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博碩士論文 etd-0710101-220715 詳細資訊
Title page for etd-0710101-220715
論文名稱
Title
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
none
系所名稱
Department
畢業學年期
Year, semester
語文別
Language
學位類別
Degree
頁數
Number of pages
107
研究生
Author
指導教授
Advisor
召集委員
Convenor
口試委員
Advisory Committee
口試日期
Date of Exam
2001-07-05
繳交日期
Date of Submission
2001-07-10
關鍵字
Keywords
超音波泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀、化妝品、奶粉
ICP-MS, DRC, facepowder, ETV, Milk
統計
Statistics
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The thesis/dissertation has been browsed 5630 times, has been downloaded 6478 times.
中文摘要
感應偶合電漿質譜儀(Inductively Coupled Plasma Mass spectrometry,ICP-MS)是一種微量多元素分析及同位素分析技術,它結合了ICP原子化及游離化的特性,以及質譜儀的高靈敏度和測定同位素比的能力。本方法已成功地應用於許多不同種類樣品的分析,但ICP-MS分析仍須面對光譜性干擾(質量重疊干擾)和非光譜性干擾(基質效應)之問題。本研究使用不同進樣方法並配合最適化的操作條件,以期能來偵測化妝品及奶粉中有興趣元素之濃度。
本研究主要分為兩部分,第一部份為利用超音波泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀(Ultrasonic Slurry Sampler - Electrothermal Vaporization system - ICP-MS)直接測定化妝品樣品中砷、鎘、汞及鉛之含量,建立固體樣品的直接分析方法。超音波泥漿取樣法(USS)是一種將固體樣品導入電熱式揮發器(ETV)的方法,已廣泛且成功地使用在ICP-MS上,相較於傳統固體樣品需經酸消化再進行分析,泥漿取樣法的直接取樣分析有簡化樣品前處理的繁雜過程,避免於樣品前處理過程中導入污染物及降低易揮發分析物種在消化時之損失等優點,再配合ETV樣品輸入裝置,有樣品傳輸效率佳,所需體積少(<100μL)的優點。而本研究過程中,可能會遭遇到樣品不完全揮發而殘留於揮發器內或分析物濃度差異大及基質太過複雜等問題,因此將針對ETV操作變數、樣品製備及基質修飾劑等條件進行探討,來解決上述問題。最後,分別使用標準添加法及同位素稀釋法來定量測定樣品中的分析元素。
第二部份是以動力反應室結合感應偶合電漿質譜儀(ICP-Dynamic Reaction Cell-MS)偵測奶粉中Ca、Fe、Zn分析之應用,由於ICP-DRC-MS是利用分析物與干擾離子之間和反應氣體有不同的化學反應,來降低光譜性干擾的問題;本研究中40Ca、56Fe、64Zn主要有40Ar、40Ar16O、40Ca16O、32S16O16O等質量重疊干擾,而奶粉中存有大量的Ca及S,因此同時偵測40Ca、56Fe、64Zn是相當困難的,研究中將再藉由使用去除溶劑進樣系統(ARIDUS Desolvating Sample Introduction System)以減少氧化物(MO+、XO+)的形成,來避免質量重疊的干擾,以期能建立同時偵測奶粉中40Ca、56Fe、64Zn之方法。實驗中將分別探討ARIDUS Desolvating Sample Introduction System變數及DRC系統各個變數對分析物及分析物的影響,最後將對市售奶粉樣品中的Ca、Fe、Zn元素進行分析。

Abstract
none
目次 Table of Contents
論文摘要--------------------------------------------------------------------------------Ⅰ
謝誌--------------------------------------------------------------------------------------Ⅱ
目錄--------------------------------------------------------------------------------------Ⅲ
圖表目錄--------------------------------------------------------------------------------Ⅵ

第一章 感應偶合電漿質譜儀簡介-------------------------------------------------1
壹、前言-------------------------------------------------------------------------------- 2
貳、基本原理-------------------------------------------------------------------------- 3
參、功能與限制----------------------------------------------------------------------- 6
一、光譜性干擾-------------------------------------------------------------------- 8
二、非光譜性干擾---------------------------------------------------------------- 9
肆、應用-------------------------------------------------------------------------------- 11
一、同位素測量--------------------------------------------------------------------11
二、元素分析---------------------------------------------------------------------- 13
伍、參考資料------------------------------------------------------------------------- 14

第二章 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於土壤樣品 中鋅、鎘、鉈及鉛等元素之分析應用---------------------------------16
壹、前 言------------------------------------------------------------------------------17
一、元素的毒性及對人體的危害---------------------------------------------- 18
貳、實 驗 部 份---------------------------------------------------------------------21
一、儀器裝置及操作條件------------------------------------------------------- 21
二、試劑藥品及溶液的配置---------------------------------------------------- 29
參、土 壤 樣 品 泥 漿 製 備---------------------------------------------------33
肆、結 果 與 討 論---------------------------------------------------------------- -36
一、修飾劑的選擇----------------------------------------------------------------36
二、泥漿製備之變數對分析物訊號的影響----------------------------------43
三、熱解溫度及揮發溫度的選擇----------------------------------------------48
四、光譜(同質量)干擾-------------------------------------------------------- 51
五、樣品定量分析----------------------------------------------------------------55
伍、結 論----------------------------------------------------------------------------- 59
陸、參 考 資 料-------------------------------------------------------------------- 60

第三章 動力反應室結合感應偶合電漿質譜儀偵測奶粉中Ca、Fe、Zn分析之應用-----------------------------------------------------------------------------------64
壹、前 言------------------------------------------------------------------------------65
貳、Dynamic Reaction Cell的原理------------------------------------------------68
參、實驗部份--------------------------------------------------------------------------70

一、儀器裝置-----------------------------------------------------------------------70
二、試劑藥品及溶液的配置-----------------------------------------------------73
三、實驗過程----------------------------------------------------------------------- 74
肆、結 果 與 討 論----------------------------------------------------------------- 76
一、ARIDUS(去溶劑進樣系統)操作條件的作適化-------------------- 76
二、DRC系統之最佳化----------------------------------------------------------86
三、校正曲線與偵測極限的估計----------------------------------------------101
四、真實樣品的分析-------------------------------------------------------------101
伍、結 論---------------------------------------------------------------------------- 105
陸、參 考 資 料------------------------------------------------------------------- 106

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