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A new method for separation and determination of Cr(III) and Cr(VI) in water samples by high-performance liquid chromatography based on anion exchange stationary phase of ionic liquid modified silica

机译:基于离子液体改性二氧化硅阴离子交换固定相的高效液相色谱分离测定水样中Cr(III)和Cr(VI)的新方法

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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.
机译:在这项工作中,制备了N-甲基咪唑氯化物离子液体官能化的二氧化硅,并用作阴离子交换固定相,用于通过高效液相色谱(HPLC)在200 nm处进行UV检测分离铬。将Cr(VI)作为HCr2O7-和螯合的Cr(III)与邻苯二甲酸氢钾(PHP)作为Cr(PHP)(2)(-)保留在制备的色谱柱上,并使用由5%甲醇组成的流动相进行分离pH 6.5的25 mM磷酸盐缓冲液。使用Box-Behnken(BBD)设计,通过响应面方法(RSM)对影响螯合/分离步骤的几个变量进行建模。通过具有95%置信限的方差分析(ANOVA)检验了自变量及其相互作用的显着性。在优化的条件下,Cr(III)和Cr(VI)阴离子物种被很好地分离,每个Cr物种在保留时间分别为2.3和4.3分钟时有一个峰。 Cr(III)的峰面积与浓度之间的线性关系在0.025-30范围内,Cr(VI)的峰面积与浓度之间的关系为0.5-20 mg L-1,Cr(III)的检出限为0.010和0.210 mg L-1 )和Cr(VI)。该方法通过同时分离和测定自来水和地下水样品中的Cr种类而得到验证,而无需进行任何预处理。

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