摘要
目前傳統檢測鄰苯二甲酸（政府公告方法CNS15138），都是利用索式萃取方法來萃取，萃取時間一般都要8~16小時，使用萃取溶劑大約100ml~250ml，但卻對沒有即方便的微波萃取政府公告方法，只需要5~10分鐘，使用萃取溶劑10~20ml，本研究開發最佳微波萃取技術，以針對塑料樣品中的禁用物質鄰苯二甲酸進行萃取，開發節省時間，使用少量溶劑的微波萃取技術。微波萃取最佳萃取條件的選擇是以探討萃取時間、萃取溶劑、等參數對萃取效率的影響。找出最佳微波萃取條件之後，再用氣相層析質譜儀來進行定性定量分析。 本研究最佳微波萃取條件為；500W微波功率於100℃溫度及20mL之甲醇氯仿1:2溶劑中進行20分鐘萃取，之後分別對標準樣品進行分析並與傳統索式方法所得結果比較。標準樣品參考值DBP、BBP、DEHP、DNOP為5.0ppm；DINP、DIDP為20.0ppm、標準樣品索式萃取所得結果分別為：DBP 4.95 ppm、BBP 4.96 ppm、DEHP 4.94 ppm、DNOP 4.98 ppm、DINP 19.94 ppm、DIDP 19.96 ppm；標準樣品微波萃取所得結果分別為：DBP 4.96 ppm、BBP 4.95 ppm、DEHP 4.96 ppm、DNOP 4.97 ppm、DINP 19.96 ppm、DIDP 19.95 ppm。 實驗最後並針對市面上所販售的塑膠奶瓶、兒童積木的這兩種嬰兒和兒童會放入口中的產品和假皮及電線絕緣外皮的這兩種只會接觸人體皮膚的產品做微波萃取;結果顯示本研究測試的塑膠奶瓶和兒童積木並沒有鄰苯二甲酸的含量被檢測出來，但是假皮卻有高濃度的鄰苯二甲酸含量DINP 3712550ppm DIDP 30165ppm，而電線絕緣外皮也有較高的鄰苯二甲酸被檢測出來DEHP 1684ppm DINP 1597ppm，可見在假皮和電線絕緣外皮因為只會接觸人體皮膚不會吞入口中，所以製造商可能會因此疏於嚴格的把關導致會有鄰苯二甲酸被使用而檢測出來。
並列摘要
Currently the traditional examination method for phthalate (Government Announced Method CNS15138) uses the soxhlet extract method，which takes generally 8~16 hours for the process and use about 100ml ~ 250ml of extractive solvent。But there is no Government Announced Method for convenient microwave extract which only needs 5~10 minutes and use 10ml ~ 20ml of extractive solvent。This research developed the best microwave extract technology，which extract the forbidden phthalate materials hidden inside the plastic sample。This microwave extract technology method not only saves time，but also uses less solvents。The best conditions for microwave extract method are to discusses the extract time, the extractive solvent, and the influence on the parameters for the extract efficiency。After the best microwave extract condition is discovered，we use the Gas Chromatography/Mass Selective Detector to analyze the qualitative and quantitative analysis。 In this research, the best microwave extract condition is: 500W microwave power in temperature 100℃degree and 20mL of methyl alcohol and chloroform 1:2 solvents for 20 minutes extraction。 Afterwards we compare and analyze the standard sample with the traditionally extracted results。Standard sample reference value DBP、 BBP、DEHP、DNOP are 5.0ppm； DINP、 DIDP are 20.0ppm， the standard sample soxhlet extract obtained result respectively are: DBP 4.95 ppm, BBP 4.96 ppm, DEHP 4.94 ppm, DNOP 4.98 ppm，DINP 19.94 ppm，DIDP 19.96 ppm；The standard sample microwave extract obtained results respectively are：DBP 4.96 ppm，BBP 4.95 ppm，DEHP 4.96 ppm，DNOP 4.97 ppm，DINP 19.96 ppm，DIDP 19.95 ppm.。 In the end the experiment aimed at the revertex milk bottle and children building block these two types of items which sells in the market and can be easily put in the mouth。The experiment also tested the non-conductive skin of electric wires and imitation leather。The result showed highly concentrated phthalate content DINP 3712550ppm DIDP 30165ppm in the imitation leather, but found nothing in the revertex milk bottle and building block。But the electric wire protective skin also has the high phthalate to examine DEHP 1684ppm DINP 1597ppm。Therefore we can concluded that because imitation leather and electric wire skin only contacts the human skin and not swallowed, so when the manufacturer test and the phthalate materials they tent to not focus in these areas and thus not tested。
參考文獻
延伸閱讀
- 林文喜（1967）。芳香烴之紫外光譜分析 第三報 二甲苯及乙苯之定量。化學，(56年2)，51-54。https://doi.org/10.6623/chem.1967011
- 吳信宏（2008）。以微波輔助萃取搭配液相層析質譜儀檢測固態樣品中六溴環十二烷之方法開發〔碩士論文，國立中央大學〕。華藝線上圖書館。https://www.airitilibrary.com/Article/Detail?DocID=U0031-0207200917352894
- 林芷韻（2015）。以聚苯乙烯高分子結合活性碳之整體成形管柱進行鄰苯二甲酸酯類化合物的固相微萃取〔碩士論文，中原大學〕。華藝線上圖書館。https://doi.org/10.6840/cycu201500921
- 黃世睿 (2013). Material Characterization at Microwave Frequency [master's thesis, National Tsing Hua University]. Airiti Library. https://doi.org/10.6843/NTHU.2013.00543
- 林辰（2014）。The study of Microwave Absorption on Conducting Surface〔碩士論文，國立臺灣大學〕。華藝線上圖書館。https://doi.org/10.6342/NTU.2014.02226