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研究生:蕭柏鎧
研究生(外文):Po-kai Hsiao
論文名稱:感應耦合電漿質譜儀於矽粉末中硼、磷及微量元素分析之應用
指導教授:江旭禎江旭禎引用關係
指導教授(外文):Shiuh-Jen Jiang
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:2010
畢業學年度:98
語文別:中文
論文頁數:127
中文關鍵詞:去除溶劑電熱式揮發感應耦合電漿質譜儀
外文關鍵詞:ETVdesolvatingsiliconboronICP-MSphosphorus
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感應耦合電漿質譜儀(Inductively Coupled Plasma Mass Spectrometry,ICP-MS)結合了 ICP 原子化及游離化效率高之特性以及質譜儀高靈敏度和可測定同位素比的能力,使其成為極佳之微量多元素分析技術。然而在 ICP-MS 之分析上仍會遭遇光譜性及非光譜性干擾之問題,在本研究中將嘗試使用不同樣品前處理方式及搭配不同樣品輸入裝置,期望能降低分析上之干擾,以對太陽能級(Solar grade)矽粉末中硼、磷及微量不純物的分析,提供一簡單、快速及準確之方法。
研究分為兩個部分,第一部分以感應耦合電漿質譜儀結合配備去除溶劑系統的微同心圓氣動式霧化器(ARIDUS-I desolvating sample introduction system)為進樣裝置,測定矽粉末樣品中硼、鋁、磷、鈦、鐵及銅的含量。在樣品前處理部分,採用硝酸及氫氟酸混合酸於室溫下將樣品完全消化,並在消化過程前,於0.1 g矽粉末樣品中先加入500 μg mannitol,以避免硼於樣品消化過程之揮發損失。研究中依序探討樣品溶解方法、硼與磷之偵測以及 ARIDUS-I操作條件對離子訊號的影響。實驗結果證明,在最適化條件下,ARIDUS-I能有效去除氟化矽及溶劑,降低矽基質及氧化物造成之光譜性干擾。最後將開發之方法應用於矽粉末樣品中硼、鋁、磷、鈦、鐵及銅的分析,並和工研院材化所提供之GD-MS參考值做比較。添加回收率在94-107%之間,硼、鋁、磷、鈦、鐵及銅之方法偵測極限分別為0.032、0.067、0.13、0.0038、1.0 and 0.0024 μg g-1。此分析方法簡單快速,適用於矽粉末樣品中微量元素的例行分析。
第二部分研究則以超音波泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀(Ultrasonic Slurry Sampling - Electrothermal Vaporization Inductively Coupled Plasma Mass Spectrometry,USS-ETV-ICP-MS)測定矽粉末樣品中硼、鋁、磷、鐵、鎳、銅、鋅、鎘及鉛元素的濃度,以建立直接分析固體樣品的方法。在樣品前處理部分,直接將矽粉末配製成泥漿樣品,再以超音波泥漿取樣法(USS)將其導入電熱式揮發器(ETV),相較於傳統矽粉末樣品需先經酸消化溶解後再進行分析,具有簡化樣品前處理步驟,避免樣品前處理過程導入污染,以及降低易揮發元素如硼…等在酸消化過程中損失之優點。ETV樣品輸入裝置則採用低溫揮發的方式,藉由分析物與矽基質之不同揮發行為,期望能減輕矽基質所造成之光譜性干擾。研究中對修飾劑的選擇、泥漿樣品的配製、儀器設定條件及基質干擾等因素進行探討。由實驗結果發現以citric acid作為修飾劑有助於提升分析物離子訊號,並將ETV揮發溫度設定為1900℃時,能有效減輕矽基質所造成之多原子離子干擾。最後將最適化條件應用於數個矽粉末樣品之分析,並比對不同分析方法的定量結果以進一步驗證開發方法之可行性。
目 錄
論文提要 I
謝誌 IV
目錄 V
圖表目錄 VIII

第一章 感應耦合電漿質譜儀結合去除溶劑進樣裝置於矽粉末樣品中硼、鋁、磷、鈦、鐵及銅之分析應用
壹、前言 1
貳、實驗部份 7
一、 儀器裝置及操作條件 7
二、 試劑藥品12
三、 標準品及所需溶液之配製13
四、 樣品配製14
參、結果與討論 18
一、 樣品前處理方法之比較18
二、 硼之偵測探討20
三、 磷之偵測探討21
四、 ARIDUS 去溶劑進樣系統操作條件最適化探討27
五、 校正曲線與偵測極限的估計45
六、 矽樣品之分析47
肆、結論 53
伍、參考文獻54

