工作场所空气中痕量重金属速测方法的研究
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摘要
目的:建立一种快速消解并同时测定工作场所空气中痕量重金属钴(Co)﹑铜(Cu)﹑铅(Pb)﹑镍(Ni)、镉(Cd)﹑锌(Zn)的方法。
     方法:采用微波消解法,在180℃﹑20atm﹑800w条件下消解采样滤膜;用壳聚糖在消解溶液pH=5.0,室温(20~30℃)条件下富集,直接火焰原子法测定富集消解液中痕量重金属Co﹑Cu﹑Pb﹑Ni、Cd﹑Zn。
     结果:微波消解法与混酸消解法相对标准偏差(RSD)范围分别为3.0%~12.7%和6.7%~22%,微波消解法RSD明显低于混酸消解法,说明微波消解法精密度好于混酸法;Co﹑Cu﹑Pb﹑Ni、Cd﹑Zn检出限分别为4.85、2.42、3.17、5.47、0.42、0.51ng/ml;标准曲线回归系数(r)范围为0.999 1~0.999 9;回收率范围为91.3%~108.4%;用标准物质(GBW08401)进行质控测试,分析结果与标准值吻合;样品测定值与石墨炉原子法相比,无显著性差异(P﹥0.05)。
     结论:该方法简便、快速、准确、灵敏度高,适合工作场所空气中痕量重金属Co﹑Cu﹑Pb﹑Ni、Cd﹑Zn的测定。
Objective:To find a method of digesting membranes rapidly and simultaneously determining trace heavy metals of Pb, Cd, Cu, Co, Ni and Zn in the air of workplaces.
     Methods: In the paper, trace heavy metals of Pb, Cd, Cu, Co, Ni and Zn in the the air of workplaces were pretreated by microwave digestion (at 180℃, 20atm , 800w) and concentrated by absorption on chitosan (at pH = 5.0, 20℃~30℃),Determined Co, Cu, Pb , Ni, Cd and Zn in digesting liquids with direct flame atomic absorption spectrophotometry.
     Results: Microwave digestion relative standard deviation (RSD) range of 3.0% ~12.7% was significantly higher than mixed acid method of 6.7%~22%, indicated good precision compared with the mixed acid method; The detection limit of this method was 3.17ng/ml for Pb, 0.42 ng/ml for Cd , 2.42 ng/ml for Cu, 4.85 ng/ml for Co, 5.47ng/ml for Ni and 0.51ng/ml for Zn;Standard linear correlation (r) were of the range 0.9991~0.9999; Recovery ratio were of the range 91.3%~108.4%; The standard reference materials was used as quality control standards and the analysis results conformed well to the certified values, the sample results have no significance different(P﹥0.05)compared with graphite furnace atomic absorption spectyometry.
     Conclusion: The method was simple, rapid , accurate and highly sensitive. It was suitable for determining trace heavy metals of Pb, Cd, Cu, Co, Ni and Zn in the air of workplaces.
引文
[l]黄丽,李加新,周宁怀等.环境污染与防治,2001,23(5):245.
    [2] Muzzarelli R A A Chitin.New York,Pergamon press,1977,134.
    [3]郭敏杰,刘振,李海.壳聚糖吸附重金属离子的研究进展[J].化工环保,2004,24(4):262.
    [4]刘振南.壳聚糖对重金属离子吸附的研究[J].广西化工,1996,2:8-11.
    [5]缪茜,孙静.壳聚糖吸附剂研究[J].北京工业职业技术学院学报,2004,3(3):25.
    [6] Qu X,Wirsen A,Albertsson A C.Polymer,2000,41(12):4589-4598.
    [7]石光,袁彦超.应用化学,2005,22(2):195-197.
    [8] Kufita K,Koyama Y,Nishimura S,et al,Chem Lett,1989:l597.
    [9] Ruiz M ,Sastre A,Guibal E.Separation Sci Techn,2002,37(10) :2385
    [10]谢华林,张萍,蒋宏伟等.大气颗粒物中重金属元素在不同粒径上的形态分析[J].环境工程,2002,20(6):55-57.
    [11] Mohanral R,Azeez P A,Priscilla T,et a1.Heavy metal in airborne particulate matter of urban Coimbatore[J].Environmental Contamination and Toxicology,2004,47:162-167.
    [12]吕昌银.毋福海.空气理化检验[M].北京:人民卫生出版社,2006:15.
    [13]李晓,杨立中.成都市东郊TSP及Pb、Cd、Hg、As浓度日变化规律研究[J].地质灾害与环境保护,2004,15(3):35-38.
