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標題: 鉍吸收法應用於高氯鹽水樣COD分析的探討
The Application of bismuth-based adsorption method on COD determination of highly saline Wastewater
作者: 林芝萍
Chih-Ping, Lin
關鍵字: bismuth-based adsorbent;鉍吸收劑;COD;highly saline;化學需氧量;高氯鹽
出版社: 環境工程學系所
引用: 田瑤。2000。水中化學需氧量分析方法之改善。中興大學環境工程研究所碩士論文。 行政院環境保護署(92.11.26.)放流水標準。 行政院環境保護署。1998。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 W516.53A。 行政院環境保護署。1998。水中化學需氧量檢測方法─重鉻酸鉀迴流法,NIEA W515.53A。 行政院環境保護署。1999。水中化學需氧量檢測方法─密閉迴流滴定法,NIEA W517.50B。 許元正。1994。含高鹵離子水中化學需氧量分析方法之研究。工業污染防治。第51期。 柳鍾坦與凌文秀。1994。鹵離子對化學需氧量之干擾及其抑制方法。工業污染防制期刊。第49期:107-123。 鄭晴方。2002。高氯鹽水樣COD分析方法之比較與改善。中興大學環境工程研究所碩士論文。 Baumann, F.J..1974. Dichromate reflux chemical oxygen demand. Anal Chem., 46: 91-105. Bertram F.W., Carlisle O.T., Murray J.E., Marren G.W., Connel C.W. and Connel C.H.. 1958. Chemical oxygen demand of pertrochenical wastes-Modification of standard catalytic reflux procedure. Anal Chem.,30:1482. Clesceri L.S., Greenberg, A.E., and Easton, A.D.. 1998. Standard Methods for the Examination of Water and Wastewater 20th Edition, AWWA WEF., ISBN 0-87553-235-1. Cripps, J.M. and Jenkins, D.. 1964. A COD method suitable for the analysis of highly waters. Journal WPCF. 36:1240-1246. Dobbs, R.A. and Williams, R.T.. 1963. Elimination of chloride interference in chemical oxygen demand test. Anal Chem., 35(8):1064-1067. Harris, D.C.,2005,Exploring chemical analysis,3rd.ed.,W.H.Freeman and Company. Moore, W.A., Kroner, R.C. and Ruchhoft, C.C.. 1949. Dichromate reflux method for determination of oxygen consumed. Anal Chem., 21:953-957. Moore, W.A.. 1951. Determination of oxygen-consumed values of organic wastes. Anal Chem.. 23:1297-1300. Thompson, K.C., Mendham, D., Best, D., and de Cassers, K.F.. 1986. Simple method for minimizing the effect of chloride on the chemical oxygen demand test without the use of mercury salts. Analyst, 111:483-485. Vaidya, B., Watson, S.W., Coldiron, S.J.and Porter, M.D.. 1997. Reduction of chloride ion interference in chemical oxygen demand(COD)determinations using bismuth-based adsorbents. Anal Chem., 357:167-175.
化學需氧量(Chemical oxygen demand﹐COD)是有機污染物在水環境系統中一個極重要的指標。由需氧量的高低可瞭解水中有機物污染的程度。化學需氧量的檢測一般採用重鉻酸鉀迴流法,而水中氯離子一直是此法在分析COD時的困擾。目前國內針對含高氯離子(2,000 mg/L以上)水樣之COD檢測方法,使用高鹵重鉻酸鉀迴流法,該方法試劑量大,廢液產生量大,對環境的污染大,檢測成本也高,故有必要尋找其他的替代方法。
本研究針對文獻上提及的鉍吸收法,探討其應用於含高氯離子(2,000 mg/L以上)水樣COD檢測之適用性。經探討後求得,鉍吸收法的重要操作條件為:高鹵水樣1.0 mL,使用0.5 g鉍吸收劑量、加熱去氯時間為2小時,重鉻酸鉀消化試劑不含汞。
利用上述的鉍吸收法求得,COD空白分析值為7.5 ± 8.7 mg/L,方法偵測極限值為24 mg/L,可容忍的氯離子濃度達40,000 mg/L。分析COD 100 mg/L含氯離子濃度0 - 40,000 mg/L之人工配製標準水樣,得COD分析值為95 - 119 mg/L,相對標準偏差為5 - 14%。分析COD值50 - 200 mg/L,氯離子濃度20,000 mg/L的人工配製標準水樣,得COD回收率為98 - 107%,相對標準偏差為6 – 11%。
取台中港附近的海水、電廠廢水廠進流水、電廠廢水廠放流水、電廠廢水廠活性碳塔進流水及某工廠廢水為真實水樣,使用本鉍吸收法分析結果,得海水COD值為14.8 ± 10.5 mg/L,與使用傳統高鹵法測定值(15.6 ± 7.5 mg/L)相近。雖然其他水樣之鉍吸收法測定值與高鹵法測定值間有些差異,但使用鉍吸收法之添加回收率均在75 – 120%範圍,依環境樣品的添加分析標準(回收率100 ± 20 %)而言,大致上仍在可接受範圍之內。
經由人工配製水樣及真實水樣的分析得知,鉍吸收法適用之氯離子濃度可高達40,000 mg/L,水樣中COD濃度可達300 mg/L,較行政院環境保護署公告方法之適用範圍更廣,且廢液量較少,對環境產生之污染衝突亦較小。

Chemical Oxygen Demand ( COD) is a usual and important index for monitoring organic pollution of water and wastewater. There are several methods that can be used for COD determination when samples have high chloride content. The method described by National Institude of Environmental Analysis (NIEA W516.53A)in Taiwan is tedious, time-consuming and can produce a large amount of toxic liquid waste. So, it has the need to find an alternative that is more friendly to the environment.
In this study , the suitability of a bismuth-based adsorbent mentioned in literature was evaluated to reduce the interference from high concentration of chloride(Cl->2,000 mg/L)in the determination of COD. Chloride ion is removed at 150℃ as hydrochloric acid gas from acidified sample solution reacted in a closed tube and captured by the adsorbent suspended above the heated solution. In this work, the optinum conditions obtained for the removal of chloride ion are as follows: 0.5 g of bismuth-based adsorbent is used for 1.0 mL of water sample followed by 2hr of reflux reaction at 150℃. Afterwards, the solution is digested for COD determination without Hg(Ⅱ)as a masking agent.
The blank value collected by this method is 7.5 ± 8.7 mg/L and the method detection limit is 24 mg/L. For the standard solutions contanining theoretical COD value(ThCOD)of 100 mg/L and 0 - 40,000 mg Cl- /L, the recoveries are at the range of 95-119% and the relative standard deviation(RSD)are at the range of 5-14%. For the standard solutions(ThCOD 50-200 mg/L, each containing 20,000 mg Cl-/L), the recoveries range from 98% to 107% and the RSDs range from 6% to 11%. Using this method, the seawater samples collected from the nearby seashore have COD values of 14.8 ± 10.5 mg/L, that agree with the results(15.6 ± 7.5 mg/L)examinated by the NIEA W516.53A method. Totally, the spike tests have recoveries of 75-120% for all real samples including the sea water samples mentioned above.
The results from this study show that this bismuth-based adsorption method is applicable for water samples of low-level matrix in COD determination. For complicated water samples this method still exists some limitations, although it produces small amount of liquid waste and has smaller harmful effect to the environment.
其他識別: U0005-2408200723424500
Appears in Collections:環境工程學系所

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