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A method for evaluating the interactions between metal ions and nonionic surfactants in aqueous solutions containing high-concentration HCl, using gas pressure-driven low-pressure high-performance liquid chromatography (LP-HPLC) as a highly acid-resistant HPLC system, was developed. To construct the LP-HPLC for this purpose, poly(styrene- co-divinylbenzene)-based low-flow-resistance monolithic columns tolerant to highly acidic conditions were prepared using low-conversion thermal polymerization. Thermal polymerization at 65 °C for 1.5 h (monomer conversions, 33 % for styrene and 59 % for divinylbenzene) allowed preparation of a column with both high separation efficiency (around 60,000 plates m for alkylbenzenes) and a quite low back pressure of 0.14 MPa at a linear flow rate of 1 mm s (2.8 × 10 m in permeability). The base column prepared under the above conditions was coated with a nonionic surfactant, polyoxyethylene nonylphenyl ether (PONPE, average oxyethylene unit numbers ( n) = 3, 7.5, 15, and 20), and used for evaluation of the interactions between PONPEs and metal ions in 6 M HCl. The interactions between PONPEs and Au(III), Ga(III), Fe(III), Zn(II), and Cu(II) were successfully evaluated using both breakthrough and chromatographic methods. Furthermore, a study of the effect of the polyoxyethylene (POE) chain length revealed that the use of PONPE with the longer POE moiety enhanced the magnitude of the interaction together with the increase in the amount of oxyethylene (OE) units coated on the monolith. Moreover, the interactions of metal ions with a single OE unit were almost constant in the range of n = 7.5-20, whereas the suppression of the interaction between Au(III) with the shortest PONPE chain ( n = 3) was also observed. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Voltage-induced impedance variation of the minicolumn (i.d. 0.53 mm, length 2 mm) packed with cation exchanger was investigated to develop a sensing method. An aqueous sample solution containing the metal cations was continuously supplied to the minicolumn during the impedance measurement with the simultaneous application of both alternating current voltage (amplitude, 1.0 V; frequency, 200 kHz to 6 Hz) and direct current (DC) offset voltage (0.1 to 1.0 V). On a complex plane plot, the profile of the column impedance consisted of a semicircle (200 kHz to 100 Hz) and a straight line (<100 Hz), of which slope varied with the magnitude of the applied DC offset voltage ( VDC). The slope– VDC relation depended on the kind of the metal cation and its concentration; in particular, the slope– VDC relations of monovalent cations (Na+ and K+) and divalent ones (Mg2+ and Ca2+) were significantly different. With the change in the concentration of minor divalent salt of MgCl2 or CaCl2 (60 to 140 μM) in the sample solution containing 10 mM NaCl, the slopes showed almost linear relationships between those with application of VDC = 0.1 V and 1.0 V both for magnesium and calcium additions. In the case of plural addition of both MgCl2 and CaCl2 to the solution, the data points in the slope0.1 V–slope1.0 V plot were located between the two proportional lines for single additions of magnesium and calcium, reflecting both the mixing ratio and net concentrations of the divalent cations. Thus, simulations determination of Mg2+ and Ca2+ can be attained on the basis of the slope0.1 V–slope1.0 V relation obtained by the impedance measurements of the minicolumn. Actually, the contents of both magnesium and calcium cations in the bottled mineral waters determined simultaneously using the proposed method were almost equivalent to those obtained by the atomic absorption spectrometric measurement. [ABSTRACT FROM AUTHOR]