請用此 Handle URI 來引用此文件: http://hdl.handle.net/11455/5121
標題: 建立土壤重金屬快速檢測方法
Rapid determination of heavy metals in soils
作者: 林煌仁
Lin, Huang-Jen
關鍵字: soil
土壤
metal
microwave digestion
rapid determination
重金屬
微波消化
快速分析
出版社: 環境工程學系
摘要: 本研究以建立土壤重金屬快速檢測方法為目的,利用微波輔助加熱方式快速消化土壤,並以火焰原子吸收光譜儀分析鉛、鎘、鋅及銅四種金屬元素,再與傳統方法比較。首先,探討密閉微波消化與開放聚焦式微波消化方法之最適操作條件;其次分析土壤標準參考樣品CRM 2004、CRM 141R及CRM 026-050,評估方法的準確性;最後以建立之微波消化程序分析桃園、彰化、高雄及台東等地區之不同土樣,以探討方法之適用性及可能的影響。希望藉此研究成果能提供一快速、準確、靈敏之土壤重金屬分析方法。 研究結果顯示,密閉微波法之較佳操作條件為土樣0.5 g、靜置時間1 hr、功率600 W、微波升溫時間15 min、微波消化溫度180 ℃、微波消化時間10 min;開放微波法為土樣0.5 g、靜置時間1 hr、功率30% (75 W)、微波消化時間5 min。之後再以建立之微波法及傳統熱板迴流法消化三種土壤參考樣品,結果顯示密閉微波消化法Pb的回收率在118% - 136%之間、Cd的回收率在104% - 121%之間、Zn的回收率在115% - 118%之間、Cu的回收率在110% - 121%之間;開放聚焦式微波消化法四種金屬元素回收率則介於92% - 117%之間;熱板迴流法回收率介於73% - 131%之間。若將密閉微波消化溫度設定為112 ℃時,除Pb外,Cd、Zn、Cu的分析值與參考值已相近。顯示對此三種金屬而言,微波法可取代傳統方法並可快速獲得其在土中含量的資訊。 以20種不同土樣進行消化分析並與傳統熱板迴流法比較,結果顯示對Cd及Zn三種消化方法間無明顯差異;Pb及Cu則以密閉微波(180 ℃)>開放微波≒熱板迴流,且整體而言,密閉微波法高出傳統熱板迴流約16%。若將密閉微波消化溫度設定為112 ℃,則微波法與熱板迴流結果相近。三種消化方法分析相對標準偏差(RSD)在3.1%以內,添加回收率在94%-111%之間。而以土壤基本性質探討Pb及Cu在密閉微波與熱板迴流消化結果之差異,結果顯示Pb的部份隨著粘粒含量增加,兩個消化方法之測值差異愈大;Cu的部份則當砂粒含量增加時,兩方法之測值差異愈小,而當坋粘粒含量增加時,差異則愈大。
The purpose of this research is to develop a rapid determination method for heavy metals (Pb、Cd、Zn、Cu) in contaminated soil. Microwave digestion techniques including closed-microwave and focused-microwave systems were utilized to dissolve the metals from soil samples. Afterward, the extraction solution was analyzed by flame atomic absorption spectrophotometry (AA). Firstly, the microwave operation parametes (including sample amount, settling time after adding oxidizing reagent—aqua regia, microwave power, digestion temperature, and digestion time) were optimized. Three standard reference materials (CRM 2004, CRM 141R and CRM 026-050) were then analyzed to assess the accuracy of the developed method. Under the closed-microwave digestion (sample 0.5 g, settling for 1hr, power 600W, 180 ℃, digestion for 10 min) the recoveries for Pb, Cd, Zn, Cu were between 118%-136%, 104%-121%, 115%-118% and 110%-121% respectively. On the other hand, under the focused-microwave digestion (sample 0.5g, settling for 1hr, power 75W, digestion for 5 min), the recoveries for Pb, Cd, Zn, Cu were all between 92%-117%. The microwave digestion methods were also compared with traditional hotplate reflux method. The result shows that open focused-microwave digestion method has the same digestion efficiency with traditional method. Twenty soil samples collected from polluted and unpolluted area were digested using the developed microwave method and analyzed by AA. The precision expressed as relative standard deviation (RSD) was within 3.1%. The recovery of standard addition was 94%-111%.
URI: http://hdl.handle.net/11455/5121
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