FAAS Determination of Trace Amounts of Cadmium in Water Samples-On-line Preconcentration of Cadmium with FI-Knotted Reactor
摘 要
在火焰原子吸收光谱测定水样中痕量镉的方法中,提出了在流动注射-编结反应器对痕量镉离子作在线预富集中用两次引入作为镉离子的配位体的吡咯烷二硫代氨基甲酸铵(APDC)溶液的模式.在此模式中,预先将APDC溶液涂覆在编结反应器的内壁上(这就是第一次引入APDC溶液);第二次引入是将APDC溶液与试样溶液同时注入并在编结反应器中汇合.富集时样品溶液的流速为6.0 mL·min-1,富集时间为60 s.按此方法操作镉的富集系数达到21,此值均高于单独用APDC溶液预涂覆编结反应器模式的富集系数(9)或单独用APDC溶液与试样溶液同时注入并汇合模式的富集系数(16).方法的检出限(S/N=3)为0.32 μg·L-1,方法的进样频率为每小时36个样品,对20 μg·L-1镉标准溶液测定11次,测得方法的相对标准偏差为2.7%.应用此方法测定了几个水样中镉含量,并作回收试验,所得回收率在92.0%~99.0%之间.
Abstract
In the FAAS determination of trace amounts of cadmium in water sample,on-line preconcentration of Cd2+ ion with flow injection knotted reactor was adopted,in which 1-pyrrolidine carbodithioic acid (ammonium salt,abbreviated as APDC) was used as ligand for Cd2+,and the mode of duplicate introduction of the APDC solution into the reactor was introduced. The APDC solution was pre-coated on the inner wall of the knotted reactor (KR),i.e.,the 1st introduction of APDC solution;and the 2nd introduction of APDC solution was carried out simultaneously with the introduction of sample solution. Flow-rate of sample solution in the FI-preconcentration was taken as 6.0 mL·min-1,and the time for preconcentration was taken as 60 s. Concentration factor of Cd2+ by this method attained to a value of 21,which is higher than the values 9 and 16 attained by either the mode of pre-coating on the inner wall of KR or the mode of introduction simultaneously with the sample solution separately. Detection limit (S/N=3) of the method found was 0.32 μg·L-1,and the sampling frequency of 36 samples per hour was achieved. Precision was tested at the concentration level of 20 μg·L-1 of Cd2+,value of RSD (n=11) obtained was 2.7%. In analyzing several water samples by this method,in which (w) 0.01% triethanolamine solution was added as masking agent,values of recovery found were in the range of 92.0%-99.0%.
中图分类号 O657.31
所属栏目 试验与研究
基金项目 国家自然科学基金资助课题(29973029)
收稿日期 2008/3/18
修改稿日期
网络出版日期
作者单位点击查看
备注苏耀东(1947-),男,浙江海盐人,教授,主要研究方向为痕量分析.
引用该论文: SU Yao-dong,WANG Zhong-yuan,LI Zhuo,Wang Min,GAN Li-hua. FAAS Determination of Trace Amounts of Cadmium in Water Samples-On-line Preconcentration of Cadmium with FI-Knotted Reactor[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(9): 818~820
苏耀东,王中瑗,李卓,王敏,甘礼华. 火焰原子吸收光谱法测定水样中痕量镉-用流动注射-编结反应器对痕量镉作在线预富集[J]. 理化检验-化学分册, 2008, 44(9): 818~820
被引情况:
【1】付海曦,刘威,张春辉,李艳, "水体中重金属离子的检测方法研究进展",理化检验-化学分册 48, 496-503(2012)
【2】刘文英,苏耀东,李卓,甘礼华, "流动注射-火焰原子吸收光谱法测定水样中铬(Ⅲ)和铬(Ⅵ)",理化检验-化学分册 46, 1365-1368(2010)
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】叶玉兰,李永生,孟钢,等.大孔型阴树脂交换性能测定的流动注射分析法[J].理化检验-化学分册,2007,43(8):669-672.
【2】吴冬梅,王爱霞.微型柱现场预富集流动注射火焰原子吸收光谱法测定环境水样中钴[J].理化检验-化学分册,2007,43(7):552-557.
【3】Fang Z L. Flow Injection Atomic Absorption Spectrometry[M]. Wiley: Chichester U K,1995.
【4】苏耀东,朱文颖,覃俐,等.空气隔离法流动注射在线预富集火焰原子吸收测定水样中的痕量铜和镉[J].光谱学与光谱分析,2006,26(5):959-962.
【5】Li Y,Jiang Y,Yan X P,et al. A flow injection on-line multiplexed sorption preconcentration procedure coupled with flame atomic absorption spectrometry for determination of trace lead in water,tea,and herb medicines[J]. Anal Chem,2002,74(5):1075-1080.
【6】吴宏,金焰,田野,等.流动注射编结反应器在线分离富集技术在原子光谱中的应用[J].分析化学,2007,35(6):905-911.
【7】Koleva B D,Benkhedda K,Ivanova E,et al. Determination of trace elements in natural waters by inductively coupled plasma time of flight mass spectrometry after flow injection preconcentration in a knotted reactor[J]. Talanta,2007,71(1):44-50.
【2】吴冬梅,王爱霞.微型柱现场预富集流动注射火焰原子吸收光谱法测定环境水样中钴[J].理化检验-化学分册,2007,43(7):552-557.
【3】Fang Z L. Flow Injection Atomic Absorption Spectrometry[M]. Wiley: Chichester U K,1995.
【4】苏耀东,朱文颖,覃俐,等.空气隔离法流动注射在线预富集火焰原子吸收测定水样中的痕量铜和镉[J].光谱学与光谱分析,2006,26(5):959-962.
【5】Li Y,Jiang Y,Yan X P,et al. A flow injection on-line multiplexed sorption preconcentration procedure coupled with flame atomic absorption spectrometry for determination of trace lead in water,tea,and herb medicines[J]. Anal Chem,2002,74(5):1075-1080.
【6】吴宏,金焰,田野,等.流动注射编结反应器在线分离富集技术在原子光谱中的应用[J].分析化学,2007,35(6):905-911.
【7】Koleva B D,Benkhedda K,Ivanova E,et al. Determination of trace elements in natural waters by inductively coupled plasma time of flight mass spectrometry after flow injection preconcentration in a knotted reactor[J]. Talanta,2007,71(1):44-50.
相关信息