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研究生:鄭芳宇
研究生(外文):Fang Yu
論文名稱:海水化學需氧量分析方法之研究
論文名稱(外文):The study of chemical oxygen demand determination of saline water
指導教授:黃平志
口試委員:桂椿雄戴嘉慧
學位類別:碩士
校院名稱:正修科技大學
系所名稱:化工與材料工程研究所
學門:民生學門
學類:美容學類
論文種類:學術論文
論文出版年:2008
畢業學年度:97
語文別:中文
論文頁數:89
中文關鍵詞:化學需氧量、、、、、、低鹵高鹵脫氯迴流液氧化還原作用自我分解反應
外文關鍵詞:Chemical oxygen demandLow halogenHigh halogenBack-flow liquidShed chlorineOxidation-Reduction actionSelf-decomposition reaction
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化學需氧量是反映水體受有機物污染程度的重要指標之一,然而水樣中若存有氯離子,在化學需氧量的測定上則會具有嚴重的干擾而導致測值偏高,進而誤判其分析結果;本研究針對行政院環境保護署環境檢驗所水質檢驗公告方法(NIEA W516.54A),含高濃度鹵離子水中化學需氧量檢測方法-重鉻酸鉀迴流法,提出步驟上的改善與建議,以期更能精準測量海水中之化學需氧量。本研究參考上述方法,以氯離子濃度2000 mg/L為低鹵與高鹵水樣之分水嶺,針對脫氯時間長短、重鉻酸鉀迴流液濃度及添加硫酸鉻鉀與否,由其結果探討海水化學需氧量之最適化方法。由實驗結果得知,高鹵樣品其脫氯時間以4小時以上為佳;採用0.001667 M重鉻酸鉀迴流用做為氧化劑,一方面可減少重鉻酸根離子與氯離子的氧化還原作用,另一方面可降低滴定步驟上的誤差;添加硫酸鉻鉀可抑制重鉻酸根離子在消化迴流時之自我分解反應。本研究探討之最適方法,其適用範圍為COD濃度20 mg/L以下,且氯鹽濃度高達20000 mg/L時仍可適用,故其應亦適於海水化學需氧量之檢測。而由整個研究過程,係建議當水中氯離子濃度高於1000 mg/L時,若先經脫氯過程則應可改善實驗數據品質。
The chemical oxygen demand is reflects the water body one of organic matter pollution degree important targets, however in water sample if has the chloride ion, can have the serious disturbance in the chemical oxygen demand determination to cause to measure the value is high, then misinterprets its analysis result, this research in view of Executive Yuan environmental protection bureau environment examination center water quality examination announcement method (NIEA W516.54A), the high concentrated halogen ion of chemical oxygen demand examination method including of water-Potassium Dichromate back-flow method, proposes in the step improvement and the suggestion, by the time can in the fine accurate survey sea water the chemical oxygen demand. This research reference above method, take chloride ion density 2000 mg/L as the low halogen and watershed of the high halogen water sample, in view of shed chlorine time length, Potassium Dichromate Back-flow liquid concentration and Increase Chromium-potassium sulfate or not, discusses the sea water chemical oxygen demand by its result the most suitable method. By experimental result knowing, the high halogen sample its shed chlorine time take 4 hours above as good, uses 0.001667 M Potassium Dichromate back-flow with to do for the oxidant, on the one hand may reduce the dichromate ion and the chloride ion Oxidation-Reduction action, on the other hand may reduce in the titrate step the error, the increase Chromium-potassium sulfate may suppress the dichromate ion in the digestion back-flow of the self-decomposition reaction. This research discussion most suitable method, its applicable scope is COD below density 20 mg/L, also the chlorine salinity reaches as high as when 20000 mg/L was still suitable, therefore its should also be suitable for examination the sea water chemical oxygen demand. But by entire research process, is the suggestion when in the water the chloride ion density is higher than 1000 mg/L, If passes through the shed chlorine process to be supposed first to be possible to improve the empirical datum quality.
