毛细管前螯合双（水杨醛）四甲基乙二胺从矿石和原油油样品中萃取分离钒的 MEKC 测定法。

MEKC determination of vanadium from mineral ore and crude petroleum oil samples using precapillary chelation with bis(salicylaldehyde)tetramethyl-ethylenediimine.

机构信息

High Tech Central Resource Laboratory, University of Sindh, Jamshoro, Sindh, Pakistan.

出版信息

J Sep Sci. 2009 Sep;32(18):3169-77. doi: 10.1002/jssc.200900278.

DOI:10.1002/jssc.200900278

PMID:19746397

Abstract

An analytical procedure has been developed for the separation of Cu(II), Ni(II), Co(II), Fe(II), Pd(II), Th(IV), V(IV), and determination of Fe(II), Co(II), Ni(II), and V(IV) by MEKC after chelation with bis(salicylaldehyde)tetramethylethylenediimine (H(2)SA(2)Ten). Uncoated fused silica capillary was used with an applied voltage of 30 kV with photo-diode array detection at 228 nm. SDS was added as micellar medium at pH 8.2 with sodium tetraborate buffer (0.1 M). Linear calibrations were established within 0.015-1000 microg/mL of each element with LOD within 5-67 ng/mL. The method was applied for the determination of vanadium from crude oil and ore samples in the range 0.34-2.40 and 114.2-720.7 microg/g with RSD 1.7-3.8 and 0.98-2.30% (n = 3), respectively. Fe, Ni, and Co present in crude oil and ore samples were also determined with RSD 1.3-2.8, 1.1-4.1, and 1.2-3.5% (n = 3), respectively. The results were compared with that of supplier's specifications and atomic absorption spectrometry (AAS). Method was evaluated by standard addition technique.

摘要

已经开发出一种分析程序，用于通过螯合 bis(salicylaldehyde)tetramethylethylenediimine (H(2)SA(2)Ten) 分离 Cu(II)、Ni(II)、Co(II)、Fe(II)、Pd(II)、Th(IV)、V(IV)，并通过 MEKC 测定 Fe(II)、Co(II)、Ni(II)和 V(IV)。使用未涂覆的熔融石英毛细管，在 228nm 处用光二极管阵列检测施加 30kV 的电压。在 pH 8.2 下添加 SDS 作为胶束介质，并使用硼酸钠缓冲液（0.1M）。每个元素的线性校准范围为 0.015-1000μg/mL，LOD 在 5-67ng/mL 范围内。该方法用于测定原油和矿石样品中的钒，范围为 0.34-2.40 和 114.2-720.7μg/g，RSD 分别为 1.7-3.8%和 0.98-2.30%（n=3）。还测定了原油和矿石样品中的 Fe、Ni 和 Co，RSD 分别为 1.3-2.8%、1.1-4.1%和 1.2-3.5%（n=3）。结果与供应商规格和原子吸收光谱法（AAS）进行了比较。该方法通过标准添加技术进行了评估。