2,3-聚季铵盐附聚型离子色谱固定相的制备及其在SO_4^(2-)分析中的应用  

Preparation of an agglomerated ion chromatographic stationary phase with 2,3-ionene and its application in SOSO_4^(2-) analysis

作　　者：王慕华[1] 刘军伟[2] 黄忠平[3] 张嘉捷[2] 朱岩[2] 

机构地区：[1]丽水学院化学系,浙江丽水323000 [2]浙江大学化学系,浙江杭州310028 [3]浙江工业大学化工学院,浙江杭州310014

出　　处：《色谱》2015年第7期678-682,共5页Chinese Journal of Chromatography

基　　金：浙江省自然科学基金项目(Y4110532,LY12B05003);浙江省高等学校访问学者专业发展项目(FX2013148);国家重大科学仪器设备开发专项(2012YQ09022903);浙江省公益性科技计划(分析测试)项目(2012C37038)

摘　　要：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0.999 2;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。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＆nbsp;suitable for the detection of SO2-4 in complex matrix samples.

关 键 词：2 3-聚季铵盐 附聚型离子色谱固定相 硫酸根离子 制备 

分 类 号：O658[理学—分析化学]