極限為2.308 ng/mL、六氯苯偵測極限為2.640 ng/mL、鄰苯二甲酸二(2-乙基己基)酯(DEHP)偵測極限為25.816 ng/mL，多氯聯苯的偵測極限方面，一至十氯聯苯偵測極限約在1.833至3.187 ng/mL，多環芳香烴化合物偵測極限則約2.098 ng/mL至3.122 ng/mL，經參考「固定污染源有害空氣污染物排放標準」(草案)之周界標準值及本計畫設計之採樣體積約162.5m3所得之預估標準值總量，比較結果顯示各待測物MDL值皆低於十分之一標準值總量(設計方法開發之目標)，分析條件可符合方法建立期望。而LC/MS/MS檢量線部分，經測試確認查核後，聯苯胺及4,4’-亞甲雙(2-氯苯胺)二項線性迴歸相關係數R皆達到0.999以上。在方法偵測極限結果，聯苯胺為0.230 ng/mL、4,4’-亞甲雙(2-氯苯胺)偵測極限為0.231 ng/mL，經參考「固定污染源有害空氣污染物排放標準」草案中規範周界標準值，與規劃之採氣體積後預估標準值總量進行比對，聯苯胺與4,4-亞甲雙(2-氯苯胺)MDL可低於預估標準值總量之十分之一，MDL可達到法所需方法設計建立之期望。在採樣部分，本計畫亦針對所參照之NIEA A801方法規範中，吸附劑(XAD2)填充量(60g)於實務採樣過程會產生之採樣系統壓損問題，進行採樣條件調整與測試。測試內容包含填充介質量與採樣流率之調整，測試結果顯示在填充30公克XAD2吸附劑且搭配高量採樣器於採樣流率0.112 m3/min可達到最適的採樣條件，而針對聯苯胺與4,4'-亞甲雙(2-氯苯胺) 經參考委會CLA 2101、NIEA A705方法採用甲醇(含0.17%三乙胺)為吸收液，並在HPLC/MS/MS分析下可獲得良好的回收率。相關條件亦運用於實場採樣作業，本計畫共計完成國內工廠4處次周界空氣實廠採樣，經由實廠驗證可知調查技術開發之可行性。此外，計畫執行期間(109年8月、10月)分別成果完成兩場次調查技術擴散，並提出本計畫相關調查技術草案，提供日後環保署檢測技術援引之參考。
中文關鍵字	有害空氣污染物，周界空氣，串聯質譜儀

