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研究生:黃式揚
研究生(外文):Shih-Yang Huang
論文名稱:Ⅰ.以開放式聚焦微波消化器配合分光光度計偵測廢水中化學需氧量之研究Ⅱ.以微波法處理土壤中多苯環芳香烴之初步研究
論文名稱(外文):A Study on the Determination of the Chemical Oxygen Demand in Wastewaters Using Open Focus Microwave Digestor Coupled with Spectrophotometry
指導教授:許道平
指導教授(外文):Tau-Being Hsu
學位類別:碩士
校院名稱:淡江大學
系所名稱:水資源及環境工程學系
學門:工程學門
學類:環境工程學類
論文種類:學術論文
論文出版年:1999
畢業學年度:87
語文別:中文
論文頁數:171
中文關鍵詞:化學需氧量微波消化消化液分光光度計流動注入分析
外文關鍵詞:chemical oxygen demand(COD)microwave dugestiondigest reagentspectrophotometryflow injection analysis
相關次數:
  • 被引用被引用:0
  • 點閱點閱:321
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  • 下載下載:0
  • 收藏至我的研究室書目清單書目收藏:0
論文提要內容:
Ⅰ.以開放式聚焦微波消化法配合分光光度計偵測廢水中化學需氧量之研究
傳統偵測水中化學需氧量的方法,主要是以重鉻酸鉀迴流法加熱2小時,再以滴定方式滴定殘餘之重鉻酸鉀,其過程不僅耗時且廢液量多。本研究之目的是以開放式聚焦微波消化水樣,再以分光光度計偵測化學需氧量。進而研究以流動注入分析法,將微波消化後之樣品注入分光光度計內直接偵測。
本研究利用直交表中四個因子實驗設計探求微波最佳化條件,選取微波功率、微波時間、水樣/消化液(v/v)比及硫酸銀試劑量為四個因子。結果顯示初步微波條件:(1)微波功率:90W,(2)微波時間:2分鐘,(3)水樣/消化液(v/v)比:2.5/1.5,(4)硫酸銀試劑量:3.0ml。
初步微波條件對於鄰苯二甲酸氫鉀標準品之回收率不錯,但品管樣品之回收率不高。故調整微波功率為300W(最佳微波條件),對於品管樣品之平均回收率即可達到98.9%。以最佳微波條件分析不同來源真實水樣,水樣中氯鹽濃度1000mg/l以下,化學需氧量500mg/l以下時,其效果較好。微波消化後之水樣,以流動注入法注入分析,亦可得到不錯之測值,對於染整業廢水、造紙業廢水及垃圾滲出水,其平均回收率皆可達90.3%以上。
Ⅱ.以微波法處理土壤中多苯環芳香烴之初步研究
以微波方式處理土壤中之有機物,具有設備簡單、操作容易等優點。本研究之目的為以微波法處理固態樣品中之有機污染物,然後以微波萃取殘餘之有機污染物進入氣相層析儀中分析。其處理流程為添加Cu2O及NaOH溶液於裝有已添加芘(pyrene)固態樣品之微波容器中上,再以微波照射以分解有機污染物。
初步以金剛砂添加芘(20μg/g)作為模擬樣品,添加藥劑微波處理後,再以微波萃取裝置萃取得到殘餘芘含量。均質化模擬樣品(金剛砂中添加芘20μg/g)由微波萃取裝置MES 1000萃取後,經由F test及t test證實均質化效果良好。微波處理方面,使用家用微波爐713.6W、微波時間40分、Cu2O 0.3g、NaOH 10N 0.1ml及5ml水之條件下,於固相樣品中芘之平均去除率可達92.7%。

Ⅰ.A Study on the Determination of the Chemical Oxygen Demand in Wasterwaters Using Open Focus Microwave Digestor Coupled with Spectrophotometry
The traditional method for the determination of Chemical Oxygen Demand (COD) in wastewaters is mainly to digest the organics by open reflux method and then to titrate the residual Potassium dichromate by ferrous ammonium sulfate. This process not only is time-consuming but also requires a large amount of reagent. Therefore, the goals of this study are to digest the organics in wastewaters using open focus microwave digestor and then to determine the COD values by spectrophotometry.