摘要.......................................................................................................Ⅰ
Abstract ................................................................................................Ⅱ
致謝.......................................................................................................Ⅲ
目錄.......................................................................................................Ⅳ
表目錄...................................................................................................Ⅶ
圖目錄...................................................................................................Ⅷ
第一章 緒論...........................................................................................1
1.1前言................................................................................................1
1.2干擾................................................................................................3
1.3研究目的........................................................................................4
1.4研究方向........................................................................................4
第二章 文獻回顧...................................................................................5
2.1化學需氧量部分............................................................................5
2.2氯鹽干擾部份................................................................................7
2.2.1扣除法.....................................................................................7
2.2.2抑制法.....................................................................................8
2.2.3沉澱分離法.............................................................................9
2.2.4酸式吸收法...........................................................................10

第三章 實驗部份.................................................................................12
3.1設備及器材..................................................................................12
3.2試劑..............................................................................................13
3.3實驗步驟......................................................................................16
3.3.1低鹵試驗...............................................................................17
3.3.2高鹵試驗...............................................................................17
3.4結果計算......................................................................................18
第四章 結果與討論.............................................................................19
4.1低鹵部分......................................................................................19
4.1.1採用0.008333 M重鉻酸鉀...................................................19
4.1.2採用0.004167 M重鉻酸鉀...................................................26
4.1.3採用0.001667 M重鉻酸鉀...................................................32
4.1.4不同重鉻酸鉀濃度對各水樣基質之比較...........................38
4.1.5不同重鉻酸鉀濃度之空白比較...........................................46
4.1.6針對0.001667 M重鉻酸鉀之氧化力測試...........................47
4.1.7滴定液的濃度變化...............................................................48
4.2高鹵部分......................................................................................49
4.2.1脫氯時間之比較...................................................................49
4.2.2採用0.008333 M重鉻酸鉀...................................................51
4.2.3採用0.004167 M重鉻酸鉀...................................................52
4.2.4採用0.001667 M重鉻酸鉀...................................................53
4.2.5不同重鉻酸鉀濃度對各水樣基質之比較...........................54
4.2.6不同重鉻酸鉀濃度之空白比較...........................................58
4.2.7針對0.001667 M重鉻酸鉀重複性試驗...............................59
第五章 結論與建議.............................................................................60
參考文獻...............................................................................................61
附錄.......................................................................................................65
中文部份
1. 李中光、章帘~、蕭薀華,水質分析(第五版),滄海書局,2004。
2. 江漢全,水質分析(革新二版),三民書局,2004。
3. 蕭薀華、傅崇德、章帘~,環境工程化學(第四版),滄海書局,1999。
4. 章裕民,環境工程化學(修訂新版),文京圖書,1998。
5. 闕山仲、方嘉德、徐照程、陳秀珍,分析化學,藝軒圖書,2001。
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7. 行政院環境保護署環境檢驗所水質檢驗方法,水中化學需氧量檢測方法-重鉻酸鉀迴流法,NIEA W515.54A,2007。
8. 行政院環境保護署環境檢驗所水質檢驗方法,含高濃度鹵離子水中化學需氧量檢測方法-重鉻酸鉀迴流法,NIEA W516.54A,2007。
9. 行政院環境保護署環境檢驗所水質檢驗方法,水中化學需氧量檢測方法-密閉迴流滴定法,NIEA W517.51B,2007。
10. 柳鍾坦、凌文秀,鹵離子對化學需氧量之干擾及其抑制方法,工業污染防治期刊,第49期,107-123,1994。
11. 曾昭桓、陳秀卿,以氯化銀分離法去除高濃度氯鹽干擾的水中化學需氧量分析,中國環境工程學刊,第三卷,第四期,237-240,1993。
12. 酗艇縑A含高鹵離子化學需氧量分析方法之研究,工業污染防治,51(7),137-149,1994。
13. 鄭幸雄、鄭盟東,化學需氧量測定方法之探討,成大環工所,水技術研討會論文集,8-26,1980。
14. 張月,COD測定中氯離子干擾的消除方法,中國環境工程技術中心,2004。
15. 田東紅,化學需氧量-重鉻酸鉀法結果出現偏差原因的探討,內蒙古環境科學,2007。
16. 林俊鑫,氯鹽對COD分析影響之研究,台灣大學環境工程所碩士論文,1980。
17. 吳怡嬅,含高濃度氯離子水樣化學需氧量分析方法改進之研究,中山大學海洋資源所碩士論文,1998。
18. 田瑤,水中化學需氧量(COD)分析方法之改善,中興大學環境工程所碩士論文,2000。
19. 鄭晴方,高氯鹽水樣COD分析方法之比較與改善,中興大學環境工程所碩士論文,2002。
英文部分
20. Standard Methods for the Examination, Vater Sewage and Industrial Wastes, American Public Health Association, 10th, Ed., 1955.
