第一篇研究為利用雲點萃取法結合電熱式揮發感應耦合電漿質譜儀於水樣中分析銀奈米粒子。實驗中利用雲點萃取法 ( Cloud point extraction，CPE ) 作為前處理方法，萃取及預濃縮銀奈米粒子 ( Silver nanoparticles，AgNPs )，再利用泥漿取樣法結合電熱式揮發樣品進樣系統，來對微胞相的樣品進行取樣。本實驗是在水樣中先加入腐植酸 ( Humic acid ) 來防止銀奈米粒子在前處理過程中溶解，接著加入硫代硫酸鈉與銀離子形成水溶性錯合物，再加入界面活性劑Triton X-114進行萃取，AgNPs會因為疏水性進入微胞相中，當加熱至雲點溫度 ( Cloud point temperature ) 時，會產生相分離的現象，可有效將銀離子分離，且具有濃縮的優點。實驗中藉由微波來輔助雲點萃取，以提升萃取效率，縮短萃取時間。實驗結果中雲點萃取法之最適化為添加100 mg L-1腐植酸、0.25% m/v Na2S2O3和0.4% m/v Triton X-114，再加入HNO3將pH值調至2.0，於40℃進行微波輔助萃取20分鐘。搭配ETV樣品需求量少的優點，直接對萃取後的微胞相進行分析，以減少對微胞相的稀釋，另外實驗中也針對影響分析物揮發訊號之因素進行探討，包含修飾劑的添加、ETV的裂解溫度及揮發溫度等。最後使用基質匹配校正曲線法對RO水、自來水和澄清湖湖水樣品進行定量分析，此方法對銀奈米粒子的偵測極限為具有0.002 μg L-1。
第二篇研究為利用電熱式揮發感應耦合電漿質譜儀對眼影中鉻、砷、鎘、銻、汞和鉛元素分析之應用。實驗在動態反應室 ( Dynamic reaction cell，DRC ) 系統下進行，選擇氧氣作為反應氣體來減輕樣品與石墨爐中碳原子對分析物所造成的光譜干擾，由實驗結果發現以1.0% m/v Thioacetamide ( TAA ) 作為修飾劑有助於提升分析物訊號，經最適化探討後，乳濁狀眼影樣品濃度除了分析鉛元素時配製0.1% m/v外，其餘分析物則以1.0% m/v乳濁狀樣品進行定量，裂解溫度與揮發溫度分別設定為250℃和1600℃，並在實驗中探討是否有其他干擾物對分析物造成光譜干擾。最後，將本系統運用於市售眼影樣品之定量分析上，由於眼影無標準參考樣品，因此以乳霜標準參考樣品GBW09305來驗證本方法之準確性。實驗中分別使用標準添加法與同位素稀釋法進行定量分析，同時與消化後以傳統式霧化器所得結果相互比較，證明此方法之可行性。此方法對於鉻、砷、鎘、銻、汞和鉛元素偵測極限分別為0.023、0.004、0.003、0.006、0.001和0.021 μg L -1。

