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研究生:姜義峰
論文名稱:以液相微萃取法搭配多元素石墨爐原子吸收光譜儀偵測水樣中的鉛、鎘元素
論文名稱(外文):Determination of lead and cadmium in water samples by liquid-phase microextraction coupled with graphite furnace atomic absorption spectrometry.
指導教授:黃賢達黃賢達引用關係
學位類別:碩士
校院名稱:國立清華大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2007
畢業學年度:95
語文別:中文
論文頁數:71
中文關鍵詞:液相微萃取法石墨爐原子吸收光譜儀鈀修飾劑
外文關鍵詞:leadcadmiumliquid-phase microextractionGFAASpalladium chemical modifier
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本研究以三液相動態微萃取法(dynamic liquid-liquid-liquid microextraction, LLLME)結合多元素石墨爐原子吸收光譜儀偵測水樣中的鉛、鎘元素。利用有機相中的螯合劑(dithizone),螯合水樣裡的重金屬,反萃重金屬至受層(acceptor phase)硝酸中,再與鈀修飾劑一同注入石墨爐內進行偵測。與傳統液液萃取或固相萃取法相比,此法較簡便,溶劑用量大幅減少;相較於固相微萃取法,則具有耗材花費較少的優點。石墨爐原子吸收光譜儀的最佳化溫控程式與鈀修飾劑用量分別為:灰化溫度600℃、原子化溫度2000℃;5μg鈀。探討各種可能影響萃取效率的變因包括:有機溶劑的選擇、予層(donor phase)水樣pH值、受層(acceptor phase)硝酸濃度、螯合劑用量、樣品攪拌速率與萃取時間。在最佳化條件下(1% dithizone/4-nitro-m-xylene萃取液、予層水樣pH=5、受層硝酸濃度10% 、攪拌速率700r.p.m.、萃取時間40分鐘),鉛、鎘的偵測極限分別為0.032 ng/mL、0.037 ng/mL;精密度是以添加低濃度分析物在真實樣品(0.1 ng/mL Pb、0.2 ng/mL Cd),重複分析5次所得相對標準偏差(RSD)表示之。求得Pb、Cd精密度分別為7%、4%。未來工作為添加低濃度待測物於真實樣品,計算相對回收率,若其值落在100±15% 的範圍內,即可用檢量線進行定量。
In this thesis, we combined dynamic liquid-liquid-liquid microextraction (LLLME) with multi-elements graphite furnance atomic absorption spectrometry (GFAAS) to determine trace lead and cadmium in water samples. In the extraction step, two elements in 30 mL of the water sample which adjusted to pH 5 (donor phase) were extracted into an organic film containing a chelating agent (1 % dithizone) in 4-nitro-m-xylene and then back-extracted to 5 μL, 10 % nitric acid solution (acceptor phase). 4.5 μL acceptor phase and 0.5 μg palladium (chemical modifier) were injected into the graphite tube by syringe simultaneously. The continual movement of organic and acceptor phases not only resulted in a renewable organic film but also enhanced the enrichment factor. Under the optimized conditions (ashing temp. 600℃, atomization temp. 2000℃, stirring rate 700 r.p.m., extraction time 40 minutes), the detection limits and relative standard deviations (RSDs) were 0.032 ng/mL, 0.037 ng/mL ; 7%, 4% for lead and cadmium, respectively.
第一章 緒論
……………………………………………………………………1
1-1 分析物簡介
…………………………………………………………………1
1-1-1 鉛
……………………………………………………………………………2
1-1-2 鎘 ……………………………………………………………………………5
1-2 微量重金屬元素的分析方法之回顧與探討 ………………………………7
1-3 多元素石墨爐原子吸收光譜儀 ……………………………………………8
1-4 化學修飾劑…………………………………………………………………11
1-4-1 鈀修飾劑的應用……………………………………………………………12
1-4-2 氫氣的使用…………………………………………………………………13
1-4-3 鎂修飾劑的應用……………………………………………………………14
1-5 微量元素前濃縮方法………………………………………………………14
1-6 液相微萃取法………………………………………………………………16
1-6-1 單滴微萃取法………………………………………………………………16
1-6-2 中空纖維液相微萃取法……………………………………………………17
1-6-3 溶劑棒微萃取………………………………………………………………20
1-6-4 薄膜輔助溶劑萃取…………………………………………………………21
1-6-5 分散式液液微萃取法………………………………………………………21
1-7 本論文研究方向……………………………………………………………22
第二章 實驗…………………………………………………………………………24
2-1 試藥…………………………………………………………………………24
2-2 儀器裝置……………………………………………………………………24
2-3 藥品純化及器皿清洗………………………………………………………25
2-4 實驗步驟……………………………………………………………………25
第三章 結果與討論…………………………………………………………………27
3-1 螯合劑萃取體系……………………………………………………………27
3-2 三液相動態微萃取機制……………………………………………………27
3-3 最佳化條件探討……………………………………………………………29
3-3-1 最佳溫控程式的尋找………………………………………………………29
3-3-2 鈀修飾劑用量………………………………………………………………29
3-3-3 萃取溶劑的選擇……………………………………………………………30
3-3-4 予層水樣pH值的影響 ……………………………………………………31
3-3-5 螯合劑用量…………………………………………………………………32
3-3-6 受層硝酸濃度的影響………………………………………………………32
3-3-7 樣品攪伴速率………………………………………………………………32
3-3-8 萃取時間……………………………………………………………………33
3-3-9 偵測極限、精密度…………………………………………………………33
3-4 未來的實驗方向與展望……………………………………………………34
第四章 結論…………………………………………………………………………35
參考資料 ……………………………………………………………………………36




















表目錄
表(一) 四種儀器的偵測極限比較…………………………………………………48
表(二) 側向加熱石墨爐與縱向加熱石墨爐原子吸收光譜儀原子化溫度比較…49
表(三) 數種商業化原子吸收光譜儀之比較………………………………………50
表(四) 常用化學修飾劑……………………………………………………………51
表(五) 儀器實驗參數………………………………………………………………52
表(六) 實驗偵測極限與精密度……………………………………………………53
表(七) 不同液相微萃取法應用於Pb、Cd萃取之比較……………………………54





















圖目錄
圖(一) 二度空間光譜形成示意圖………………………………………………55
圖(二) SIMA 6000光學系統設計 ………………………………………………56
圖(三) 固態光電半導體偵測器與光電倍增管量子效率比較…………………57
圖(四) 側向加熱式石墨爐原子化器……………………………………………58
圖(五) 以中空纖維保護有機層的兩液相微萃取法裝置圖……………………59
圖(六) 實驗裝置示意圖…………………………………………………………60
圖(七) 雙硫腙與其金屬錯合物結構圖…………………………………………61
圖(八) 三液相動態微萃取法萃取機制示意圖…………………………………62
圖(九) 灰化溫度對原子吸收訊號之影響………………………………………63
圖(十) 原子化溫度對原子吸收訊之影響………………………………………64
圖(十一) Pd修飾劑用量對原子吸收訊號之影響…………………………………65
圖(十二) 有機溶劑對萃取效率之影響……………………………………………66
圖(十三) Donor phase pH值對萃取效率之影響…………………………………67
圖(十四) Dithizone濃度對萃取效率之影響 ……………………………………68
圖(十五) 硝酸濃度對萃取效率之影響……………………………………………69
圖(十六) 樣品攪拌速率對萃取效率之影響………………………………………70
圖(十七) 萃取時間對萃取效率之影響……………………………………………71
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