第一部分的研究將以泥漿取樣法結合USS-ETV-DRC-ICP-MS直接對於燃油樣品中之硫、砷、鎘、汞、鉛元素的含量進行分析，研究中對於乳化樣品的配製、添加之修飾劑、無機酸、界面活性劑對於分析物訊號的影響、儀器操作條件以及多原子離子之光譜干擾等參數進行探討，由實驗結果發現以Pd做為修飾劑能夠提升分析物之熱穩定性，在樣品中添加Tartaric acid與HNO3則能夠有效的改善訊號的分岔，Triton X-100能夠使燃油樣品均勻地乳化，因此選擇1 μg Pd、0.5% m/v Tartaric acid、1% m/v Triton X-100與0.5% v/v HNO3作為最適化條件，熱解溫度為380℃，揮發溫度為2100℃。使用ICP-MS進行分析常受限於光譜干擾造成定量的準確度不佳，因此可搭配動態反應管（Dynamic reaction cell，DRC）來減輕光譜干擾，如本研究中的32S+嚴重受到16O16O+離子的光譜干擾，因此採用O2作為反應氣體去除此干擾，並對於氣體流速、Rpq等參數進行探討，此外藉由在樣品中添加不同濃度的干擾物，偵測分析元素之訊號面積與同位素比例的變化，確定本研究之方法不會受到光譜干擾影響，最後將此最適化條件應用於燃油樣品中微量元素之定量分析。
單粒子感應耦合電漿質譜儀（Single particle ICP-MS）是一種用於檢測、鑑定與量化奈米粒子的新興技術，此技術能夠提供元素組成、粒徑、粒子濃度等資訊外，尚可同時對金屬離子進行檢測，第二部分的研究為單粒子感應耦合電漿質譜儀於銀離子與銀奈米粒子之分析，研究中對於取樣數目進行優化後，選擇取樣數目為24000進行實驗，探討不同濃度之銀離子及不同粒徑大小之銀奈米粒子與訊號之關係、粒子濃度與訊號產生頻率之關係，展示了此方法同時偵測奈米粒子與金屬離子之可行性，研究中發現儀器背景雜訊需在巨集中設定適當的Minimum Noise Threshold來消除，透過傳統霧化器及酸消化的方式對於實驗結果進行驗證，最後將此技術應用於環境水樣品中奈米粒子的檢測，未來希望能夠進一步應用於不同樣品及不同元素奈米粒子的分析。

The first research, the determination of S, As, Cd, Hg and Pb in fuels by USS-ETV-ICP-MS was described. Palladium and tartaric acid was used as the modifier to enhance the ion signals. In the experiment procedure, the operation conditions, sample concentration, DRC system conditions and spectral interference were studied. Vaporization temperature and ash temperature was set as 2100oC and 380oC. Oxygen was used in the dynamic reaction cell to convert 32S+ to 32S16O+, that can reduce the interference causing by 16O16O+. Finally, the method has been applied to determine S, As, Cd, Hg and Pb in SDF-3X, a sulfur standard solution in diesel fuel and three different kinds of fuels by using standard addition method and ARIDUS-DRC-ICP-MS method. After digestion, compare with the quantitative results obtained from the conventional pneumatic nebulizer to verify the feasibility. The method detection limit estimated from standard addition curves was 39, 0.07, 0.10, 0.07, 0.07 ng g-1 for S, As, Cd, Hg and Pb respectively.
The second research, determination of dissolved silver(I) and silver nanoparticles based on single particle detection by ICP-MS was studied. ICP-MS is unique in its ability to provide information on nanoparticle size, size distribution, elemental composition, and number concentration in a single, rapid analysis. In the experiment procedure, the influences of number of readings were studied. In order to get enough pulse signals, 24000 readings were chosen. The study found that we should set the Minimum Noise Threshold to eliminate the instrument background noise. Through pneumatic nebulizers and acid digestion, we can validate the results. Finally, environmental water being added with silver nanoparticles was tested to obtain a similar size distribution and number concentration that demonstrates the feasibility of simultaneously detecting nanoparticles and metal ions.

目錄
論文審定書 i
謝誌 ii
摘要 iii
Abstract iv
目錄 v
圖目錄 viii
表目錄 x


第一章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於燃油樣品中微量元素分析之應用
壹、前言 1
一、研究背景 1
二、硫、砷、鎘、汞及鉛之個論 3
三、超音波泥漿取樣法結合電熱式揮發樣品輸入系統簡介 4
貳、實驗部分 9
一、 儀器裝置及操作條件 9
二、 試劑藥品及溶液的配製 15
參、結果與討論 20
一、 修飾劑的選擇 20
二、 界面活性劑對分析物訊號的影響 25
三、 酸對分析物訊號的影響 25
四、 樣品稀釋倍數探討 28
五、 裂解溫度及揮發溫度的探討 31
六、 DRC系統之最適化 31
七、 光譜干擾 39
八、 校正曲線 39
九、 定量分析 44
肆、結論 50
伍、參考文獻 51


