超音波泥漿取樣法（Ultrasonic Slurry Sampler，USS）是將固體樣品直接導入電熱式揮發（Electrothermal vaporization，ETV）裝置的一種方法，目前已廣泛地結合感應耦合電漿質譜儀（ICP-MS）進行各式樣品中微量元素之分析。有別於傳統的固體樣品須經過繁瑣、耗時的前處理步驟，泥漿取樣法的直接取樣技術不僅步驟簡單快速、避免樣品於前處理時導入汙染的機會，更能夠降低易揮發物種於處理過程中損失等優點。其配合乾進樣系統ETV作為樣品輸入裝置，能夠有效地降低氧化物及氫氧化物所造成的光譜性干擾，相較於傳統氣動式霧化器而言，其具有較佳的靈敏度及分析物傳輸效率、較低的偵測極限，另外，所需的樣品量少可避免因樣品體積量少造成偵測上的限制，將其有效地與ICP-MS結合應用於微量元素分析上。
研究分為兩部分，第一部分為利用 USS-ETV-ICP-MS 同時對於道路塵土樣品中微量貴金屬－鈀、鉑、銠、金等四個元素的含量進行偵測。於研究中將對於修飾劑、泥漿樣品的配製及儀器設定等參數條件進行探討。由實驗結果得知，利用2% m/v Ammonium pyrrolidine dithiocarbamate（APDC）作為修飾劑，能夠有效地降低分析物揮發溫度，提升分析物的訊號；而泥漿樣品的配製則選擇0.5% m/v的濃度作為稀釋倍數，若泥漿樣品濃度太低，產生的訊號較小，容易造成定量上誤差，而泥漿樣品濃度太高可能會導致較大的基質效應，且易使樣品揮發不完全；儀器部分則使用裂解溫度400oC及揮發溫度2600oC作為參數條件之設定，可得到最佳的訊號，並於研究中探討可能干擾物所造成光譜干擾的程度。最後，以最適化後之分析方法對標準參考樣品－BCR 723、NIST SRM 2709和不同地區的道路塵土進行定量分析並驗證此方法之可行性。此方法對於鈀、鉑、銠、金等元素的方法偵測極限分別可達0.7、0.1、0.2、0.1 ng g-1。
第二部分則是以鈀奈米粒子（Palladium nanoparticles，Pd-NPs）作為電熱式揮發感應耦合電漿質譜法的修飾劑應用於食用油中銅、砷、汞、鉛等元素之分析。Pd-NPs是由還原試劑－Ascorbic acid和CMC（Carboxymethyl cellulose）作為保護試劑所合成的，於研究中將針對合成出來的Pd-NPs尺寸進行分析且對於修飾劑、乳濁液樣品配製和儀器設定條件等參數進行最適化探討。在實驗結果中發現使用500 ng Pd-NPs修飾劑濃度及添加50 mg L-1 Ascorbic acid做為混和基質修飾劑，可有效提升分析物訊號；乳濁液樣品配製是選擇5% m/v的食用油濃度並添加1.5% m/v界面活性劑Triton-X 100進行樣品乳化步驟，而ETV的昇溫程式選擇500oC的裂解溫度及2600oC為揮發溫度設定，於各分析條件最適化後，將此系統應用於三種市售食用油的定量分析。由於食用油並無標準參考樣品，實驗時選擇礦物油標準品（Mineral oil standard）進行分析，其定量結果與標準參考值相吻合，驗證了此分析方法的可行性。並使用標準添加法與同位素稀釋法來定量食用油樣品中各元素的濃度，並同時消化食用油樣品以氣動式霧化器進行定量並相互比較結果。此方法對於銅、砷、汞及鉛元素的方法偵測極限分別為0.2、0.1、0.8、0.2 ng mL-1。

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論文摘要……………………………………………………………………………......І
謝誌…………………………………………………………………………………...III
目錄…………………………………………………………………………………...IV
圖表目錄………………………………………..…………………………………….VI
<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道路塵土中微量貴金屬元素分析之應用
壹、 前言………………………………………………………………………………..1
一、 研究背景……………………………………………………………………..1
二、 超音波泥漿取樣法結合電熱式揮發樣品輸入系統簡介…………………..3
貳、 實驗部分
一、 儀器裝置及操作條件……………………………………………………….6
二、 試劑藥品及溶液的配製…………………………………………………...12
&#21442;、結果與討論
一、修飾劑的選擇……………………………………………………………….17
二、界面活性劑對分析物訊號的影響………………………………………….18
三、酸對分析物訊號的影響……………………………………………………..22
四、稀釋倍數的探討……………………………………………………………22
五、裂解溫度及揮發溫度的選擇……………………………………………….25
六、光譜(同質量)干擾…………………………………………………………..25
七、校正曲線……………………………………………………………………..31
八、樣品定量分析………………………………………………………………..34
肆、結論………………………………………………………………………………..36
伍、參考文獻…………………………………………………………………………..39
<第二章> 以鈀奈米粒子為修飾劑於電熱式揮發感應耦合電漿質譜法中食用油之微量元素分析應用
壹、前言……………………………………………………………………………….44
一、 研究背景……………………………………………………………………44
二、 銅、砷、汞及鉛之個論……………………………………………………47
三、 同位素稀釋法………………………………………………………………49
貳、實驗部分
一、儀器裝置及操作條件……………………………………………………….50
二、試劑藥品及溶液的配製…………………………………………………….51
&#21442;、結果與討論
一、PdNPs之鑑定………………………………………………………………..63
二、PdNPs濃度的選擇…………………………………………………………..64
三、H2O2對分析物訊號的影響………………………………………………….67
四、混合基質修飾劑的選擇……………………………………………………..67
五、添加酸的探討………………………………………………………………..71
六、添加界面活性劑濃度的探討………………………………………………..71
