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研究生:郭武居
研究生(外文):Wu-Chu Guo
論文名稱:塑膠材料中重金屬含量之測定
論文名稱(外文):Determination of Heavy Metal in Plastic Materials
指導教授:鄭國忠鄭國忠引用關係
口試委員:陳炎輝蔡德華郭文正
口試日期:2007-06-22
學位類別:碩士
校院名稱:國立臺北科技大學
系所名稱:化學工程研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2007
畢業學年度:95
語文別:中文
論文頁數:117
中文關鍵詞:塑膠材料微波消化重金屬感應耦合電漿發射光譜儀
外文關鍵詞:plastic materialsmicrowave digestionheavy metalICP-OES
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本研究以建立塑膠材料之重金屬檢測方法為目的,利用微波輔助加熱方式快速消化高密度聚乙烯塑膠,並以感應耦合電漿發射光譜儀分析鉛、鎘、汞及鉻四種重金屬元素。
首先,探討密閉微波消化方法之最適操作條件;其次分析高密度聚乙烯塑膠標準參考樣品BCR 680,評估方法的準確性;最後以建立之微波消化程序分析高密度聚乙烯之真實樣品,以探討方法之適用性及可能的影響。在微波消化試劑方面,只使用硝酸,發現可得到具有可信賴的結果。希望藉此研究成果能提供一快速、準確、靈敏之塑膠材料中重金屬分析方法。
研究結果顯示,取樣品0.2 g加入10mL之65%硝酸,以密閉微波消化法之較佳操作條件為,微波升溫時間3分鐘、微波消化溫度160 ℃、微波消化時間15分鐘。最後使用感應耦合電漿發射光譜儀(ICP-OES),來分析高密度聚乙烯塑膠消化液中微量元素鎘、鉻、汞、鉛的含量,可同時定量出重金屬鎘、鉻、汞、鉛的含量,並獲得良好的精準度。本研究經由添加標準品分析的方式,高密度聚乙烯塑膠樣品中鎘、鉻、汞及鉛的添加標準品分析之回收率分別在98.9~104.6%、98.6~101.8%、99.8~103.8%、99.1~103.2%的範圍內,對於真實樣品的測定,可得良好回收率,未發現有基質干擾的情形。本研究建立之模式,可提供進行微波消化不同基質之塑膠樣品測定其重金屬含量之參考方法。
The purpose of this research is to develop a rapid determination method for heavy metals (Pb、Cd、Hg、Cr) in high density polyethylene(HDPE).
Firstly, the microwave operation parameters (including sample amount, adding oxidizing reagent—HNO3, digestion temperature, and digestion time) were optimized. The standard reference materials (BCR 680) were then analyzed to assess the accuracy of the developed method. In the digestion, we only use the HNO3, without the HF. Heavy metals were quantitated by ICP-OES methods. We get a good and reliable data. The results were in good agreement with certified reference material (BCR 680), and successfully applied to the determination of cadmium, chromium, mercury and lead in plastic materials.
In this thesis, an amount (0.2 g) of HDPE sample was placed in a teflon vessel. One-stages of microwave digestion (10 mL of nitric acid) was performed at 160℃ for 15 min. Matrix spike studies were done on cadmium, chromium, mercury and lead in HDPE. The matrix spike recovery results are 98.9%~104.6%,98.6%~101.8%,99.8%~103.8% and 99.1%~103.2%, respectively, indicating that the matrix does not have major interfering capacity.
中文摘要 i
英文摘要 ii
誌謝 iii
目錄 iv
表目錄 vi
圖目錄 viii
第一章 緒論 1
1.1 前言 1
1.2 研究動機與背景 5
1.3 研究目的 11
第二章 文獻回顧 12
2.1 認識微波 12
2.2 微波加熱的原理 13
2.3 微波與化學研究相關的應用 17
2.4 消化前處理方法 17
2.5 密閉式微波系統 18
2.6 高密度聚乙烯中重金屬分析方法 19
2.6.1 檢測塑膠中的重金屬常使用的前處理方法 20
2.6.1.1 BS EN 1122方法概要 21
2.6.1.2 U.S.EPA SW 846-Method 3050B方法概要 23
2.6.1.3塑膠類食品器具、容器、包裝重金含量方法概要 25
2.6.1.4 U.S.EPA SW 846-Method 3052方法概要 25
2.6.2塑膠樣品的消化 25
2.6.2.1微波消化法之影響因子 25
第三章 實驗藥品及儀器設備與實驗方法 31
3.1實驗藥品及試劑一般藥品及試劑 31
3.1.1一般藥品及試劑 31
3.1.2重金屬標準品及標準參考樣品 31
3.2實驗儀器 32
3.3塑膠樣品微波消化 32
3.3.1消化試劑的選擇 33
3.3.2不同消化條件的消化效果 34
3.3.2.1消化持續時間對消化效率之影響 34
3.3.2.2消化溫度對消化效率之影響 35
3.3.2.3樣品重量對消化效率之影響 35
3.3.3微波消化條件 35
3.4 感應耦合電漿發射光譜儀上機分析 38
3.4.1 ICP-OES分析條件及儀器設定參數 38
3.4.2 檢量線配製 39
3.5 真實樣品的檢測 40
3.5.1樣品研磨 40
3.5.2樣品消化及分析 40
3.5.3品質管制 41
3.5.3.1方法偵測極限(method detection limit, MDL)測定 41
3.5.3.2檢量線(Calibration Curve)製作 42
3.5.3.3 檢量線確認(Calibration verification) 43
3.5.3.4 空白(Blank)樣品分析 43
3.5.3.5 品管查核樣品(Quality check sample)分析 44
3.5.3.6 重複(Duplicate analysis)樣品分析 44
3.5.3.7 添加(Spike analysis)標準品分析 45
第四章 結果與討論 46
4.1高密度聚乙烯之微波消化條件 46
4.1.1 微波消化時間之探討 46
4.1.2 微波消化溫度之探討 47
4.1.3 微波消化樣品量之探討 48
4.2高密度聚乙烯真實樣品檢測分析 67
4.2.1方法偵測極限檢測結果 67
4.2.2 檢量線檢測結果 67
4.2.3 空白試驗結果 67
4.2.4 品管查核樣品分析結果 67
4.2.5 重複樣品分析結果 68
4.2.6 添加標準品分析結果 68
4.3 微波消化和加熱板消化的比較 68
第五章 結論 83
5.1結論 83
5.2建議 83
參考文獻 84
附 錄 89
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