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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Effect of eluent composition and pH and chemiluminescent reagent pH on ion chromatographic selectivity and luminol-based chemiluminescence detection of Co2+,Mn2+ and Fe2+ at trace levels
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Effect of eluent composition and pH and chemiluminescent reagent pH on ion chromatographic selectivity and luminol-based chemiluminescence detection of Co2+,Mn2+ and Fe2+ at trace levels

机译：洗脱液组成，pH和化学发光试剂pH对痕量水平的Co2 +，Mn2 +和Fe2 +的离子色谱选择性和基于鲁米诺的化学发光检测的影响

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摘要

The alkaline-luminol/H2O2-based chemiluminescent (CL) detection of Fe2+,Co2+,and Mn2+,separated with aDionex CS5A ion chromatographic phase was studied by means of a multi-pump flow system allowing the variation of the post-column solution composition.A perchlorate gradient at pH 1.9 (with HC1) was used to separate cations partially complexed with 5.6mM oxalate present in the eluent and necessary for the chosen separation phase.A 0.91 mM luminol,3.3 mM H2O2 in 0.25 M carbonate buffer at pH 10.5 composition was chosen as CL reagent solution.The chosen pH value warrants signal repeatability and wider linearity range although absolute signal is not maximum.The CL signal was related to the pH of the two post-column mixing solutions.Calibration plots of Co2+ and Fe2+ were linear in the chosen concentration range whilst a parabolic model was the best fit for Mn2+.Detection limits were 0.24,0.50 and 375 nM for Co2+,Fe2+ and Mn2+,respectively.The method was used to determine Co2+ at trace level in commercial copper chelates used for animal feeding.A comparison with a chromatographic method with spectrophotometric detection was made giving results comparable both in absolute values and accuracy.
机译：利用多泵流路系统研究了用aDionex CS5A离子色谱相分离的Fe2 +，Co2 +和Mn2 +的基于碱-米诺醇/ H2O2的化学发光（CL）检测方法，该方法可以改变柱后溶液的组成。 pH 1.9（含HCl）的高氯酸盐梯度用于分离与洗脱液中存在的5.6mM草酸盐部分络合的阳离子，这对于选定的分离阶段是必需的。在pH 10.5的0.25 M碳酸盐缓冲液中组成0.91 mM的鲁米诺，3.3 mM的H2O2选择CL试剂溶液，选择的pH值可保证信号的重复性和线性范围，尽管绝对信号不是最大信号.CL信号与两种柱后混合溶液的pH有关.Co2 +和Fe2 +的校准图呈线性在选定的浓度范围内，而抛物线模型最适合Mn2 + .Co2 +，Fe2 +和Mn2 +的检测极限分别为0.24、0.50和375 nM。该方法用于测定痕量水平的Co2 +在用于动物饲养的商品化铜螯合物中进行了比较。与采用分光光度法检测的色谱方法进行了比较，得出的结果在绝对值和准确性上均具有可比性。

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