The four factors of mix-level orthogonal array design were used in this study to search the best condition for microwave diges-tion . Those four factors were microwave power, digestion time, sample/digestion reagent ratio, Ag2SO4 volume. The results were showed that the optimized digestion conditions were(1) microwave
power: 90W, (2)digestion time: 2 mins, (3) sample/digestion reagent ratio: 2.5/1.5 (v/v), (4) Ag2SO4 solution volume: 3.0mL.
In the beginning,the recovery of COD using potassium biphthalate(KHP) as standard were good by the microwave digestion , but poor for COD quality control sample. Therefore, the power of microwave was changed from 90W to 300W. For QC sample, average recovery was increased to 98.9%. The average recovery of the wasterwaters from different sources were good using the best microwave digestion if chloride concentration were below 1000mg/L and COD values were below 500mg/L in wastewaters. After digesting and centrifuging samples, samples were injected into flow injection analysis system and the results were comparable. The average COD recovery of the wastewaters from garbage leachate (diluted 4 times) were 94.1%.
Ⅱ. Decomposition of the Polycyclic Aromatic Hydrocarbons in Soil Using Microwave Energy
The aims of this study were to treat the organic compounds in soil by microwave irradiation then to detect residual compounds by microwave extraction and gas chromatography(GC).
The advantages of decomposing the organics in soil by microwave energy are easy operation and simple equipment. The treating process was to add Cu2O and NaOH into the microwave vessel containing pyrene spiked sand(60~45 mesh), followed by microwave irradiation.
First, the pyrene(20μg/g) was spiked into the sand before homogeneous test was completed, extracted by microwave-assisted extraction and the average recovery of pyrene was good, proven by F test and t test. Then, the parameters used for decomposing the pyrene in the soil were household microwave: 713.6W, treatment time: 40mins., reagent: Cu2O (0.3g), NaOH (10N 0.1mL) and water (5mL). Finally, the average decomposing efficiency of the pyrene was 92.7 %.

第一部份 以開放式聚焦微波消化法配合分光光度計
偵測廢水中化學需氧量之研究
目 錄
中文摘要Ⅰ
英文摘要Ⅲ
表 目 錄Ⅷ
V
圖 目 錄
第一章 緒 論1