21. Standard Methods for the Examination of Wastewater, American Public Health Association, 20th, Ed., 1998.
22. Moore, W. A., R. C. Kroner and C. C. Ruchhoft, Dichromate Reflux Method for Determination of Oxygen Consumed, Analytical Chemistry Vol. 21, No. 8, August 1949.
23. Moore, W. A., F. J. Ludzack and C. C. Ruchhoft, Determination of Oxygen-Consumed Values of Organic Wastes, Analytical Chemistry Vol. 23, NO. 9, September 1951.
24. Moore, W. A. and W. W. Walker, Determination of Low Chemical Oxygen Demands of Surface Water by Aichromate Oxidation, Analytical Chemistry Vol. 28, NO. 2, February 1956.
25. Bertram, F. W., O. T. Carlisle, J. E. Murray, G. W. Warren and C. W. Connell, Chemical Oxygen Demand of Petrochemical Wastes Analytical Chemistry Vol. 30, NO. 9, September 1958.
26. Baumann, F. J., Dichromate Reflux Chemical Oxygen Demand Analytical Chemistry Vol. 46, NO. 9 August 1974.
27. Dobbs, R. A. and R. T. Williams, Elimination of Chloride Interference in the Chemical Oxygen Demand Test, Analytical Chemistry Vol. 35, NO. 8, July 1963.
28. Cripps, J. H. and O. Jenkins, A COD method suitable for the analysis of highly saline waters, JWPCF, Vol. 36, NO. 10, October 1964.
29. Thompson. K. C., Mendham D., Best D., de Cassers, K. E., Simple method for minimizing the effect of chloride on the Chemical oxygen demand test without the use of mercury salts, Analyst, 111, 483-485, 1986.
30. Cameron, W. M. and Moore, T. B., The influence of chloride on the dichromate-value test, Analyst, 82, 677-682, 1957.
31. Vaidya B., Reduction of chloride ion interference in chemical oxygen demand determination using bismuth-based adsorbents, Analytical Chemistry, 357, 167-175, 1997.
32. Ramon Ramon, Francisco Valero, Manuel del Valle, Analytica Chimica Acta, 491, 99-109, 2003.
33. DIN 38409-H41-2, Determination of the Chemical Oxygen Demand (COD), December 1980.
34. DIN 38409-H43-2, Determination of the Chemical Oxygen Demand (COD), December 1981.
35. DIN 38409-H44-2, Determination of the Chemical Oxygen Demand (COD), December 1992.
36. ASTM, Standard Test Methods for Chemical Oxygen Demand ( Dichromate Oxygen Demand ) of Water, D1252-06, 2006.
37. Angel Cuesta, Jose L. Todoli, Juan Mora, Antonio Canals, Analytica Chimica Acta, 372, 399-409, 1998.
38. Liberato Ciavatta and Maria Grimaldi, Istituto di Chimica Analitica dell’Universita, Naples, Italy, 1967.
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