Low-cost Arduino controlled dual-polarity high voltage power supply.

Ion Mobility Spectrometry (IMS) provides low ppbv detection limits for gas-phase or aqueous analytes. These instruments rely an electric field to produce ion motion. This electric field is typically 200-600 V/cm with a 15 cm cell, requiring an HV source of 6-10 kV. In this work, we present a low-cost alternative for supplying this high voltage. Inexpensive, commercially available 0-20 kV HV modules are mapped to an analog 0-5 V input signal, controlled using an Arduino microcontroller and digital analog converter. Dual polarities are selectable through a front-panel switch and ramps potentials between settings to avoid damage to attached devices.

Optical and mass spectral characterization of the electrospray ionization/corona discharge ionization interface.

The interchange between electrospray ionization (ESI) and corona discharge ionization (CDI) with respect to applied bias on the needle is customarily placed at the point where light production begins at the tip of the needle. If a liquid sample is flowing through a needle that is observed to produce light, the ionization process is assumed to be harsher and the term coronaspray ionization has been coined to describe this hybrid ionization mechanism. In this work, the transition between ESI and CDI is investigated with respect to applied bias through optical and mass spectrometric measurements. As a function of applied bias potential, the optical signal at the tip of the needle was recorded simultaneously with the resultant ionization products. In this effort, the production of ions from an electrospray ionization needle has been demonstrated to produce light regardless of bias if ions are also formed. With this understanding, an ESI/CDI needle was designed to allow the bias to be temporarily pulsed over the 'onset' voltage necessary for ionization and the rise and decay of the optical signal was measured. Positive mode CDI onset to a stable discharge state within 0.05 ms, while positive ESI required 1.9 ms to reach a stable condition. In the negative mode, the stability of the ionization process was highly variable in both ESI and CDI modes, though CDI was generally faster to reach the stable mode of operation. When the resultant ions were investigated, the effect of increased bias on an ESI needle was found to be species-dependent. Recognizing that the range of compounds probed was limited, for those examined, it appears that stable, non-labile species may be investigated via ESI under extremely high biases while labile species demonstrate a narrow range of stable biases before significant fragmentation occurs.

Improved ion mobility resolving power with increased buffer gas pressure.

Security and military applications of analytical techniques demand a small, rugged, reliable instrument that has traditionally been served well by atmospheric pressure ion mobility spectrometry (IMS) systems. Modern threats stipulate these instruments must reliably operate in increasingly complex environments. Previous work has demonstrated that increasing the pressure of an IMS drift tube has the potential to increase the resolving power of IMS, but operation at low temperatures resulted in a leveling of the measured resolving power as a function of pressure. By creating a novel aperture grid/Faraday plate design, a high-pressure IMS (HPIMS) system has been created that maintains a resolving power efficiency of 80% regardless of the pressure applied to the cell. This allows previously unattainable resolving powers to be achieved utilizing a small (10.7 cm) IMS cell. Using high pressure, a stand-alone IMS cell of 10.7 cm length has demonstrated a resolving power of 102 when operated at 2.5 atm. An increase in peak-to-peak resolution was also noted as pressure increased. Finally, the slope of the resulting inverse mobility/pressure curve for a single analyte has been shown to be proportional to the collision-cross-section of the analyte of interest, providing a novel method for the calculation of collision-cross-section of target ions from the HPIMS data.

Radiative ion-ion neutralization: a new gas-phase atmospheric pressure ion transduction mechanism.

All atmospheric pressure ion detectors, including photo ionization detectors, flame ionization detectors, electron capture detectors, and ion mobility spectrometers, utilize Faraday plate designs in which ionic charge is collected and amplified. The sensitivity of these Faraday plate ion detectors are limited by thermal (Johnson) noise in the associated electronics. Thus approximately 10(6) ions per second are required for a minimal detection. This is not the case for ion detection under vacuum conditions where secondary electron multipliers (SEMs) can be used. SEMs produce a cascade of approximately 10(6) electrons per ion impinging on the conversion dynode. Similarly, photomultiplier tubes (PMTs) can generate approximately 10(6) electrons per photon. Unlike SEMs, however, PMTs are evacuated and sealed so that they are commonly used under atmospheric pressure conditions. This paper describes an atmospheric pressure ion detector based on coupling a PMT with light emitted from ion-ion neutralization reactions. The normal Faraday plate collector electrode was replaced with an electrode "needle" used to concentrate the anions as they were drawn to the tip of the needle by a strong focusing electric field. Light was emitted near the surface of the electrode when analyte ions were neutralized with cations produced from the anode. Although radiative-ion-ion recombination has been previously reported, this is the first time ions from separate ionization sources have been combined to produce light. The light from this radiative-ion-ion-neutralization (RIIN) was detected using a photon multiplier such that an ion mobility spectrum was obtained by monitoring the light emitted from mobility separated ions. An IMS spectrum of nitroglycerin (NG) was obtained utilizing RIIN for tranducing the mobility separated ions into an analytical signal. The implications of this novel ion transduction method are the potential for counting ions at atmospheric pressure and for obtaining ion specific emission spectra for mobility separated ions.

Voltage sweep ion mobility spectrometry.

Ion mobility spectrometry (IMS) is a rapid, gas-phase separation technique that exhibits excellent separation of ions as a standalone instrument. However, IMS cannot achieve optimal separation power with both small and large ions simultaneously. Similar to the general elution problem in chromatography, fast ions are well resolved using a low electric field (50-150 V/cm), whereas slow drifting molecules are best separated using a higher electric field (250-500 V/cm). While using a low electric field, IMS systems tend to suffer from low ion transmission and low signal-to-noise ratios. Through the use a novel voltage algorithm, some of these effects can be alleviated. The electric field was swept from low to high while monitoring a specific drift time, and the resulting data were processed to create a 'voltage-sweep' spectrum. If an optimal drift time is calculated for each voltage and scanned simultaneously, a spectrum may be obtained with optimal separation throughout the mobility range. This increased the resolving power up to the theoretical maximum for every peak in the spectrum and extended the peak capacity of the IMS system, while maintaining accurate drift time measurements. These advantages may be extended to any IMS, requiring only a change in software.

High-pressure ion mobility spectrometry.

The effects of above-ambient pressure on ion mobility on resolving power, resolution, and ion current were investigated using a small, stand-alone ion mobility spectrometer (IMS). This work demonstrates the first example of ion mobility spectrometry at pressures above ambient. Ion mobility spectra of chemical warfare agent (CWA) stimulant dimethyl methylphosphonate (DMMP) and several other standard compounds are shown for superambient conditions. The IMS was operated at pressures from 700 to 4560 Torr. An optimal resolving power was obtained at a specific voltage as a function of pressure, with higher optimal resolving powers obtained at higher voltages, as predicted from standard IMS theory. At high pressures, however, resolving power did not increase as much as theory predicted, presumably due to ion clustering. Nevertheless, an increase in pressure was found to improve resolution in IMS. One example where high pressure improved resolution was the separation of cyclohexylamine (K(0) = 1.83) and 2-hexanone (K(0) = 1.86) (where K(0) is the reduced mobility value). The product ions of these two compounds could not be separated at ambient pressure but could be nearly baseline separated when the pressure of the buffer gas was raised to 2280 Torr. Total ion current was also examined at pressures from ambient up to 4560 Torr. Total ion current, when investigated with pressure, was found to reach a maximum, initially rising with increased pressure.