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Plistil A.,VICI Valco Instruments | Barnett H.E.,VICI Valco Instruments | Tolley H.D.,Brigham Young University | Stearns S.D.,VICI Valco Instruments
Analytical Chemistry

In this work, a novel splitless nanoflow gradient generator integrated with a stop-flow injector was developed and evaluated using an on-column UV-absorption detector. The gradient pumping system consisted of two nanoflow pumps controlled by micro stepper motors, a mixer connected to a serpentine tube, and a high-pressure valve. The gradient system weighed only 4 kg (9 lbs) and could generate up to 55 MPa (8000 psi) pressure. The system could operate using a 24 V DC battery and required 1.2 A for operation. The total volume capacity of the pump was 74 μL, and a sample volume of 60 nL could be injected. The system provided accurate nanoflow rates as low as 10 nL/min without employing a splitter, making it ideal for capillary column use. The gradient dwell volume was calculated to be 1.3 μL, which created a delay of approximately 4 min with a typical flow rate of 350 nL/min. Gradient performance was evaluated for gradient step accuracy, and excellent reproducibility was obtained in day-to-day experiments (RSD < 1.2%, n = 4). Linear gradient reproducibility was tested by separating a three-component pesticide mixture on a poly(ethylene glycol) diacrylate (PEGDA) monolithic column. The retention time reproducibility was very good in run-to-run experiments (RSD < 1.42%, n = 4). Finally, excellent separation of five phenols was demonstrated using the nanoflow gradient system. © 2015 American Chemical Society. Source

Sharma S.,Brigham Young University | Tolley L.T.,Southern Illinois University Carbondale | Tolley H.D.,Brigham Young University | Plistil A.,VICI Valco Instruments | And 2 more authors.
Journal of Chromatography A

Over the last four decades, liquid chromatography (LC) has experienced an evolution to smaller columns and particles, new stationary phases and low flow rate instrumentation. However, the development of person-portable LC has not followed, mainly due to difficulties encountered in miniaturizing pumps and detectors, and in reducing solvent consumption. The recent introduction of small, non-splitting pumping systems and UV-absorption detectors for use with capillary columns has finally provided miniaturized instrumentation suitable for high-performance hand-portable LC. Fully integrated microfabricated LC still remains a significant challenge. Ion chromatography (IC) has been successfully miniaturized and applied for field analysis; however, applications are mostly limited to inorganic and small organic ions. This review covers advancements that make possible more rapid expansion of portable forms of LC and IC. © 2015 Elsevier B.V. Source

Sharma S.,Brigham Young University | Plistil A.,VICI Valco Instruments | Simpson R.S.,VICI Valco Instruments | Liu K.,Brigham Young University | And 3 more authors.
Journal of Chromatography A

Liquid chromatography (LC) has lagged behind gas chromatography (GC) in developments related to hand-portable instrumentation. In this work, a new battery-operated (24V DC) nano-flow pumping system with a stop-flow injector was developed and integrated with an on-column UV-absorption detector (254nm) that was reduced in size to an acceptable weight and power usage for field operation. The pumping system, which includes nano-flow pump, stepper motor and high-pressure valve weighs only 1.372kg (3lbs) and can generate up to 110.32MPa (16,000psi) pressure. A major advantage of this pump is that it does not employ a splitter, since it was specifically designed for capillary column use. The volume capacity of the pump is 24μL, and a sample volume as low as 10nL can be injected. Flow rate calibration (300nL to 6.12μL per min) was performed, and an accuracy >99.94% was obtained. The percent injection carry-over was found to be low (RSD 0.31%), which makes it practical for quantitative analysis. The detector linear range and limit of detection (LOD) were determined using sodium anthraquinone-2-sulfonate. A linear regression coefficient (R) of 0.9996 was obtained for a plot of log peak area versus log concentration over the range of 3.2μM to 6.5mM, and the LOD (S/N=3) was found to be 7.8fmol (0.13μM). The short term noise of the detector is comparable to commercially available detectors (~10-5AU). In this work, the system was tested in the laboratory using regular line power (120V AC) with an AC to DC adapter. Reversed-phase isocratic separations were performed using a 15.5cm×75μm i.d. fused silica capillary column containing a monolithic stationary phase synthesized from 1,6-hexanediol dimethacrylate. Good retention time repeatability (RSD 0.09-0.74%) was obtained for a mixture containing an unretained marker (i.e., uracil) and a homologous series of alkyl benzenes. © 2013 Elsevier B.V.. Source

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