School of Chemical Engineering, Xi'an University, Xi'an 710065, China.
School of Chemistry and Chemical Engineering, Yan'an University, Yan'an 716000, China.
Molecules. 2018 Oct 10;23(10):2597. doi: 10.3390/molecules23102597.
A simple and sensitive cloud point extraction method for the preconcentration of ultra-trace amounts of nickel as a prior step to its determination by graphite furnace atomic absorption spectrometry was proposed. It is based on the reaction of nickel with 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in HAc⁻NaAc buffer media and mixed micelle-mediated extraction of the complex using the anionic surfactant sodium dodecyl sulfate sodium (SDS) and non-ionic surfactant (1,1,3,3-Tetramethylbutyl)phenyl-polyethylene (Triton X-114). The optimal reaction and extraction conditions such as pH, concentration of 5-Br-PADMA, SDS and Triton X-114, equilibrium temperature, incubation, and centrifuge time were evaluated and optimized. Under the optimal conditions, the calibration graph was linear over the range 0.1⁻5.5 ng/mL of nickel with a correlation coefficient of 0.9942. The detection limit obtained was 0.031 ng/mL, and the relative standard deviation was 2.1% for nickel ( = 2 ng/mL, = 6). The proposed method was successfully applied to the determination of nickel in water samples.
提出了一种简单灵敏的浊点萃取方法，用于预富集痕量镍，作为石墨炉原子吸收光谱法测定镍的前处理步骤。该方法基于镍与 2-(5-溴-2-吡啶偶氮)-5-二甲氨基苯胺（5-Br-PADMA）在 HAc⁻NaAc 缓冲介质中的反应，以及使用阴离子表面活性剂十二烷基硫酸钠（SDS）和非离子表面活性剂（1,1,3,3-四甲基丁基）苯基-聚乙二醇（Triton X-114）对配合物进行混合胶束介导萃取。评估和优化了最佳反应和萃取条件，如 pH 值、5-Br-PADMA、SDS 和 Triton X-114 的浓度、平衡温度、孵育和离心时间。在最佳条件下，镍的校准曲线在 0.1⁻5.5 ng/mL 范围内呈线性，相关系数为 0.9942。获得的检测限为 0.031 ng/mL，镍的相对标准偏差为 2.1%（ = 2 ng/mL， = 6）。该方法成功应用于水样中镍的测定。
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