HPSEC-UV-TOC联用技术测定有机物相对分子质量分布

采用在线高效凝胶色谱仪(HPSEC)和紫外检测器以及TOC检测仪联用测定有机物相对分子质量分布.通过同步测定样品中大范围相对分子质量区间的UV254和TOC,更深入和准确地了解有机物的结构特性,特别是一些不含共轭双键和芳香度的有机物.结果显示,TOC检测仪能够简单快捷地检测出水中所有有机物的相对分子质量分布,包括蔗糖、海藻酸钠等对紫外响应较低的亲水性有机物;样品进样量与TOC响应线性正相关,进样量越大,响应越强;离子强度从0升至0.2mol.L-1,峰面积仅减小1.2%,离子强度对有机物相对分子质量分布测定影响较小;样品pH值在中性或酸性时不影响测定结果,pH值为碱性时,TOC响应异常;采用流动相配定的样品较超纯水配定的样品,相对分子质量分布曲线中干扰峰明显减小,出峰效果更好;该联用技术可以很好地表征湘江原水及其4种亲疏水性组分的相对分子质量分布.

Determination of the Distribution of Relative Molecular Mass of Organic Matter by High Pressure Size Exclusion Chromatography with UV and TOC Detectors

An on-line high pressure size exclusion chromatography (HPSEC) with UV and TOC detectors was adapted to examine the distribution of relative molecular mass of natural organic matter (NOM). Through synchronous determination of UV₂₅₄ and TOC responses in a wide range of relative molecular mass, it was possible to accurately characterize the structure of NOM, especially for some non-aromatic and non-conjugated double bond organics which have low response to UV. It was found that, TOC detector was capable of detecting all kinds of organic matters, including sucrose, sodium alginate and other hydrophilic organic compounds. The sample volume had a positively linear correlation with the TOC response, indicating that the larger volume would produce stronger responses. The effect of ion strength was relatively low, shown by the small decrease of peak area (1.2%) from none to 0.2 mol·L^-1 NaCl. The pH value of tested samples should be adjusted to neutral or acidic because when the samples were alkaline, the results might be inaccurate. Compared to the sample solvents adopted as ultrapure water, the samples prepared by mobile phase solvents had less interference to salt boundary peak. The on-line HPSEC-UV-TOC can be used accurately to characterize the distribution of relative molecular mass and its four fractions in River Xiang.