第二章 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於矽粉末樣品中硼、鋁、磷、鐵、鎳、銅、鋅、鎘及鉛之分析應用
壹、前言 59
貳、實驗部份 63
一、 儀器裝置及操作條件63
二、 試劑藥品及溶液的配製69
三、 矽粉末泥漿樣品之製備與消化72
參、結果與討論 76
一、 修飾劑的選擇76
二、 泥漿樣品稀釋倍數對分析物訊號的影響81
三、 酸的濃度對分析物訊號的影響83
四、 界面活性劑對分析物訊號的影響86
五、 熱解溫度及揮發溫度的選擇88
六、 DRC 系統之探討91
七、 光譜(同質量)干擾之探討96
八、 樣品定量分析102
肆、結論 107
伍、參考文獻 108
第一章
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第二章
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1. 微波輔助產生揮發性基質化合物結合感應偶合電漿質譜儀於硒及鍺粉末和矽及石英中微量不純物分析之應用
2. 動力反應室感應偶合電漿質譜儀於水樣中砷與硒之物種分析以及魚肉樣品中微量元素分析之應用
3. 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於土壤與油漆樣品中微量元素分析之應用
4. 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
5. 以溶膠-凝膠法製備磷/矽之有機-無機奈米複合材料及其難燃性與熱性質之研究
6. 泥漿取樣法結合電熱式揮發原子光譜儀於魚肉及食用油樣品中微量元素分析之應用
7. 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
8. 感應偶合電漿質譜儀於化妝品及奶粉樣品中元素分析之應用
9. 含磷及含矽熱可塑性聚氨基甲酸酯之合成與特性
10. 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於藥錠及中草藥中微量元素分析之應用
11. 微波輔助霧點萃取法結合動態反應管感應耦合電漿質譜儀於水樣中微量鉻、銅、鎘及鉛分析之應用
12. 一、雷射剝蝕結合感應耦合電漿質譜儀分析鋼鐵中輕元素之應用;二、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
13. 新穎自熄性有機/無機環氧樹脂奈米複合材料之合成與性質研究
14. 含磷/矽雙環戊二烯高分子的製備及其難燃特性之探討
15. 核心層光電子激發術對化學氣相沈積法在Si(111)-7x7與Ge(100)-2x1表面上成長磷薄膜現象的研究
 
1. 泥漿取樣法結合電熱式揮發感應耦合電漿質譜儀於藥錠及中草藥中微量元素分析之應用
2. 流動注入化學蒸氣生成技術結合感應耦合電漿質譜儀於土壤中銅、鋅、鎘及中草藥中砷、汞、鉛分析之應用
3. 液相層析結合感應耦合電漿質譜儀於環境樣品中鉈及食用油中砷物種分析之應用
4. 感應耦合電漿質譜儀於食品中多重微量元素與鉻、砷及硒物種型態分析之應用
5. 微波輔助霧點萃取法結合動態反應管感應耦合電漿質譜儀於水樣中微量鉻、銅、鎘及鉛分析之應用
6. 開發雷射剝蝕感應耦合電漿質譜直測技術進行生物樣品及半導體材料中微量元素分析之研究
7. 液相層析結合感應耦合電漿質譜儀於環境樣品中鉻與硒及穀物樣品中砷與硒型態分析之應用
8. 一、雷射剝蝕結合感應耦合電漿質譜儀分析鋼鐵中輕元素之應用;二、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
9. 感應偶合電漿質譜儀於魚肉樣品中微量元素及砷物種分析之應用
10. 動態反應管感應偶合電漿質譜儀於鋼鐵樣品中硼、矽、硫及磷與食品樣品中鈣及磷之分析應用
11. 微波輔助產生揮發性基質化合物結合感應偶合電漿質譜儀於硒及鍺粉末和矽及石英中微量不純物分析之應用
12. 液相層析結合感應耦合電漿質譜儀與電灑質譜儀於營養補給品中含硒化合物與藍綠藻中含砷化合物之分析應用
13. 液相層析法結合動態反應管感應偶合電漿質譜儀於環境及生物樣品中鉻、釩、硒及碲物種分析之應用
14. 液相層析結合感應偶合電漿質譜儀於銻、鉈、砷與硒分析之應用
15. 氫化物生成技術結合動態反應管感應偶合電漿質譜儀在生物及鎳合金樣品中鎵,鍺,砷,硒,銻之分析
 
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