Simultaneous separation of common mono- and divalent cations on a calcinated silica gel column by ion chromatography with indirect photometric detection and aromatic monoamines–oxalic acid, containing crown ethers, used as eluent

Abstract

The application of unmodified silica gel (Super Micro Bead Silica Gel B-5, SMBSG B-5) as a cation-exchange stationary phase in ion chromatography with indirect photometric detection (IC–IPD) for the separation of common mono- and divalent cations (Li +, Na +, NH 4 +, K +, Mg 2+ and Ca 2+) was carried out using various aromatic monoamines {tyramine [4-(2-aminoethyl)phenol], benzylamine, phenylethylamine, 2-methylpyridine and 2,6-dimethylpyridine} as eluents. When using these amines as eluents, the peak resolution between these mono- and divalent cations was not quite satisfactory and the peak shapes of NH 4 + and K + were largely destroyed on the SMBSG B-5 silica gel column. Hence, the application of SMBSG B-5 silica gel calcinated at 200, 400, 600, 800 and 1000 °C for 5 h in the IC–IPD was carried out. The peak shapes of the monovalent cations were greatly improved with increasing calcination temperature and, as a result, symmetrical peaks of these mono- and divalent cations were obtained on the SMBSG B-5 silica gel calcinated at 1000 °C as the stationary phase. In contrast, the peak resolution between these mono- and divalent cations was not improved. Therefore, crown ethers [18-crown-6 (1,4,7,10,13,15-hexaoxacyclooctadecane), 15-crown-5 (1,4,7,10,13-pentaoxacyclopentadecane)] were added to the eluent for the complete separation of these mono- and divalent cations. Excellent simultaneous separation and highly sensitive detection at 275 nm were achieved in 25 min on a column (150×4.6 mm I.D.) packed with SMBSG B-5 silica gel calcinated at 1000 °C by elution with 0.75 m M tyramine–0.25 m M oxalic acid at pH 5.0 containing either 1.0 m M 18-crown-6 or 10 m M 15-crown-5.