七、食用油樣品之稀釋倍數……………………………………………………..75
八、裂解溫度的選擇……………………………………………………………..78
九、揮發溫度的選擇……………………………………………………………..78
十、光譜(同質量)干擾…………………………………………………………...81
十一、校正曲線…………………………………………………………………85
十二、食用油樣品定量分析……………………………………………………85
肆、結論………………………………………………………………………………..93
伍、參考文獻…………………………………………………………………………..94
附錄………………………………………………………………………………..…100
圖表目錄
<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道路塵土中微量貴金屬元素分析之應用
圖1-1 超音波泥漿取樣器的設計……………………………………………………5
圖1-2 ETV-ICP-MS 系統裝置簡圖………………………………………………...8
圖1-3 ARIDUS Desolvating Sample Introduction System 之構造圖……………..11
圖1-4 泥漿樣品製備流程圖………………………………………………………..15
圖1-5 基質修飾劑APDC濃度對分析物訊號的影響……………………………..20
圖1-6 泥漿中土壤濃度對分析物訊號影響………………………………………..23
圖1-7 裂解溫度對分析物相對訊號的影響………………………………………..26
圖1-8 揮發溫度對分析物相對訊號的影響………………………………………..27
表1-1 ICP-MS 系統操作條件………………………………………………………9
表1-2 ETV昇溫程式……………………………………………………………….10
表1-3 微波消化步驟設定…………………………………………………………..16
表1-4 添加不同修飾劑對分析物訊號之影響……………………………………..19
表1-5 添加Triton X-100對分析物訊號結果比較………………………………...21
表1-6 泥漿中土壤濃度對分析物訊號結果比較…………………………………..24
表1-7 各元素於ICP-MS分析中常見多原子離子造成的同質量干擾…………...29
表1-8 比較ETV和傳統式霧化器進樣方式產生氧化物的比例…………………30
表1-9 模擬基質中多元子離子對分析物訊號及同位素比測量之影響…………..32
表1-10 模擬基質中多元子離子對分析物訊號及同位素比測量之影響…………..33
表1-11 檢量線法與標準添加法斜率之比較………………………………………..35
表1-12 不同泥漿樣品標準添加法斜率之比較……………………………………..35
表1-13 以USS-ETV-ICP-MS偵測標準參考樣品中鈀、鉑、銠及金的濃度………..37
表1-14 以USS-ETV-ICP-MS偵測道路塵土樣品中鈀、鉑、銠及金的濃度………..38
<第二章> 以鈀奈米粒子為修飾劑於電熱式揮發感應耦合電漿質譜法中食用油之微量元素分析應用
圖2-1 食用油乳濁狀樣品製備流程圖……………………………….…………….59
圖2-2 Ascorbic acid 之分子結構圖……………….………………………….……65
圖2-3 Carboxymethyl cellulose sodium salt之分子結構圖…………….……….…65
圖2-4 以DLS分析溶液中Pd-NPs粒徑分佈結果………………………….……..66
圖2-5 Pd-NPs之TEM影像圖…………………….…………………………….…66
圖2-6 以EDS分析Pd-NPs之訊號………………………………….…….……….66
圖2-7 Pd-NPs 濃度對分析物訊號的影響……………………….……….……….68
圖2-8 添加不同修飾劑濃度所得之分析物訊號圖……………….……….………69
圖2-9 H2O2濃度對分析物訊號的影響………………………………....….…...….70
圖2-10 Ascorbic acid濃度對分析物訊號的影響………………...…….….….…….73
圖2-11 HNO3濃度對分析物訊號的影響………………………………..……….…74
圖2-12 Triton X-100濃度對分析物訊號的影響…………………………..…..……76
圖2-13 裂解溫度對分析物訊號的影響………………………………………...…...79
圖2-14 揮發溫度對分析物訊號的影響…………………...……………………...…80
圖2-15 以USS-ETV-ICP-MS 偵測食用油中銅、砷、汞及鉛之訊號圖……..……92
表2-1 ICP-MS 系統操作條件……………………………………………..………54
表2-2 ETV昇溫程式………………………………………………………….……55
表2-3 各元素之同位素含量比…………………………………………………..…60
表2-4 各樣品中添加於乳濁液樣品中不同濃度之濃縮同位素濃度………..……61
表2-5 微波消化步驟設定………………………………………………..…………62
表2-6 添加不同混合修飾劑對分析物訊號結果比較……………………..………72
表2-7 泥漿樣品食用油濃度對分析物訊號結果比較……………..………………77
表2-8 各元素於ICP-MS分析中常見多原子離子造成的同質量干擾……...……82
表2-9 模擬基質中多原子離子對銅及汞訊號及同位素比測量的影響……..……83
表2-10 模擬基質中多原子離子對砷訊號的影響…………………………..………84
表2-11 檢量線法與標準添加法斜率之比較………………………………..………87
表2-12 不同樣品標準添加法斜率之比較…………………………………..………88
表2-13 市售食用油成分表…………………………………………………..………89
表2-14 以USS-ETV-ICP-MS 偵測食用油中銅、砷、汞及鉛的濃度………………90

<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道路塵土中微量貴金屬元素分析之應用
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