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用于超痕量钼选择性分离与预富集的均相液-液萃取法

Homogeneous liquid-liquid extraction method for the selective separation and preconcentration of ultra trace molybdenum.

作者信息

Ghiasvand A R, Shadabi S, Mohagheghzadeh E, Hashemi P

机构信息

Department of Chemistry, Lorestan University, Falak-al-Aflak Street, Khorram-Abad, Iran.

出版信息

Talanta. 2005 May 15;66(4):912-6. doi: 10.1016/j.talanta.2004.12.041. Epub 2005 Jan 19.

Abstract

A new simple and efficient homogeneous liquid-liquid extraction method for the selective separation and preconcentration of molybdenyl ions was developed. alpha-Benzoin oxime (ABO) was investigated as a complexing ligand, and perfluorooctanoate ion (PFOA(-)) was applied as a phase-separator agent under strongly acidic conditions. Under the optimal conditions ([ABO]=2.1x10(-3)M, [PFOA(-)]=1.8x10(-2)M, [HNO(3)]=1.7M, [acetone]=11.8% (v/v)), 10mug of molybdenum in 5ml aqueous phase could be extracted quantitatively into 40mul of the sedimented phase. The maximum concentration factor was 125-fold. Thiocyanate was applied as a chromogenic reagent for the direct spectrophotometric determination of molybdenum in the sedimented phase. The reproducibility of the proposed method is at the most 2.4%. The influence of the type and concentration of acid solution, the concentration of ABO, the type and volume of the water-miscible organic solvent, the concentration of PFOA(-), and the effect of different diverse ions on the extraction and determination of molybdenum(VI) were investigated. The proposed method was applied to the extraction and determination of molybdenum(VI) in natural water, Spinach, and Lucerne samples. A satisfactory agreement exists between the results obtained by the proposed method and those reported by GF-AAS.

摘要

开发了一种用于选择性分离和预富集钼酰离子的新型简单高效均相液-液萃取方法。研究了α-苯偶姻肟(ABO)作为络合配体,并在强酸性条件下将全氟辛酸根离子(PFOA(-))用作相分离剂。在最佳条件下([ABO]=2.1×10(-3)M,[PFOA(-)]=1.8×10(-2)M,[HNO(3)]=1.7M,[丙酮]=11.8%(v/v)),5ml水相中10μg钼可定量萃取到40μl沉淀相中。最大浓缩因子为125倍。硫氰酸盐用作显色剂,用于直接分光光度法测定沉淀相中的钼。所提出方法的重现性最高为2.4%。研究了酸溶液的类型和浓度、ABO的浓度、与水混溶的有机溶剂的类型和体积、PFOA(-)的浓度以及不同多种离子对钼(VI)萃取和测定的影响。所提出的方法应用于天然水、菠菜和苜蓿样品中钼(VI)的萃取和测定。所提出方法获得的结果与石墨炉原子吸收光谱法(GF-AAS)报告的结果之间存在令人满意的一致性。

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