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研究生:黃仕一
研究生(外文):Shih-Yi Hu
論文名稱:泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於穀物樣品中微量元素之分析應用
指導教授:江旭禎江旭禎引用關係
口試委員:眭台生曾韋龍
口試日期:2009-07-21
學位類別:碩士
校院名稱:國立中山大學
系所名稱:化學系研究所
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:2009
畢業學年度:96
語文別:中文
論文頁數:141
中文關鍵詞:電熱式揮發微量元素動態反應室感應耦合電漿質譜儀穀物
外文關鍵詞:trace elementsETVSeAsZnCuFeCrICP-MSDRCcereals
相關次數:
  • 被引用被引用:4
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  • 下載下載:24
  • 收藏至我的研究室書目清單書目收藏:0
本研究是以電熱式揮發感應耦合電漿質譜儀(ETV-ICP-MS,Electrothermal Vaporization Inductively Coupled Plasma Mass Spectrometry)偵測穀物樣品中之微量元素,以ETV作為樣品輸入裝置時,具有樣品傳輸效率佳、所需樣品體積少等優點,並利用其昇溫程式可有效地降低氧化物與氫氧化物所造成的干擾;再配合超音波泥漿取樣法(USS,Ultrasonic Slurry Sampling)的使用,可減少樣品前處理的過程,因而可降低在前處理過程中汙染物的導入。
研究分為兩個部分,第一部分為利用泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀(USS-ETV-ICP-MS)測定穀物樣品中鉻、鐵、銅、鋅、砷及硒等元素的含量,並配合動態反應室(DRC,Dynamic Reaction Cell)的使用,以降低因基質或輸送氣體所造成的光譜干擾。研究中對修飾劑、DRC系統的條件、泥漿樣品的配製及儀器的設定條件等因素進行探討。由實驗結果發現,以thioacetamide(TAC)當作修飾劑時可以有效提升分析物的訊號;在DRC系統中,選擇以甲烷當作反應氣體來減輕實驗中因樣品基質及輸送氣體所產生的光譜干擾。分析條件最適化後,將選擇對NIST SRM 1567a、NIST SRM 1568a及市售麵粉及米樣品進行定量分析,並比對不同分析方法之定量結果,驗證以USS- ETV- ICP-MS分析穀物樣品中鉻、鐵、銅、鋅、砷及硒的可行性。此方法對鉻、鐵、銅、鋅、砷及硒的方法偵測極限分別為1.3、18、4.0、12、2.0及2.1 ng g-1。
第二部分則是使用USS-ETV-ICP-MS對穀物樣品中更多微量元素(釩、鉻、鈷、鎳、銅、鋅、硒、鎘、汞及鉛)的同時分析。在實驗中使用8-HQ(8-hydroxyquinoline-5-sulfonic acid)、Triton X-100及較低的揮發溫度(1900℃),使得分析物在泥漿與水溶液中具有相似的靈敏度,因此可使用水溶液校正曲線法定量,比起傳統以標準添加法定量,可減少樣品配製及分析時所需的時間。在各分析條件最適化後,將分析物分成兩組,一組為無干擾或利用ETV之昇溫程式即可將其干擾去除之元素(即釩、鈷、鎳、鎘、汞及鉛)是於標準模式下偵測;另一組為需要以DRC系統去除干擾之元素(即鉻、銅、鋅及硒)是於DRC模式下偵測。最後,將此系統應用於穀物樣品的定量,對測定釩、鉻、鈷、鎳、銅、鋅、硒、鎘、汞及鉛的方法偵測極限分別為1.3、2.1、3.6、4.3、6.8、16、1.7、0.6、0.8及2.6 ng g-1。
論文提要................................................................................................... I
謝誌..........................................................................................................III
目錄..........................................................................................................IV
圖表目錄.................................................................................................VII
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穀物樣 品中鉻、鐵、銅、鋅、砷及硒等元素之分析應用
壹、前言 .............................................................................................. 1
一、研究背景 ............................................................................... 1
二、鉻、鐵、銅、鋅、砷及硒之個論....................................... 5
三、超音波泥漿取樣法結合電熱式揮發樣品輸入系統簡介 .. 7
四、動態反應室(DRC)系統簡介 ........................................ 10
五、同位素稀釋法 ..................................................................... 13
貳、實驗部分 .................................................................................... 16
一、儀器裝置及操作條件 ......................................................... 16
二、試劑藥品及溶液的配製 ..................................................... 22
三、泥漿樣品的製備與消化 ..................................................... 27
參、結果與討論 ................................................................................ 29
一、修飾劑的選擇 ..................................................................... 29
二、DRC系統之最佳化 ........................................................... 38
三、酸對分析物訊號的影響 ..................................................... 44
四、稀釋倍數的探討 ................................................................. 47
