顧曉明 秦宏兵 朱君
摘 要:用微波消解法對空氣濾膜和廢氣濾筒進行前處理,通過電感耦合等離子體發射光譜法測定了鉻、銅、鎳的濃度,并對測定結果進行了分析。結果表明,對空氣樣品中鉻、銅、鎳分析時微波消解法的檢出限分別為0.006μg/m3、0.003μg/m3、0.04μg/m3,精密度分別為1.5%、3.2%、3.5%,加標回收率分別為104%、105%、103%。對廢氣樣品中鉻、銅、鎳分析時,微波消解法的檢出限分別為2.0μg/m3、0.8μg/m3、1.0μg/m3,精密度分別為3.5%、4.4%、4.3%,加標回收率分別為104%、107%、106%。同時對有證濾膜進行了測定,結果均合格。微波消解法測定的鉻、銅、鎳含量有較好的檢出限、精密度和準確度,與電熱板消解法不存在顯著性差異,均適用于空氣和廢氣顆粒物中的鉻、銅、鎳的測定。
關鍵詞:微波消解;電感耦合等離子體發射光譜法;顆粒物;濾膜;濾筒;重金屬
中圖分類號 O657.31 文獻標識碼 A 文章編號 1007-7731(2018)13-0091-03
Abstract:The air filter membrane and exhaust gas filter cartridge were pretreated by microwave digestion,and the concentration of chromium,copper and nickel was determined by inductively coupled plasma atomic emission spectrometry,and the results are analyzed.The detection limits of microwave digestion in the analysis of chromium,copper and nickel in the air samples were 0.006,0.003,and 0.04g/m3 respectively,and the precision was 1.5%,3.2% and 3.5%,respectively,and the recovery rates were 104%,105% and 103%,respectively.The detection limits of the microwave digestion method for the analysis of chromium,copper and nickel in the waste gas samples were 2,0.8,and 1 g/m3 respectively,and the precision was 3.5%,4.4% and 4.3% respectively,and the recovery rates were 104%,107% and 106%,respectively.Meanwhile,the measured results of certified filter membrane were all qualified.It is found that the content of chromium,copper and nickel determined by microwave digestion method has good detection limit,precision and accuracy,and there is no significant difference from the electrothermal plate digestion method.It is suitable for the determination of chromium,copper and nickel in air and waste gas particles.
Key words:Microwave digestion;ICP-AES;Particulate matter;Membrane;Filter cartridge;Heavy metal
環境空氣和廢氣中的重金屬元素主要來源于土壤、機動車尾氣、居民取暖及工業廢氣的排放[1],經過氣流傳輸、沉降及呼吸深入到人體肺部的氣體交換器官,對人體造成潛在的危害。目前,測定環境空氣中重金屬含量的主要方法有原子吸收光譜法、原子熒光光譜法、電感耦合等離子體發射光譜法、電感耦合等離子體質譜法[2~7]等。
空氣和廢氣顆粒物中的鉻、銅、鎳濾膜及濾筒的消解方法主要采用電熱板消解法,該方法對溫度控制的要求較高,需將加熱的溫度控制在(100±5)℃,且要加蓋回流防止金屬組分揮發。而微波消解具有用酸量小,消解速度快,消解比較完全,易揮發元素不易損失等優點。……