    [14]于燕,张振军,李义平.西安市大气颗粒物污染现状及其金属特征研究[J].环境与健康杂志,2003,20(6):359-360.
    [15]王章玮,张晓山,张逸等.北京市大气颗粒物PM2.5、PM10及降雪中的汞[J].环境化学,2004,23(6):668-673.
    [16]沈轶,陈立民,孙久宽等.上海市大气PM2.5中Cu、Zn、Pb、As等元素的浓度特征[J].复旦大学学报,2002,41(4):405-408.
    [17]赵美萍,邵敏.环境化学[M].北京:北京大学出版社.2005:186.
    [18]钱嫦萍,陈振楼,毕春娟等.潮滩沉积物重金属生物地球化学研究进展[J].环境科学研究,2002,15:49-51.
    [19] Wang S X,Zhang S Z,Shan X Q,et a1.Fractionation of heavy metals in different particle-size sediments and its relationship with heavy metal pollution[J].Environmental Contamination and Toxicology,2003.71:873-880.
    [20] Tessier A,Campbell P R C ,Bisson M ,et a1.Sequential extraction procedure for the speciation of particulate tracemetal[J].Analytical Chemistry,1979,51:850-851.
    [21]陈子金.工作场所中重金属存在形式探索[J].中国卫生检验杂志,1995(特刊):172-174.
    [22]齐文启,陈光,孙宗光等.大气颗粒物监测分析及今后研究课题[J].中国环境监测,2003,19(1):51-62.
    [23]王荫淞,李爱国,魏仑等.用X射线吸收近边结构谱研究大气颗粒物中元素的种态[J].核技术,2004,27(11):810-813.
    [24]陶俊,陈刚才,赵琦等.重庆市大气TSP中重金属分布特征[J].重庆环境科学,2003,25(12):15-19.
    [25]张元勋,王荫淞,李德禄等.上海冬季大气可吸入颗粒物的PIXE研究[J].中国环境科学,2005,25(增刊):1-5.
    [26] Horacio B,Marcelo O.Study of atmospheric particulate matter in Buenos Aires city[J].Atmospheric Environment,2003,37:1135-1147.
    [27]孙微,王磊,李一峻等.电化学分析方法在元素形态分析中的应用[J].分析化学,2004,32(4):541-545.
    [28] GBZ/T 160—2004《工作场所空气有毒物质测定》[S].
    [29] GBZ/T 192.1—2007工作场所空气中粉尘测定[S].
    [30]张伶,黄开宇,张吉广.微波消解石墨炉原子吸收法测定空气中的锰(铅)[J].2002,1:44.
    [31]但德忠,徐先顺,罗方若等.现代微波制作技术[M].成都:四川大学出版社,2003:61,72.
    [32]张加玲.卫生化学[M].北京:中国协和医科大学出版社,2003:34,213.
    [33]高焰,王东海,林玉斌等.空气中铅镉超声浸取原子吸收方法研究[J].中国环境监测,2003,19(4):37.
    [34]黄达卿,陈亮,弯军英等.壳聚糖对金属离子的吸附选择性[J].广州化工,2005,33(6):38.
    [35]姚瑞华,孟范平,张龙军等.改性壳聚糖对重金属离子的吸附研究和应用进展[J].材料导报,2008,22(4):66.
    [36]缪茜,孙静.壳聚糖吸附剂研究[J].北京工业职业技术学院学报,2004,3(3):25.
    [37] JJF 1059—1999,测量不确定度评定与表示.北京:中国计量出版社.
    [l]黄丽,李加新,周宁怀等.环境污染与防治,2001,23(5):24.
    [2] Muzzarelli R A A Chitin.New York,Pergamon press,1977,134.
    [3] Tseng R L,W u F C,Juang R S.J Chem Teehnol Blot,1999,74:533-538.
    [4] Dong S K,Byoung Y P.J Chem Teehnol Blot,2001,76:l179-l184.
    [5] Kurita K,Sannan T,1wakura Y ,J Appl Polym Sei,1979,23 :511-521.
    [6]柯火仲,吕禹泽.化学世界,1991,4:158 160.
    [7]郭敏杰,刘振,李海.壳聚糖吸附重金属离子的研究进展[J].化工环保,2004,24(4):262.
    [8]刘振南.壳聚糖对重金属离子吸附的研究[J].广西化工,1996,(2):8-11.