五、界面活性劑對分析物訊號的影響..................................... 49
六、熱解溫度(Pyrolysis Temperature)及揮發溫度 (Vaporization Temperature)的選擇 .............................. 49
七、光譜(同質量)干擾 ......................................................... 52
八、校正曲線 ............................................................................. 56
九、樣品定量分析 ..................................................................... 59
肆、結論 ............................................................................................ 68
伍、參考文獻 .................................................................................... 69
第二章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀以水溶液 檢量線法定量穀物樣品中微量元素之分析應用
壹、前言 ............................................................................................ 81
一、研究背景 ............................................................................. 81
二、釩、鈷、鎳、鎘、汞及鉛之個論..................................... 83
貳、實驗部分 .................................................................................... 86
一、儀器裝置及操作條件 ......................................................... 86
二、試劑藥品及溶液的配製 ..................................................... 90
三、水溶液標準品與泥漿樣品靈敏度的比較 ........................ 92
四、水溶液校正曲線及泥漿樣品的製備與消化 .................... 94
參、結果與討論 ................................................................................ 98
一、修飾劑的選擇 ..................................................................... 98
二、界面活性劑對分析物訊號的影響................................... 103
三、酸與鹼對分析物訊號的影響 ........................................... 105
四、揮發溫度(Vaporization Temperature)的選擇 ............ 108
五、稀釋倍數的探討 ............................................................... 113
六、光譜(同質量)干擾 ....................................................... 113
七、樣品定量分析 ................................................................... 118
肆、結論 .......................................................................................... 125
伍、參考文獻 .................................................................................. 126
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75.黎伯謙 "泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於米及塑膠樣品中微量元素分析之應用", 中山大學碩士論文, 民國92年6月.
76.曾彥傑 "泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於土壤及生物樣品中微量元素分析之應用", 中山大學碩士論文, 民國95年7月.
77.陳淑楓 "泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於魚肉和土壤樣品中微量元素分析之應用", 中山大學碩士論文, 民國87年7月.
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79.Coedo, A. G.; Dorado, T.; Padilla, I.; Maibusch, R.; Kuss, H. M., Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for steelmaking flue dust analysis. Spectrochim. Acta B 2000, 55 (2), 185-196.
80.蔡育端 "動力反應室感應耦合電漿質譜儀於水樣品中砷與硒之物種分析及魚肉樣品中微量元素分析之應用", 中山大學碩士論文, 民國92年7月.
81.何巧瑜 "泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於奶粉及土壤樣品中微量元素分析之應用", 中山大學碩士論文, 民國91年6月.
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6. 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於米及塑膠樣品中微量元素分析之應用
7. 動力反應室感應偶合電漿質譜儀於土壤及沉積土中鍺、砷及硒元素分析之應用
8. 雷射剝蝕取樣法結合感應偶合電漿質譜儀於泥土及沉積土樣品中微量元素分析之研究
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12. ㄧ、毛細管電泳結合感應耦合電漿質譜儀於砷及硒物種分析之應用二、液相層析結合感應耦合電漿質譜儀於鉈物種分析之應用
13. 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於奶粉及土壤樣品中微量元素分析之應用
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