1-1前言 1
1-2研究動機1
1-3研究目的及內容2
第二章 文獻回顧4
2-1化學需氧量4
2-1-1化學需氧量概述4
2-1-2化學需氧量測定物質的限制4
2-1-3化學需氧量的催化劑5
2-2化學需氧量之干擾9
2-3化學需氧量之測定方法12
2-3-1重鉻酸鉀法13
2-3-2高錳酸鉀法18
2-4微波加熱法18
2-4-1微波原理18
2-4-2微波法簡介20
2-4-3微波化學需氧量(COD)相關文獻21
2-5流動注入分析法(FLOW INJECTION ANALYSIS)23
2-5-1樣品和試劑的輸送系統23
2-5-2樣品注射器和偵測器24
2-5-3流動注入分析法的原理25
2-5-4流動注入分析法相關文獻28
第三章 實驗材料、設備與方法31
3-1實驗藥品及試劑 31
3-1-1一般藥品、試劑31
3-1-2化學需氧量標準溶液32
3-1-3氯鹽標準溶液 32
3-1-4化學需氧量測定試劑33
3-1-5氯鹽測定試劑 33
3-2 實驗設備 34
3-2-1一般實驗設備 34
3-2-2密閉式比色法之設備34
3-2-3微波加熱系統設備35
3-2-4流動注入分析法實驗設備36
3-3實驗方法 40
3-3-1密閉式比色法實驗流程40
3-3-2微波加熱法實驗流程42
3-3-3氯鹽測定流程 44
3-3-4田口式正交法尋求實驗最佳條件45
第四章 結果與討論 47
4-1 化學需氧量比色法檢量線之建立47
4-2 特性波長的尋求 47
4-3 微波條件的尋求 52
4-3-1微波加熱COD的初步效果 52
4-3-2微波條件的決定 53
4-3-3實驗條件及藥劑之驗證 55
4-4 檢量線之濃度上限 59
4-5 氯鹽干擾效應 59
4-5-1 重鉻酸鉀迴流法的氯鹽干擾效應59
4-5-2 初步微波條件的氯鹽干擾效應60
4-6 真實水樣之初步測試 64
4-7 APG盲樣標準品之初試 64
4-8 APG盲樣標準品再試驗 71
4-9 最佳微波條件對檢量線之適用性72
4-10 最佳微波條件之氯鹽干擾 72
4-11 不同來源水樣分析 74
4-11-1染整業水樣分析 74
4-11-2石化業水樣分析 79
4-11-3製酒業水樣分析 80
4-11-4食品業水樣分析 81
4-11-5垃圾滲出水水樣分析 82
4-11-6造紙業水樣分析 84
4-12 流動注入法分析 85
4-12-1實驗因子之考量 85
4-12-2流動注入法之檢量線 86
4-12-3流動注入分析法分析真實水樣87
第五章 結論與建議 95
第六章 參考文獻 97
第二部份 以微波法處理土壤中多苯環芳香烴之初步研究
目 錄
第一章 緒 論102
1-1前言 102
1-2研究目的及內容103
第二章 文獻回顧105
2-1多苯環芳香族碳氫化合物定義與來源105
2-2多苯環芳香族碳氫化合物的性質106
2-3多苯環芳香族碳氫化合物之萃取方法113
2-3-1索式萃取方法 114
2-3-2超臨界流體萃取法114
2-3-3微波輔助萃取法115
2-3-3-1微波輔助萃取法115
2-3-3-2微波輔助萃取法簡介116
2-3-3-3微波萃取相關文獻116
2-4多苯環芳香族碳氫化合物之分析方法118
2-5土壤中有機污染物之整治技術118
2-5-1移地處理 119
2-5-2現地處理 119
第三章 實驗材料、設備與方法 122
3-1實驗藥品與試劑 122
3-1-1 PYRENE 122
3-1-2有機溶劑 122
3-1-3管柱淨化藥品 123
3-2 實驗設備 124
3-2-1 一般實驗設備 124
3-2-2 氣相層析儀器和設備124
3-2-2-1氣相層析儀 124
3-2-2-2氣體 125
3-2-2-3氣體純化裝置125
3-2-2-4層析管柱 126
3-2-2-5資料處理器 126
3-2-3 濃縮、淨化設備127
3-2-3-1 Kuderna-Danish(K-D)濃縮設備127
3-2-3-2淨化設備 127
3-2-4 微波萃取裝置 128
3-2-5 微波加熱系統 129
3-3實驗方法 132
3-3-1.器皿清洗 132
3-3-2微波功率測定 135
3-3-3微波萃取流程 136
3-3-4管柱乾燥淨化 138
3-3-5 K-D濃縮 138
3-3-6 GC/FID分析條件139
3-3-7添加PAH金剛砂均質化樣品製作140
3-3-8 土壤處理流程 141
第四章 結果與討論 144
4-1 芘標準品之配製與檢量線之建立144
4-1-1標準品之配製 144
4-1-2停滯時間之鑑定及檢量線之建立144
4-1-3檢量線之查核 146
4-2 GC分離芘之條件 146
4-3 微波功率測試結果 150
4-4 微波萃取條件之回收率討論150
4-5 金剛砂加入芘模擬樣品均質化驗證154
4-6 微波處理之初步成果 157
4-7 空白試驗 161
4-7-1 溶劑空白試驗 161
4-7-2 矽膠空白試驗 161
4-7-3 無水硫酸鈉空白試驗 162
第五章 結論與建議 166
第六章 參考文獻 167

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