Preparation and characterization of open tubular ion chromatographic columns

doi:10.3724/SP.J.1123.2019.08020

Abstract

Abstract:

In recent years, significant progress has been made in the area of open tubular ion chromatography (OTIC). In particular, gradient OTIC has been realized through the development of hydroxide eluent-compatible OTIC columns. This review covers the preparation and characterization of different OTIC columns, ranging from the historic silica-based columns to the newly emerging polymer-based open tubular (OT) columns. The preparation of various OTIC stationary phases, from grafted to latex agglomerated and monolayer to multilayer phases, has been briefly introduced. The characterization of electrostatic latex agglomerated OTIC columns has been extensively discussed, e. g. fluorescent ion displacement chromatography, frontal displacement chromatography, and frontal reaction chromatography have been used to measure the capacities of OT columns, and the results are compared with the theoretical calculation values. The variable α_iex, defined as the number of ion-exchange equivalents per unit surface area, is used as an indicator of the capacity of OT columns, to enable a straightforward comparison between OT columns having different inner diameters (i.d.). The newly introduced column capacity parameter, γ_iex, defined as the stationary phase capacity per unit liquid volume present, is used to investigate the relationship between packed and OT columns when using the same stationary phase. Methods for improving the column efficiency, such as decreasing the column diameter and/or increasing the column temperature, are presented. In addition, determination of the functionalization uniformity along an OT column by (a) separately measuring the capacities of two halves of the column, (b) measuring the retention factors for several ions in successive 10 cm segments of the column in multiple injections, and (c) measuring the retention variance of a single ion in different segments of the column from a single injection, is discussed.

Key words: open tubular, column preparation, capillary column, latex agglomeration, ion chromatography (IC), review

CLC Number:

O658

HUANG Weixiong. Preparation and characterization of open tubular ion chromatographic columns[J]. Chinese Journal of Chromatography, 2020, 38(4): 399-408.

Figures/Tables 7

Fig. 1 Polymer structure[18] The monomers are shown in the inset. BDDE: 1,4-butanediol diglycidyl ether.

Fig. 2 Schematic representation of a dual-layer latex agglomerated silica open tubular column[50]

Fig. 3 Gradient chromatogram on AS18 latex agglomerated open tubular cycloolefin polymer (COP) column[27] Column: 28 μm inner diameter (i.d.), 370 μm outer diameter (o.d.), 744 mm in length. Exit capillary: silica, 25 μm i.d., 370 μm o.d., with an Analytical Foundry detector (operated at 1.2 kHz) located 33 mm from the center of the suppressor. Linear gradient expressed as t (min) and LiOH concentration (mmol/L): 0, 8.0; 3, 40.0; 7, 40.0; 7.5, 8.0. Flow rate: 168 nL/min. Suppressor active length: 0.65 mm. Current: 15 μA; 6.7 nL injection; each analyte has a concentration of 100 μmol/L, except for phosphate (200 μmol/L).

Fig. 4 (a) Anion-exchange and (b) cation-exchange capacity determination of open tubular COP column before and after latex agglomeration (dash lines represent differential data)[31] The cation-exchange capacity measurement experiment starts with a lightly sulfonated 28.0±0.5 mm i.d. COP column with an effective length of 700±1 mm. It is then coated with AS18 latex for anion-exchange capacity measurement.

Fig. 5 log10 k/γiex vs. log10[E] for packed and open tubular columns with the same stationary phase[9] Open and filled symbols are used for open tubular and packed columns, respectively. Packed column: 4 mm×250 mm, AS18, 1 mL/min, 30 ℃, linear velocity 0.178 cm/s. OT column: sulfonated cyclic olefin polymer, AS18 latex coated 19 μm i.d., 951 mm long, 39 nL/min, 22 ℃, linear velocity 0.23 cm/s. [E]: eluent concentration.

Fig. 6 van Deemter plots of latex agglomerated polymethylmethacrylate (PMMA) open tubular columns[37] Conditions: analyte, 500 μmol/L Cl-; injection volume, ~43 pL for 34 cm OT column, 90 pL for 67.5 cm OT column. Column radius: 9.8 μm; effective length: 58 cm. Eluent: 1 mmol/L sodium benzoate.

Fig. 7 (a) Anion-exchange chromatograms at different effective lengths and (b) retention factors for four anions (Cl-, N O 2 -, Br-, and N O 3 -)[31]Flow direction: a. normal; b. both normal and reverse. AS18 latex coated COP column (28 μm i.d., ~750 mm in length; CAEX (31.2±0.1) peq/mm2). 2.5 nL injected; eluent: 5.0 mmol/L NaOH@18 psi (~0.31 cm/s). Peaks: 0. system peak; 1. F-; 2. Cl-; 3. N O 2 -; 4. Br-; 5. N O 3 -.

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