ac503247g_si_001.pdf (172.19 kB)

Admittance Detector for High Impedance Systems: Design and Applications

Download (172.19 kB)
journal contribution
posted on 02.12.2014, 00:00 by Min Zhang, Brian N. Stamos, Purnendu K. Dasgupta
We describe an admittance detector for high impedance systems (small capillary bore and/or low solution specific conductance). Operation in the low frequency range (≤1 kHz, much lower than most relevant publications) provides optimum response to conductance changes in capillaries ≤20 μm in bore. The detector design was based on studies described in a preceding companion paper (Zhang, M.; Stamos, B. N.; Amornthammarong, N.; Dasgupta, P. K. Anal. Chem. 2014, 86, DOI 10.1021/ac503245a.). The highest S/N for detecting 100 μM KCl (5.5 μM peak concentration, ∼0.8 μS/cm) injected into water flowing through a capillary of 7.5 μm inner radius (r) was observed at 500–750 Hz. A low bias current operational amplifier in the transimpedance configuration permitted high gain (1 V/nA) to measure pA–nA level currents in the detection cell. Aside from an oscillator, an offset-capable RMS-DC converter formed the complete detection circuitry. Limits of detection (LODs) of KCl scaled inversely with the capillary cross section and were 2.1 and 0.32 μM injected KCl for r = 1 and 2.5 μm capillaries, respectively. When used as a detector on an r = 8 μm bore poly­(methyl methacrylate) capillary in a split effluent stream from a suppressed ion chromatograph, the LOD was 27 nM bromide (Vex 22 V p-p), compared to 14 nM observed with a commercial bipolar pulse macroscale conductivity detector with an actively thermostated cell. We also show applications of the detector in electrophoresis in capillaries with r = 1 and 2.5 μm. Efficient heat dissipation permits high concentrations of the background electrolyte and sensitive detection because of efficient electrostacking.