中文摘要

環保署於民國108年預告「固定污染源有害空氣污染物排放標準」(草案)，其中針對72項重要有害空氣污染物，擬依三階段期程制定其固定污染源排放標準，故本計畫乃參考NIEA A801、method 10、method 8270E、CLA2101與前期「排放管道中硝苯等半揮發性有機物調查技術開發」之採樣與分析技術，針對硝苯、鄰苯二甲酸二(2-乙基己基)酯、六氯乙烷、聯苯胺、4,4'-亞甲雙(2-氯苯胺)、六氯苯、多氯聯苯及多環芳香烴等空氣污染物進行GC/MS/MS與LC/MS/MS調查技術之研究開發。本計畫規劃探討前述污染物相關採集效率、層析儀器最佳化分析條件、適用濃度範圍、保存條件及可能造成之干擾及去除方法等，建立合宜之調查技術作業程序。並依循環檢所所訂之「環境檢測標準方法驗證程序準則」針對所建立的調查技術進行評估，包括檢量線建立、方法偵測極限測定、品保品管規範（如準確度及精密度）建立及真實樣品採樣、樣品前處理及分析測定等。最後根據計畫執行調查技術建立成效，於期末報告須提出符合環檢所方法格式規範之空氣中前述空氣污染物調查技術草案。在GC/MS/MS部分，針對檢量線測試為依據NIEA M731 方法以內標準品進行校正 (感應因子校正法)所得結果，各待測物相對標準偏差RSD(%)結果皆能符合方法技術上可接受之規定(< 30%)。在方法偵測極限結果，六氯乙烷偵測極限為2.506 ng/mL、硝苯偵測極限為2.308 ng/mL、六氯苯偵測極限為2.640 ng/mL、鄰苯二甲酸二(2-乙基己基)酯(DEHP)偵測極限為25.816 ng/mL，多氯聯苯的偵測極限方面，一至十氯聯苯偵測極限約在1.833至3.187 ng/mL，多環芳香烴化合物偵測極限則約2.098 ng/mL至3.122 ng/mL，經參考「固定污染源有害空氣污染物排放標準」(草案)之周界標準值及本計畫設計之採樣體積約162.5m3所得之預估標準值總量，比較結果顯示各待測物MDL值皆低於十分之一標準值總量(設計方法開發之目標)，分析條件可符合方法建立期望。而LC/MS/MS檢量線部分，經測試確認查核後，聯苯胺及4,4’-亞甲雙(2-氯苯胺)二項線性迴歸相關係數R皆達到0.999以上。在方法偵測極限結果，聯苯胺為0.230 ng/mL、4,4’-亞甲雙(2-氯苯胺)偵測極限為0.231 ng/mL，經參考「固定污染源有害空氣污染物排放標準」草案中規範周界標準值，與規劃之採氣體積後預估標準值總量進行比對，聯苯胺與4,4-亞甲雙(2-氯苯胺)MDL可低於預估標準值總量之十分之一，MDL可達到法所需方法設計建立之期望。在採樣部分，本計畫亦針對所參照之NIEA A801方法規範中，吸附劑(XAD2)填充量(60g)於實務採樣過程會產生之採樣系統壓損問題，進行採樣條件調整與測試。測試內容包含填充介質量與採樣流率之調整，測試結果顯示在填充30公克XAD2吸附劑且搭配高量採樣器於採樣流率0.112 m3/min可達到最適的採樣條件，而針對聯苯胺與4,4'-亞甲雙(2-氯苯胺) 經參考委會CLA 2101、NIEA A705方法採用甲醇(含0.17%三乙胺)為吸收液，並在HPLC/MS/MS分析下可獲得良好的回收率。相關條件亦運用於實場採樣作業，本計畫共計完成國內工廠4處次周界空氣實廠採樣，經由實廠驗證可知調查技術開發之可行性。此外，計畫執行期間(109年8月、10月)分別成果完成兩場次調查技術擴散，並提出本計畫相關調查技術草案，提供日後環保署檢測技術援引之參考。

中文關鍵字

有害空氣污染物，周界空氣，串聯質譜儀

類型	檔名	檔案大小	說明	最新版公開日期
期末報告	空氣中硝苯等半揮發性有機物調查技術開發(12)成果報告.pdf	12MB		2021/1/1 上午 12:00:00

摘要	The Environmental Protection Administration Executive Yuan announced the “Emission Standards for Hazardous Air Pollutants from Stationary Pollution Sources” (draft) in 2019. There are 72 important hazardous air pollutants planned to develop the emission standards according to a three-stage schedule. The research method is based on NIEA A807, Method 10, and Method 8270E for sampling and analytical development of Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Benzidine, 4,4'-Methylenebis(2-chloroaniline), Hexachlorobenzene, Polychlorinated biphenyl (PCBs) and Polycyclic aromatic hydrocarbons (PAHs). The project aims to establish appropriate survey technology of the aforementioned pollutants, and the factors of collection efficiency, chromatography instrument optimization analysis conditions, applicable concentration range, storage conditions, and possible interference and removal methods caused by moisture, etc. should be considered. And then the research must be evaluated according to the "Environmental Testing Standard Method Verification Procedures Guidelines" set by the Environmental Analysis Laboratory, EPA. In the final report, the draft of development of sampling and analytical methods for semi-volatile organic compounds in stacks must be proposed, and that meets the specifications of the method format. In the beginning, six analyte including Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Hexachlorobenzene, PCBs and PAHs were tested by GC/MS/MS with reference to the NIEA M731 method. The calibration curve was verified by internal standard, and the results show that the relative standard deviation (RSD %) complies with the technically acceptable requirements of the method (<30%). Nevertheless, the results of method detection limit compared with the project's estimated emission standards, showing that all compounds meet the requirements of the regulatory standards. The method could achieve expectation of method establishment. Benzidine and 4,4'-Methylenebis(2-chloroaniline) (MOCA) were analyzed by LC/MS/MS. Regarding calibration curve, the correlation coefficient R of linear regression exceeded 0.999. The result of method detection limit compared with the project's estimated emission standards, showing that both compounds meet the requirements of the regulatory standards. The method could achieve expectation of method establishment In sampling compounds, referring to NIEA A801 method, Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Hexachlorobenzene, PCBs and PAHs sampled by 60 g adsorbent XAD2. However, in sampling process meet big trouble with pressure loss. The project get great condition with 30 g adsorbent and flow rate 0.125 m3/min. The method of sampling compounds Benzidine and MOCA referring to CLA 2101 and NIEA A705. Using Methanol with 0.17 % Triethylamine as absorbent had great recovery rate. There are 4 samplings of stacks in the domestic factory completed. The result showed that sampling and analysis condition were available. Besides, two sessions of technological diffusion were held in August and October 2020 respectively. In conclusion, the draft program of sampling and analytical methods for semi-volatile organic compounds in stacks is proposed to provide future reference of the detection technology.
英文關鍵字	Hazardous Air Pollutants, ambient air, The tandem mass spectrometer

