title: Gravity-flow open tubular cation chromatography.
abstract: We describe ion chromatography (IC) on open tubular cation exchange columns with a controllable capacity multilayered stationary phase architecture. The columns of relatively large bore (75 microm id) are fabricated by coating fused-silica capillaries with multiple layers of poly(butadiene-maleic acid) (PBMA) copolymer and crosslinking the deposited layers by thermally initiated radical polymerisation. Column capacity increases in a predictable manner with increase in the number of successively coated layers. Gravity flow with a modest head (< 2 m) can provide the desired separations within a reasonable period. We provide a minimalist configuration where no suppression is used, the sample is injected hydrodynamically as in CE, and detection is accomplished by an inexpensive homebuilt contactless conductivity detector or a capacitance to voltage digital converter. A 1 m long 75 microm bore column coated with two layers of PBMA allows gravity-flow open tubular IC to separate four alkali cations in < 10 min with a 1 mM tartaric acid (TA) eluent. Simultaneous separation of alkali and alkaline earth metal cations can be accomplished in less than 25 min using 1.75 mM pyridinedicarboxylic acid as an eluent. Contactless conductometric detection (C(4)D) allows LODs down to 150 nmol/L, corresponding to 30 fmol injections. Analysis of real water samples is demonstrated.
authors.affiliation: Department of Chemistry and Biochemistry, Mendel University of Agriculture and Forestry, Zemedelská 1, Brno, Czech Republic. kuban0@mendelu.cz
authors.forename: Petr
authors.initials: P
authors.lastname: Kubán
authors.forename: Pavlína
authors.initials: P
authors.lastname: Pelcová
authors.forename: Vlastimil
authors.initials: V
authors.lastname: Kubán
authors.forename: Lenka
authors.initials: L
authors.lastname: Klakurková
authors.forename: Purnendu K
authors.initials: PK
authors.lastname: Dasgupta
mesh_terms: D002411:Cation Exchange Resins / Q000737:chemistry*; D002412:Cations / Q000032:analysis; D002852:Chromatography, Ion Exchange / Q000295:instrumentation* / Q000379:methods*; D006112:Gravitation; D008672:Metals, Alkali / Q000032:analysis; D008673:Metals, Alkaline Earth / Q000032:analysis; D010316:Particle Size; D011109:Polymethacrylic Acids / Q000737:chemistry; D012680:Sensitivity and Specificity; D012822:Silicon Dioxide / Q000737:chemistry; D013499:Surface Properties; D013696:Temperature; D013997:Time Factors
chemical_list: D002411:Cation Exchange Resins; D002412:Cations; D008672:Metals, Alkali; D008673:Metals, Alkaline Earth; D011109:Polymethacrylic Acids; D012822:Silicon Dioxide; C068872:polybutyl methacrylate