第二章 單粒子感應耦合電漿質譜儀於銀奈米粒子與銀離子之分析
壹、前言 55
一、研究背景 55
二、單粒子感應耦合電漿質譜儀簡介 57
貳、實驗部分 61
一、 儀器裝置及操作條件 61
二、 試劑藥品及溶液的配置 61
參、結果與討論 65
一、銀奈米粒子與銀離子訊號之探討 65
二、取樣數目之優化探討 65
三、奈米粒子的偵測 69
四、銀離子與銀奈米粒子之檢測 75
五、銀奈米粒子數目濃度之驗證 75
六、環境樣品分析 77
肆、結論 83
伍、參考文獻 84

 
圖目錄
第一章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於燃油樣品中微量元素分析之應用
圖1- 1超音波泥漿取樣器裝置圖 8
圖1- 2 ETV-ICP-MS 系統裝置簡圖 11
圖1- 3薄膜去溶劑系統Aridus儀器構造 14
圖1- 4實驗流程圖 18
圖1- 5修飾劑Pd濃度對分析物訊號之影響 24
圖1- 6修飾劑tartaric acid濃度對分析物訊號之影響 26
圖1- 7界面活性劑Triton X-100濃度對分析物訊號之影響 27
圖1- 8 HNO3濃度對分析物訊號之影響 29
圖1- 9乳濁狀樣品濃度對分析物訊號之影響 30
圖1- 10裂解溫度對分析物訊號的影響 32
圖1- 11設定裂解溫度為280oC分析中油柴油中的硫、砷、鎘、汞及鉛之訊號圖 33
圖1- 12揮發溫度對分析物訊號的影響 34
圖1- 13以O2為反應氣體，改變氣體流速對分析物訊號強度及預估偵測極限之影響 36
圖1- 14以O2為反應氣體，改變Rpq值對分析物訊號強度及預估偵測極限之影響 37
圖1- 15以O2為反應氣體，改變軸場電壓對分析物訊號強度及預估偵測極限之影響 38
圖1- 16以ETV-ICP-MS分析中油柴油中的硫、砷、鎘、汞及鉛之訊號圖 49



第二章 單粒子感應耦合電漿質譜儀於銀奈米粒子及銀離子之分析
圖2-1 奈米粒子通過電漿之示意圖 58
圖2-2 單粒子感應耦合電漿質譜儀之資料處理流程圖 60
圖2-3 實驗流程圖 64
圖2- 4 以SP-ICP-MS偵測107Ag之訊號圖。(a)為分析超純水之訊號圖 (b)為分析2 ng mL-1銀離子水溶液之訊號圖 (c)為分析50 nm銀奈米粒子懸浮液之訊號圖。 66
圖2- 5 50 nm奈米粒子之粒徑分布圖 67
圖2- 6 取樣數目為4000時之粒徑分布圖 67
圖2- 7 以SP-ICP-MS分析不同粒徑奈米粒子建立之校正曲線 70
圖2- 8 以SP-ICP-MS分析不同濃度銀離子建立之校正曲線 71
圖2- 9 以SP-ICP-MS分析數目濃度奈米粒子建立之校正曲線 72
圖2- 10 以SP-ICP-MS分析數目濃度奈米粒子建立之校正曲線 73
圖2- 11 以SP-ICP-MS分析飲用水中銀奈米粒子之原始訊號圖與粒徑分佈圖 78
圖2- 12 以SP-ICP-MS分析自來水中銀奈米粒子之原始訊號圖與粒徑分佈圖 79
圖2- 13 超純水中銀奈米粒子之TEM圖 80
圖2- 14 自來水中銀奈米粒子之TEM圖 81
圖2- 15 (a)以SP-ICP-MS分析湖水中銀奈米粒子之原始訊號圖與粒徑分佈圖 82

 
表目錄
第一章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於燃油樣品中微量元素分析之應用
表1- 1 ICP-MS 系統操作條件 10
表1- 2 ETV升溫程式 12
表1- 3 微波消化步驟設定 19
表1- 4 添加Pd作為修飾劑對分析物訊號之影響 22
表1- 5 添加不同修飾劑對分析物訊號之影響 23
表1- 6 模擬基質中MoO+對分析物訊號及同位素比量測之影響 40
表1- 7 模擬基質中ArCl+對分析物訊號之影響 41
表1- 8 模擬基質中CoO+對分析物訊號之影響 42
表1- 9 水溶液校正曲線法與標準添加法斜率之比較 43
表1- 10 不同樣品標準添加法斜率之比較 45
表1- 11 使用不同方法定量柴油樣品中硫、砷、鎘、汞、鉛之濃度 46

第二章 單粒子感應耦合電漿質譜儀於銀奈米粒子及銀離子之分析
表2- 1 ICP-MS 系統操作條件 62
表2- 2 Reading數目對銀奈米粒子溶液分析結果之影響 68
表2- 3 以標準模式定量奈米粒子懸浮液 76
表2- 4 以SP-ICP-MS同時檢測銀離子與銀奈米粒子 76
表2- 5 銀奈米粒子數目濃度之檢測 76

第一章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於燃油樣品中微量元素分析之應用
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