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研究生:向曼菁
研究生(外文):Man-Ching Hsiang
論文名稱:利用多元素石墨爐原子吸收光譜儀直接且同時測定尿液中的砷、錳、鈷和鎳元素
論文名稱(外文):Direct and Simultaneous Determination of Arsenic, Manganese, Cobalt and Nickel in Urine with a Multielement Graphite Furnace Atomic Absorption Spectrometer
指導教授:黃賢達黃賢達引用關係
指導教授(外文):Shang-Da Huang
學位類別:碩士
校院名稱:國立清華大學
系所名稱:化學系
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:2002
畢業學年度:90
語文別:中文
論文頁數:104
中文關鍵詞:微量元素石墨爐原子吸收光譜儀
外文關鍵詞:trace elementAsMnCoNiETAAS
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近年來,微量元素研究被認為是關係到人類健康和長壽的一個充滿希望的新領域,已引起國內外醫學界和營養界的普遍重視。本研究以微量分析化學的方法,利用多元素石墨爐原子吸收光譜儀發展尿液中微量元素的分析技術,達成同時及快速多元素分析之目標。
本研究使用多元素石墨爐原子吸收光譜儀,直接且同時測定尿液中的砷、錳、鈷和鎳元素,由於尿液中蛋白質及無機鹽類會對直接測量產生干擾,因此先將尿液用去離子水作1:1的稀釋,且四種元素在尿液中的含量均低,故添加適當的鈀修飾劑,並尋找儀器最佳化設定。本分析方法為使用單純的去離子水(含0.2%HNO3)校正曲線,成功地定量標準尿液中的砷、錳、鈷和鎳元素,測定值均可落在認證值的85%-115%。
本方法應用於人體真實尿液的分析,不論高、低濃度之回收率均在100±20%之內。此外,砷、錳、鈷和鎳元素的偵測極限,在灰化溫度1350℃,原子化溫度2100℃時,分別為0.78ppb,0.054ppb,0.22ppb及0.35ppb;而在原子化溫度為2150℃時,四元素之偵測極限分別為0.71ppb,0.064ppb,0.36ppb及0.39ppb,相對標準偏差都小於5%。

A simple method was developed for the direct and simultaneous determination of arsenic, manganese, cobalt, and nickel in urine by a multi-element graphite furnace atomic absorption spectrometer (Perkin-Elmer SIMAA 6000). Pd was used as the chemical modifier along with a special purge gas (5% H2+95% Ar) and a two-step ashing process. The matrix interferences were removed effectively so that a simple calibration curve method could be used (with 1:1 dilution). A standard reference material (Seronorm Trace Elements Urine) was used to find the optimal temperature program and to confirm the accuracy of the technique. The analyzed values for all these elements were within 85%-115% of certified values. The recovery (using the real urine samples) were within 80%-120% for four elements. With the ashing temperature at 1350℃, and the atomization temperature at 2100℃, the detection limits were 0.78 µg l-1 for As, 0.054 µg l-1 for Mn, 0.22 µg l-1 for Co, and 0.35 µg l-1 for Ni. The relative standard deviations (RSDs) was lower than 5%.

第一章 前言…………………………………………………….. 1
1.1 生物體中的元素和組成……………………………………… 1
1.2 人體中微量元素之功能與危害………………………….... 2
1.2.1 砷(As)…………………………………………………... 3
1.2.2 錳(Mn)…………………………………………………... 4
1.2.3 鈷(Co)…………………………………………………... 6
1.2.4 鎳(Ni)………………………………………………..... 7
1.3 尿液體中微量元素分析方法之回顧與探討………………… 7
1.4 多元素原子吸收光譜儀之發展與簡介……………………… 13
1.4.1 溫控程式(Temperature program)…………………….. 18
1.4.2 溫度穩定化平台爐概念(STPF concept)……………... 20
1.5 化學修飾劑之功能………………………………………….. 23
1.5.1 鈀修飾劑的應用…………………………………………. 25
1.5.2 鎂修飾劑的應用…………………………………………. 26
1.5.3 氫氣的使用………………………………………………. 27
1.6 研究目的……………………………………………………. 28
第二章 實驗………………………………………………….. 29
2.1 儀器與裝置………………………………………………... 29
2.2 試劑………………………………………………………… 30
2.3 真實尿液樣品之收集與儲存……………………………… 30
2.4 Muromac A-1的特性與管柱製備……………………….... 31
2.5 空白尿液的製備……………………………………………. 32
2.6 鈀修飾劑的製備……………………………………………. 32
2.7 污染控制……………………………………………………. 32
第三章 結果與討論…………………………………………….. 34
3.1最佳溫控程式的尋找………………………………......... 34
3.1.1 灰化溫度…………………………………………………. 34
3.1.2 原子化溫度………………………………………………. 36
3. 2 最佳修飾劑用量的選擇………………………………….. 37
3. 3 標準尿液分析………………………………………….... 38
3.3.1 不同溫度條件的結果……………………………………. 38
3.3.2 二段式灰化步驟…………………………………………. 39
3.3.3 最佳溫控程式……………………………………………. 41
3. 4 不同方法的比較……………………………………….... 42
3. 5 真實尿液的分析……………………………………….... 42
3. 6 偵測極限與精密度……………………………………….. 44
第四章 結論…………………………………………………….. 45
參考文獻………………………………………………………….. 47

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