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1.
Anal Chem ; 79(1): 215-23, 2007 Jan 01.
Article in English | MEDLINE | ID: mdl-17194142

ABSTRACT

The fundamental aspects and the capillary electrophoresis usage of thermal marks are presented. The so-called thermal mark is a perturbation of the electrolyte concentration generated by a punctual heating of the capillary while the separation electric field is maintained. The heating pulse is obtained by powering tungsten filaments or surface mount device resistors with 5 V during a few tens to hundreds of milliseconds. In the proposed model, the variation of the transport numbers with the rising temperature leads to the formation of low- and high-concentration regions during the heating. After cooling down, the initial mobilities of the species are restored and these regions (the thermal mark) migrate chiefly due to the electroosmotic flow (EOF). The mark may be recorded with a conductivity detector as part of a usual electropherogram and be used to index the analyte peaks and thus compensate for variations of the EOF. In a favorable case, 10 mmol/L KCl solution, the theory suggests that the error in the measurement of EOF mobility by this mean is only -6.5 x 10(-7) cm2 V-1 s-1. The method was applied to the analysis of alkaline ions in egg white, and the relative standard deviations of the corrected mobilities of these ions were smaller than 1%. This is a challenging matrix, because albumin reduces the EOF to 20% of its initial value after 11 runs. The combination of thermal mark, electrolysis separated, and contactless conductivity detection allowed the measurement of the EOF of a silica capillary with unbuffered KCl solution with constant ionic strength. The overall approach is advantageous, because one can easily control the chemical composition of the solution in contact with the inner surface of the capillary.

2.
Anal Chem ; 75(15): 3853-8, 2003 Aug 01.
Article in English | MEDLINE | ID: mdl-14572053

ABSTRACT

A new microfabrication process based on a xerographic process is described. A laser printer is used to selectively deposit toner on a polyester film, which is subsequently laminated against another polyester film. The toner layer binds the two polyester films and allows the blank regions to become channels for microfluidics. These software-outlined channels are approximately 6 microm deep. Approximately twice this depth is obtained by laminating two printed films. The resulting devices were not significantly damaged after 24 h of exposure to aqueous solutions of H3PO4, NaOH, methanol, acetonitrile, or sodium dodecyl sulfate. Electric tests with an impedance analyzer and microchannels filled with KCl solution demonstrated that (1) wide channels suffer from deformation of the top and bottom walls due to the lamination of the polyester films and (2) the toner walls are somewhat porous. Although these drawbacks limit the maximum width of a channel and the minimum distance between two channels, the process is an attractive option to other expensive, laborious, and time-consuming methods for microchannels fabrication. The process has been used to implement devices for electrospray tip and capillary electrophoresis with contactless conductivity detection.

3.
Anal Chem ; 74(14): 3274-80, 2002 Jul 15.
Article in English | MEDLINE | ID: mdl-12139029

ABSTRACT

A nongravimetric quartz crystal resonator for determination of boron was proposed. The key step is the preparation of a polymer that forms a complex with boron (from borate ion). The polymeric film is deposited on one face of an electrode-separated quartz crystal. The backbone of the polymer is poly(epichlorohydrin), which is modified to anchor N-methyl-D-glucamine. After reticulation and reduction, the film presents high stability and sensitivity to boron at pH 8.5. A carrier solution containing 50 mM EDTA ensures high conductivity and the elimination of several interfering metal ions. Boron is strongly retained by the film, and a positive shift of the oscillating frequency is proportional to its concentration. Boron is eluted with 1 mL of a 1 M mannitol solution. For a 0.160-mL sample loop and concentration up to 600 microM, the calibration sensitivity was 1.67 Hz/microM and the LOD was 2 microM. This limit could be lowered to 0.3 microM by using a 1.00-mL sample loop. In both cases, it was possible to detect 3 ng of boron. It was estimated that the nongravimetric sensor is at least 10 times more sensitive that a hypothetical gravimetric sensor.

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