摘要

The Environmental Protection Administration Executive Yuan announced the “Emission Standards for Hazardous Air Pollutants from Stationary Pollution Sources” (draft) in 2019. There are 72 important hazardous air pollutants planned to develop the emission standards according to a three-stage schedule. The research method is based on NIEA A807, Method 10, and Method 8270E for sampling and analytical development of Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Benzidine, 4,4'-Methylenebis(2-chloroaniline), Hexachlorobenzene, Polychlorinated biphenyl (PCBs) and Polycyclic aromatic hydrocarbons (PAHs). The project aims to establish appropriate survey technology of the aforementioned pollutants, and the factors of collection efficiency, chromatography instrument optimization analysis conditions, applicable concentration range, storage conditions, and possible interference and removal methods caused by moisture, etc. should be considered. And then the research must be evaluated according to the "Environmental Testing Standard Method Verification Procedures Guidelines" set by the Environmental Analysis Laboratory, EPA. In the final report, the draft of development of sampling and analytical methods for semi-volatile organic compounds in stacks must be proposed, and that meets the specifications of the method format. In the beginning, six analyte including Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Hexachlorobenzene, PCBs and PAHs were tested by GC/MS/MS with reference to the NIEA M731 method. The calibration curve was verified by internal standard, and the results show that the relative standard deviation (RSD %) complies with the technically acceptable requirements of the method (<30%). Nevertheless, the results of method detection limit compared with the project's estimated emission standards, showing that all compounds meet the requirements of the regulatory standards. The method could achieve expectation of method establishment. Benzidine and 4,4'-Methylenebis(2-chloroaniline) (MOCA) were analyzed by LC/MS/MS. Regarding calibration curve, the correlation coefficient R of linear regression exceeded 0.999. The result of method detection limit compared with the project's estimated emission standards, showing that both compounds meet the requirements of the regulatory standards. The method could achieve expectation of method establishment In sampling compounds, referring to NIEA A801 method, Nitrobenzene, Bis(2-ethylhexyl)phthalate, Hexachloroethane, Hexachlorobenzene, PCBs and PAHs sampled by 60 g adsorbent XAD2. However, in sampling process meet big trouble with pressure loss. The project get great condition with 30 g adsorbent and flow rate 0.125 m3/min. The method of sampling compounds Benzidine and MOCA referring to CLA 2101 and NIEA A705. Using Methanol with 0.17 % Triethylamine as absorbent had great recovery rate. There are 4 samplings of stacks in the domestic factory completed. The result showed that sampling and analysis condition were available. Besides, two sessions of technological diffusion were held in August and October 2020 respectively. In conclusion, the draft program of sampling and analytical methods for semi-volatile organic compounds in stacks is proposed to provide future reference of the detection technology.

英文關鍵字

Hazardous Air Pollutants, ambient air, The tandem mass spectrometer