Sadeghi Susan, Moghaddam Ali Zeraatkar
Department of Chemistry, Faculty of Science, University of Birjand, Birjand, South Khorasan, Iran.
Environ Monit Assess. 2015 Dec;187(12):725. doi: 10.1007/s10661-015-4928-1. Epub 2015 Nov 3.
In this work, N-methylimidazolium-chloride ionic liquid functionalized silica was prepared and used as an anion-exchange stationary phase for separation of chromium species by high-performance liquid chromatography (HPLC) with UV detection at 200 nm. The Cr(VI) as HCr2O7(-) and chelated Cr(III) with potassium hydrogen phthalate (PHP) as Cr(PHP)2 (-) was retained on the prepared column and separated using a mobile phase composed of 5% methanol in 25 mM phosphate buffer at pH 6.5. Several variables affecting the chelation/separation steps were modeled by response surface methodology (RSM) using Box-Behnken (BBD) design. The significance of the independent variables and their interactions were tested by the analysis of variances (ANOVA) with 95% confidence limit. Under the optimized conditions, the Cr(III) and Cr(VI) anionic species were well separated with a single peak for each Cr species at retention times of 2.3 and 4.3 min, respectively. The relationship between the peak area and concentration was linear in the range of 0.025-30 for Cr(III) and 0.5-20 mg L(-1) for Cr(VI) with detection limits of 0.010 and 0.210 mg L(-1) for Cr(III) and Cr(VI), respectively. The proposed method was validated by simultaneous separation and determination of the Cr species in tap and underground water samples without impose to any pretreatment.
在本研究中,制备了N-甲基咪唑鎓氯化物离子液体功能化硅胶,并将其用作阴离子交换固定相,通过高效液相色谱(HPLC)在200 nm处进行紫外检测来分离铬物种。以HCr2O7(-)形式存在的Cr(VI)和以Cr(PHP)2 (-)形式存在的与邻苯二甲酸氢钾(PHP)螯合的Cr(III)保留在制备的柱上,并使用由25 mM磷酸盐缓冲液(pH 6.5)中5%甲醇组成的流动相进行分离。使用Box-Behnken(BBD)设计,通过响应面法(RSM)对影响螯合/分离步骤的几个变量进行了建模。通过具有95%置信限的方差分析(ANOVA)测试了自变量及其相互作用的显著性。在优化条件下,Cr(III)和Cr(VI)阴离子物种得到了很好的分离,每种Cr物种在保留时间分别为2.3和4.3 min时出现一个单峰。峰面积与浓度之间的关系在Cr(III)为0.025 - 30以及Cr(VI)为0.5 - 20 mg L(-1)范围内呈线性,Cr(III)和Cr(VI)的检测限分别为0.010和0.210 mg L(-1)。所提出的方法通过同时分离和测定自来水和地下水样品中的Cr物种进行了验证,无需进行任何预处理。