CAS OpenIR  > 研究所(批量导入)
Thesis Advisor于仲权
Degree Grantor中国科学院研究生院
Abstract无机硫阴离子的分离测定是经常遇到的分析问题之一。本文采用流动相离子色谱法(MPIC)研究了流动相的组成(CH_3CN、Na_2CO_3和离子作用试剂的浓度)、流动相的流速和柱温对SO_3~(2-)、SO_4~(2-)、S_2O_3~(2-)和S_nO_6~(2-)(n = 2-5)的容量因子的影响,并对流动相离子色谱的机理进行了比较和讨论。在实验中观察到,当分析离子的电荷相同时,离子半径越大和疏水性越强,则其保留时间越长。分析离子的容量因子随离子作用试剂烷基链的加长和浓度的增加而增大,而随流动相中CH_3CN和Na_2Co_3的浓度增加而减小,其中CH_3CN浓度的影响是非常显著的。对分子结构非常相似的连多硫酸根离子S_nO_6~(2-)(n = 2-5)同系物,容量因子的对数与其硫原子数之间存在良好的线性关系。根据色谱分离的一般原则,选出了分离测定SO_3~(2-)/SO_4~(2-)、S_2O_3~(2-)和S_nO_6~(2-)(n = 2-5)的最佳色谱条件。SO_4~(2-)、S_2O_3~(2-)和S_nO_6~(2-)(n = 2-5)连续测定的相对误差分别在0.3-2.4%之间(N = 6),SO_4~(2-)和S_2O_3~(2-)重复性测定的相对误差分别为1.8%和1.1%(M = 4,N = 6)。上述离子分别在50-500倍的浓度范围内,校正曲线呈很好的线性关系,相关系数均大于0.999。SO_4~(2-)、S_2O_3~(2-)和S_2O_6~(2-)的检测极阴分别为10、10和40ppb,S_3O_6~(2-)、S_4O_6~(2-)和S_5O_6~(2-)的检测极限分别为0.1、0.3和0.2ppm。研究了S_nO_6~(2-)(n = 2-5)在不同PH水溶液中的稳定性,并对实际样品进行了分析,得到满意结果。
Other AbstractThe separation and determination of inorganic sulfur anions is one of the analytical problems which are often dealt with. The effects of the mobile phase composition (the concentrations of CH_3CN, Na_2CO_3 and ion-interacting reagent), the velocity of mobile phase and the temperature of separation column on the capacity factors of SO_3~(2-), SO_4~(2-), S_2O_3~(2-) and S_nO_6~(2-) (n = 2 - 5) were investigated by Mobile Phase Ion Chromatography (MPIC) in this paper. A variety of mechanisms of MPIC were compared and discussed. In the experiments, it was observed that the larger radius or the more hydrophobic for the analyte anions with the same charges, the longer for its retention time. The capacity factors of the analyte anions increase with increasing the length of alkyl chain and concentration of the ion-interacting reagent, and decrease with increasing the concentrations of CH_3CN and Na_2CO_3. In these factors, the effect of the concentration of CH_3CN is very significant. In the homologous series of polythionates S_nO_6~(2-) (n = 2-5) with very similar molecular structures, a good linear relationship between the logarithm of the capacity factor and the number of sulfur atoms was observed. The optimum chromatographic conditions for the separation and determination of SO_3~(2-)/SO_4~(2-), S_2O_3~(2-) and S_nO_6~(2-) (n = 2 - 5) were obtained on the general principle of chromatographic separation. All the relative errors of continuous determination for SO_4~(2-), S_2O_3~(2-) and S_nO_6~(2-) (n = 2 - 5) are in the range of 0.3-2.4% (N = 6), and the relative errors of repeatability of determination for SO_4~(2-) and S_2O_3~(2-) are 1.8% and 1.1% respectively (M = 4, N = 6). The linearity of calibration curves of the above anions is very good within the concentration range of 50-500 times. The correlation coefficients of these curves are all larger than 0.999. The detection limits for SO_4~(2-), S_2O_3~(2-) and S_nO_6~(2-) are 10, 10 and 40ppb respectively and 0.1, 0.3 and 0.2 ppm for S_3O_6~(2-), S_4O_6~(2-) and S_5O_6~(2-) respectively. The stability of S_nO_6~(2-) (n = 2 - 5) in the solutions of different PH was investigated and the satisfactory results in the sample determinations were obtained.
Document Type学位论文
Recommended Citation
GB/T 7714
贾忠江. 流动相离子色谱法测定无机硫阴离子[D]. 中国科学院研究生院,1988.
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