A polymer resin surface polymerization-based hydroxide-selective anion exchange stationary phase

doi:10.3724/SP.J.1123.2019.07031

Abstract

Abstract:

A polystyrene-divinylbenzene (PS-DVB) microspheres-based hydroxide-selective anion exchange stationary phase is described. This stationary phase is obtained by the surface polymerization of an allyl glycidyl ether (AGE) and the pendant vinyl groups onto the surface of PS-DVB, followed by open-ring of the epoxy groups using an alkylol amine (abbreviated as P@A-M). Both alkylol amines were compared in terms of separation performance of the stationary phase. Scanning electron microscopy, infrared spectroscopy, and elemental analyses were carried out to characterize the stationary phase. The results indicated that the quaternary amine group was successfully introduced onto the surface of the PS-DVB microspheres, and that there was no obvious change in the physicochemical properties of the resin during the surface polymerization reaction. The P@A-M phase showed high hydroxide-selectivity and good separation performance (resolution>1.5) as well as high running stability (relative standard deviation of retention times<1.13%). The utility of the P@A-M phase was demonstrated by using it for the determination of inorganic anions in the tea.

Key words: ion chromatography (IC), stationary phase, pendant vinyl group, surface polymerization, allyl glycidyl ether

CLC Number:

O658

YANG Zhanqiang, LI Zongying, YANG Dehui, ZHANG Feifang, YANG Bingcheng. A polymer resin surface polymerization-based hydroxide-selective anion exchange stationary phase[J]. Chinese Journal of Chromatography, 2020, 38(4): 452-457.

Figures/Tables 7

Fig. 1 Schematic diagram of the synthesis route of P@A-M stationary phase PS-DVB: polystyrene-divinylbenzene.

Fig. 2 Scanning electron microscopy images of (a and b) PS-DVB microspheres and (c) P@A-M stationary phase

Fig. 3 (a) Nitrogen adsorption and desorption isotherms, (b) pore size distribution, and (c) IR spectrum of stationary phase

Fig. 4 Chromatograms obtained with (a) P@A-D and (b) P@A-M stationary phase Conditions: eluent, 10 mmol/L KOH; column temperature, 30 ℃; column size, 150 mm×4.6 mm; injection volume, 25 μL; flow rate, 1.0 mL/min; suppressed conductance detection.

Fig. 5 Chromatogram of the seven model anions using P@A-M anion exchange stationary phase in gradient model Conditions: eluent, 0-10.5 min (4 mmol/L KOH), 11-16 min (8 mmol/L KOH), 16.5-20 min (4 mmol/L KOH). Other conditions are the same as those in Fig. 4.

Fig. 6 Long-term stability of P@A-M anion exchange stationary phase (n=3) Conditions: eluent, 4 mmol/L KOH. Other conditions are the same as those in Fig. 4.

Table 1 Quantification parameters of the system

Anion	Linear range/ (μmol/L)	Correlation equation	R²	LOD/ (μmol/L)
F^-	5-500	P=7.7972C+0.0014	0.9999	0.0319
Cl^-	5-500	P=9.9920C-0.0374	0.9998	0.0688
N $O_{2}^{-}$	5-500	P=8.4451C-0.0141	0.9999	0.1863
Br^-	5-500	P=8.8852C-0.0578	0.9994	0.1863
N $O_{3}^{-}$	5-500	P=8.1853C-0.0319	0.9998	0.5588
S $O_{4}^{2 -}$	5-500	P=18.5879C-0.1200	0.9998	0.1064

Table 1 Quantification parameters of the system

Anion	Linear range/ (μmol/L)	Correlation equation	R²	LOD/ (μmol/L)
F^-	5-500	P=7.7972C+0.0014	0.9999	0.0319
Cl^-	5-500	P=9.9920C-0.0374	0.9998	0.0688
N $O_{2}^{-}$	5-500	P=8.4451C-0.0141	0.9999	0.1863
Br^-	5-500	P=8.8852C-0.0578	0.9994	0.1863
N $O_{3}^{-}$	5-500	P=8.1853C-0.0319	0.9998	0.5588
S $O_{4}^{2 -}$	5-500	P=18.5879C-0.1200	0.9998	0.1064

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