The first research focused on, cloud point extraction (CPE) combined with ETV-ICP-MS analysis to determine the silver nanoparticles (AgNPs) in water samples was studied in detail. The CPE techniques were utilized to extract and pre-concentrate AgNPs. Ultrasonic slurry sampling was used to combine with the electrothermal vaporization (ETV) for sampling the micelles. However, humic acid was added to prevent the dissolution of AgNPs, followed by the addition of Na2S2O3 with Ag ions to form hydrophilic complexes. Moreover, AgNPs in the presence of Triton X-114 were extracted into micelles due to hydrophobic nature. After heating to cloud point temperature, the phase separation was occurred. In our study, microwave assisted extraction techniques (MAE) were used to improve the extraction efficiency and shorten the incubation time. The optimum conditions for the CPE were to add 100 mg L-1 humic acid, 0.25% m/v Na2S2O3 and 0.4% m/v Triton X-114, and then add HNO3 to adjust the pH to 2.0. MAE was carried out at 40℃ for 20 minutes. With the advantages of small sample volume of ETV techniques, the extracted micelles were analyzed directly to reduce the dilution of the micelles. In addition to that, we explored various factors that affect the vaporizable signal of the analyte including modifier, pyrolysis temperature and vaporization temperature. Matrix-matched calibration curve was used to determinate the AgNPs in RO water, tap water and Chengcing lake water, and the detection limit of AgNPs was 0.002 μg L-1.
The second research focused on, determination of Cr, As, Cd, Sb, Hg and Pb in eyeshadow samples by ETV-ICP-MS techniques was studied in detail. In the experiment methodology was carried out under dynamic reaction cell system (DRC), with reaction gas (oxygen) was chosen to mitigate the spectral interference. The results found that 1.0% m/v thioacetamide (TAA) as a modifier to enhance the signal of the analyte. To determinate Pb, the concentration of eyeshadow samples was employed 0.1% m/v, and the concentration of eyeshadow samples was 1.0% m/v for the remaining analytes. In addition, the pyrolysis temperature of vaporization temperature were optimized at 250℃ and 1600℃ respectively. Moreover, there is no spectral interference to the analyte which we confirmed very well manner. Finally, the system was applied to determine the Cr, As, Cd, Sb, Hg and Pb in commercial eyeshadow samples. Since, there is no standard reference material (SRM) for eyeshadow samples. However, here we performed cream standard reference material GBW09305 to measure the accuracy of this method. In addition to that we explored, the standard addition method and isotope dilution method were used to determinate analytes, and compared with the results obtained by the traditional atomizer after microwave digestion to prove the feasibility of this method. The detection limit of this method Cr, As, Cd, Sb, Hg and Pb was found to be 0.023, 0.004, 0.003, 0.006, 0.001 and 0.021 μg L-1, respectively.

論文審定書 i
謝誌 ii
摘要 iii
Abstract v
目錄 vii
圖目錄 ix
表目錄 xi
第一章 雲點萃取法結合電熱式揮發感應耦合電漿質譜儀於水樣中的銀奈米粒子分析之應用
壹、 前言 1
一、 研究背景 1
二、 雲點萃取法簡介 2
三、 微波輔助萃取簡介 5
四、 超音波泥漿取樣法結合電熱式揮發樣品輸入系統簡介 5
貳、 實驗部分 8
一、 儀器裝置及操作條件 8
二、 試劑藥品及溶液的配製 12
參、 實驗過程 14
一、 雲點萃取條件之最適化 14
二、 ETV條件之最適化 18
三、 校正曲線 21
四、 樣品製備與分析 21
肆、 結果與討論 23
一、 雲點萃取條件之最適化 23
二、 ETV條件之最適化 35
三、 校正曲線 41
四、 真實樣品之測定 47
伍、 結論 52
陸、 參考文獻 53
第二章 電熱式揮發感應耦合電漿質譜儀於眼影樣品中鉻、砷、鎘、銻、汞和鉛元素分析之應用
壹、 前言 59
一、 研究背景 59
二、 動態反應室簡介 61
三、 鉻、砷、鎘、銻、汞和鉛之個論 62
四、 同位素稀釋法簡介 63
貳、 實驗部分 65
一、 儀器裝置及操作條件 65
二、 試劑藥品及溶液的配製 65
參、 實驗過程 71
一、 ETV條件之最適化 71
二、 樣品稀釋倍數之探討 73
三、 DRC系統之最適化 74
四、 ETV系統之裂解溫度和揮發溫度的選擇 75
五、 光譜 ( 同質量 ) 干擾 75
六、 校正曲線 76
七、 樣品製備與分析 76
肆、 結果與討論 80
一、 ETV條件之最適化 80
二、 樣品稀釋倍數之探討 85
三、 DRC系統之最適化 85
四、 ETV系統之裂解溫度和揮發溫度的選擇 88
五、 光譜 ( 同質量 ) 干擾 95
六、 校正曲線 95
七、 真實樣品之測定 100
伍、 結論 106
陸、 參考文獻 107

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