快速分离富集火焰原子吸收测定不同盐度海水中溶解态锌的新方法
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摘要
本文建立了一种快速分离富集火焰原子吸收测定不同盐度海水中溶解态Zn的新方法。此新方法将流动注射(FI)编结反应器(KR)空气混合吸附在线富集与火焰原子吸收光谱法(FAAS)联用。进样流速6.0 m L/min;进样时间60 s,测定20μg/L的锌,浓集系数(EF)由传统方法的9.4提高到23.9;测样频率为40/h;检出限为0.31μg/L;相对标准偏差(RSD,n=11)为2.1%。将该新方法应用于珠江口不同盐度的海水样品中溶解态的Zn的分析,所得回收率为95.4%~97.2%。该方法可以满足河口不同盐度海水中溶解态Zn的测定需求。
A high speed separation and preconcentration method in a knotted reactor coupled with flame atomic absorption spectrometry was developed for the determination of dissolved trace Zn in seawater with different salinity. This new method was based on the air mixing sorption flow injection( FI) on-line preconcentration procedure in a knotted reactor( KR) coupled with flame atomic absorption spectrometry( FAAS). The preconcentration flow rate was 6. 0 m L /min,preconcentration time was 60 s. When the 20 μg / L Zn solution was detected,the enrichment factor( EF) was promoted from 9. 4 to 23. 9 compared with the traditional method; The detection limit( 3σ) was 0. 31 μg / L for Zn;The sample throughput was 40 / h,and the relative standard deviation( RSD,n = 11) was 2. 1% for Zn. The method has been applied to the determination of dissolved trace Zn in seawater with different salinity with the recovery from95. 4% to 97. 2% and can satisfy the determination requirements of dissolved trace Zn in seawater with different salinity at estuary.
A high speed separation and preconcentration method in a knotted reactor coupled with flame atomic absorption spectrometry was developed for the determination of dissolved trace Zn in seawater with different salinity. This new method was based on the air mixing sorption flow injection( FI) on-line preconcentration procedure in a knotted reactor( KR) coupled with flame atomic absorption spectrometry( FAAS). The preconcentration flow rate was 6. 0 m L /min,preconcentration time was 60 s. When the 20 μg / L Zn solution was detected,the enrichment factor( EF) was promoted from 9. 4 to 23. 9 compared with the traditional method; The detection limit( 3σ) was 0. 31 μg / L for Zn;The sample throughput was 40 / h,and the relative standard deviation( RSD,n = 11) was 2. 1% for Zn. The method has been applied to the determination of dissolved trace Zn in seawater with different salinity with the recovery from95. 4% to 97. 2% and can satisfy the determination requirements of dissolved trace Zn in seawater with different salinity at estuary.
引文
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[12]王中瑗,张宏康,方宏达,等.非分离状态下FI-KR-FAAS测定铁的价态[J].光谱学与光谱分析,2012,32(3):817-820.
[13]李卓,苏耀东,王中瑗,等.流动注射编结反应器吸力洗脱-火焰原子吸收光谱法测定水样中铅锌[J].冶金分析,2009,29(12):13-16.
[14]王中瑗,苏耀东,李双,等.空气混合流动注射-编结反应器预富集-火焰原子吸收光谱法测定水样中痕量铅[J].冶金分析,2008,28(6):24-28.
[15]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].Analytical Chemistry,2002,74(5):1075-1080.
[2]胡未,张新申,张一,等.流动注射分光光度法测定海水中痕量锌——5-Br-PADAP-Zn2+配合物法[J].皮革科学与工程,2007,17(4):53-56.
[3]王增焕,王许诺.萃取分离-原子吸收光谱法测定海水中镉铜铅锌铬镍[J].冶金分析,2014,34(2):44-47.
[4]曲念东,田秀蕾,易志全,等.湛江港海水中总锌、总铬的含量变化与水质评价[J].海洋开发与管理,2011,28(11):69-73.
[5]O’SULLIVAN J E,WATSON R J,BUTLER E C V.An ICP-MS procedure to determine Cd,Co,Cu,Ni,Pb and Zn in oceanic waters using in-line flow-injection with solid-phase extraction for preconcentration[J].Talanta,2013,115:999-1010.
[6]VEGUERA S F J,GODOY J M,DE CAMPOS R C,et al,Trace element determination in seawater by ICP-MS using online,offline and bath procedures of preconcentration and matrix elimination[J]Microchemical Journal,2013,106:121-128.
[7]马元庆,靳洋,刘义豪,等.海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定[J].分析科学学报,2009,25(4):478-480.
[8]袁东星,王小如,杨芄原,等.海水中痕量锌的流动注射在线预富集和电感耦合等离子体原子荧光检测[J].分析化学,1992,20(2):162-164.
[9]刘琳娟,陆培培.海水中铜、铅、镉、锌国标测定条件优化[J].分析测试技术与仪器,2012,18(1):57-61.
[10]王中瑗,苏耀东,甘礼华.基于吸力洗脱的流动注射在线富集与火焰原子吸收联用测定水样中的镉[J].分析化学,2009,37(2):247-250.
[11]王中瑗,张宏康,方宏达,等.两步洗脱法FIA-FAAS测定水样中的锌[J].光谱学与光谱分析,2011,31(12):3384-3387.
[12]王中瑗,张宏康,方宏达,等.非分离状态下FI-KR-FAAS测定铁的价态[J].光谱学与光谱分析,2012,32(3):817-820.
[13]李卓,苏耀东,王中瑗,等.流动注射编结反应器吸力洗脱-火焰原子吸收光谱法测定水样中铅锌[J].冶金分析,2009,29(12):13-16.
[14]王中瑗,苏耀东,李双,等.空气混合流动注射-编结反应器预富集-火焰原子吸收光谱法测定水样中痕量铅[J].冶金分析,2008,28(6):24-28.
[15]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].Analytical Chemistry,2002,74(5):1075-1080.