首页> 中文期刊> 《色谱》 >2,3-聚季铵盐附聚型离子色谱固定相的制备及其在SO2-4分析中的应用

2,3-聚季铵盐附聚型离子色谱固定相的制备及其在SO2-4分析中的应用

         

摘要

The poly-electrolyte cation functional group of 2,3-ionene was synthesized with tet-ramethyl ethylenediamine and 1,3-dibromopropane as the raw materials. Multiporous polysty-rene-divinylbenzene microsphere particles( PS-DVB)were produced by swelling method with polystyrene as seeds and sulfonated. Then the 2,3-ionene was bonded on the sulfonated multi-porous polystyrene-divinylbenzene microsphere particles by agglomeration to get the agglomera-tive ion-exchange stationary phase. After optimizing the synthetic conditions, the new stationary phase was characterized by the techniques including scanning electron microscopy ( SEM),Fourier transform infrared spectroscopy( FTIR)and elemental analysis. The chroma-tographic column was packed by slurry method and applied in the analysis of SO 2-4 with a con-ductivity detector. SO 2-4 and other six common anions including F-,Cl-,NO-2 ,Br-,NO-3 ,PO 3-4 , were separated and analyzed rapidly on the self-regulating chromatographic column within 8 min. The linear range was from 0. 5 to 50 mg/L with correlation coefficient( r)of 0. 999 2. The LOD was 0. 04 mg/L with S/N of 3. The relative standard deviations( RSDs,n=6)were 2. 4%and 3. 1% for the peak area and retention time,respectively. The recoveries were between 99. 2% and 101. 8%. The retention times of SO 2-4 did not change significantly after long time use of the self-regulating chromatographic column. The self-regulating chromatographic column is suitable for the detection of SO2-4 in complex matrix samples.%以四甲基乙二胺和1,3-二溴丙烷为原料,合成了聚电解质阳离子功能基———2,3-聚季铵盐功能基。以聚苯乙烯为种子,通过种子溶胀法制备了多孔型聚(苯乙烯-二乙烯基苯)微球( PS-DVB),并对其进行磺化。以附聚的方式在磺化的 PS-DVB微球上附聚2,3-聚季铵盐功能基,得到附聚型离子交换固定相,通过匀浆法装入色谱柱,并将其用于 SO2-4的分离分析。SO2-4能与其他常见的6种阴离子在8 min 内完成分离,实现 SO2-4的快速测定。其中, SO2-4的线性范围为0.5~50 mg/L,线性相关系数 r为0.9992;加标回收率在99.2%~101.8%之间;峰面积和保留时间的相对标准偏差分别为2.4%和3.1%;根据信噪比( S/N=3)计算出检出限为0.04 mg/L。结果表明该自制色谱柱适用于复杂基质中 SO2-4的快速测定。

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