    [9]缪茜,孙静.壳聚糖吸附剂研究[J].北京工业职业技术学院学报,2004,39(3):25.
    [10] Qu X,Wirsen A.Albertsson A C.Polymer,2000,41(12):4589-4598.
    [11]石光,袁彦超等.应用化学,2005,22(2):195-19.
    [12] Kufita K,Koyama Y,Nishimura S,et al.Chem Lett,1989:l597.
    [13] Ruiz M ,Sastre A,Guibal E.Separation Sci Techn,2002,37(10):2385.
    [14] Inoue K ,Ohto K,Yoshizuka K,et a1.Bull Chem Soc Jpn,1997,(701):2443.
    [15] Sun Shengling,Wang Aiqin,Sep Purif Technol,2006,49(3):197.
    [16]黄晓佳,王爱勤,袁光谱.应用化学,2000,17(1):66.
    [17]张淑琴,汪玉庭,唐玉蓉.上海环境科学,2003,22(1):39-41.
    [18] Tang Y R,Zhang S O,Wang Y T.Wuhan University Journal of Natural Sciences,2002,7(2):217-221.
    [19]陈水平,汪玉庭.分析科学学报,2004,20(1):9-l2.
    [20]孙新枝,苏中兴.化学研究,2005,16(1):29-31.
    [21]陈湘平,俞继华.湿法冶金,2000,19(31):63.
    [22]陈伟,林友文.福建环境,2000,17(5):9-10.
    [23]彭长宏,汪玉庭.环境科学,1998,19(5):29-33.
    [24]Athena Webster, Merrill D Hailing, David, et a1. Carbohydrate Res,2007,342(31):l189.
    [25]李斌,崔慧.壳聚糖富集FAAS法测定水中痕量Cu(I)[J].理化检验(化学分册),2001,37(6):253-254.
    [26]汤又文,陈炳稔,朱小兰.壳聚糖预富集水样中痕量Cr(Ⅶ)的研究[J].华南师范大学学报(自然科学版),1999,(2):l71-74.
    [27]粱勇,汤又文,汪朝阳.以甲壳素为母体的螯合树脂预富集一悬浮液进样GFAAS法测定水中痕量银的研究[J].分析实验室,1999,18(5):41-43.
    [28]李琼,奚旦立.壳聚糖吸附废水中铅离子的研究[J].化工环保,2005,25(5):350-352.
    [29]张廷安,豆志河.用壳聚糖脱除废水中的铜离子[J].东北大学学报(自然科学版),2006,27(2):203-205.
    [30]张廷安,豆志河.壳聚糖絮凝剂处理废水中的Ag+[J].东北大学学报(自然科学版),2006,27(1):53-56.
    [31] Gao Yunhua,Lee K H ,Oshima M ,et a1.Adsorption behavior of metal ions on cross—linked chitosan and the determination of oxoanions after pretreatment with a chitosan column[J].Analytical Sciences 2000,16(12):1 303-1 308.
    [32] Nor Azah Yusof,Musa Ahmad.A flow cell optosensor for determination of Co2+ based on immobilised 2-(4一pyridylazo)resorcinol in chitosan membrane by using stopped flow,flow injection analysis[J].Sensors Actuators B,2002-(86):127-133.
    [33] Nor Azah Yusof,M usa Ahmad.A flow cell optosensor for lead based on immobilized gallocynin in chi—tosan membrane[J].Talanta,2002,(58):459-466.
    [34] Wang Gang,Xu Jingjuan,Ye Lihua,et a1.Highly sensitive sensors based on the immobilizatioin of tyrosinase in chitosan[J]. Bioelectrochemistry,2002,(57):33-38.
    [35] Ye Xianzeng,Yang Qinghua,Yan W ang,et a1.Electrochemical behaviour of gold,silver·platinum and palladium on the glassy carbon electrode modified by chitosan and its application[J].Talanta,1998,(47):1 099-1 106.
    [36] Lu Guanghan,Yao Xin,W u Xiaogang,et a1.Determination of the total iron by chitosan—modified glassy carbon electrode.Microchemical Journal,2001,(69):81-87.
    [37] Xu Jinrui,Liu Bin.Preconcentration and determination of Lead ions at a chitosan-modified glassy carbon electrode.Analyst,1994,(119):1 599-1 601.
    [38]Pan Y,Li Y J,Zhao H Y,Chinese J,Pharm.SCi.2OO2,11(3):97-l00.
    [39] Huang M,Ma Z S,Eugene K.Pharm.Res.2002,19(10) :1488-1494.

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