By combining the high selectivity of a gas chromatograph (GC) with the high sensitivity and decent selectivity of an ion mobility spectrometer (IMS), GC-IMS have become increasingly popular in many applications. However, most GC suffer from long analysis times. In contrast, an hyper-fast GC allows for extremely fast analysis in the tens of seconds while reaching comparably high resolution.
View Article and Find Full Text PDFBesides safety and security applications, ion mobility spectrometry (IMS) is increasingly used in other fields such as medicine, environmental monitoring and food quality analysis. However, some applications require gas chromatographic separation before analysis by IMS. Furthermore, different compounds in the sample may form positive or negative ions during ionization and therefore simultaneous detection of both ion polarities is highly beneficial to avoid two chromatographic runs of the same sample.
View Article and Find Full Text PDFFast chromatography systems especially developed for high sample throughput applications require sensitive detectors with a high repetition rate. These high throughput techniques, including various chip-based microfluidic designs, often benefit from detectors providing subsequent separation in another dimension, such as mass spectrometry or ion mobility spectrometry (IMS), giving additional information about the analytes or monitoring reaction kinetics. However, subsequent separation is required at a high repetition rate.
View Article and Find Full Text PDFIn this paper, we present a new electron capture detector based on a compact X-ray tube (X-ECD) for electron generation by soft X-ray radiation instead of using a radioactive source. ECDs are commonly used in many laboratories as standard GC detectors since their invention in the 1950s, especially for highly sensitive detection of halogenated substances, pesticides or other environmental pollutants. However, due to unsatisfactory alternatives, many ECDs are still used with radioactive β-emitters, which is difficult and expensive in most applications today due to legal restrictions.
View Article and Find Full Text PDFIn this work, we present a tandem ion mobility spectrometer (IMS) utilizing a highly efficient ion manipulator allowing to store, manipulate, and analyze ions under high electric field strengths and controlled ion-neutral reactions at ambient conditions. The arrangement of tandem drift regions and an ion manipulator in a single drift tube allows a sequence of mobility selection of precursor ions, followed by storage and analysis, mobility separation, and detection of the resulting product ions. In this article, we present a journey exploring the capabilities of the present instrument by a study of eight different primary alcohols characterized at reduced electric field strengths / of up to 120 Td with a water vapor concentration ranging from 40 to 540 ppb.
View Article and Find Full Text PDFHigh Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) are usually operated at absolute pressures around 20 mbar in order to reach high reduced electric field strengths of up to 120 Td for influencing reaction kinetics in the reaction region. Such operating points significantly increase the linear range and limit chemical cross sensitivities. Furthermore, HiKE-IMS enables ionization of compounds normally not detectable in ambient pressure IMS, such as benzene, due to additional reaction pathways and fewer clustering reactions.
View Article and Find Full Text PDFHere, we present a new and an easy to assemble dielectric barrier discharge plasma ionization source based on printed circuit boards with two parallel isolated electrodes for generating a plasma inside an inert fused silica capillary. For demonstration, this plasma source is coupled to an ion mobility spectrometer. With two different sample gas feeds the analytes can either pass through the plasma or bypass the plasma before entering the reaction region of the ion mobility spectrometer, allowing for different ionization pathways, e.
View Article and Find Full Text PDFAlthough aniline is a relatively simple small molecule, the origin of its two peaks observed in ion mobility spectrometry (IMS) has remained under debate for at least 30 years. First hypothesized as a difference in protonation site (amine benzene ring), each ion mobility peak differs by one Dalton when coupled with mass spectrometry where the faster mobility peak is the molecular ion peak, and the slower mobility peak is protonated. To complicate the deconvolution of structures, some previous literature shows the peaks as unresolved and thus proposes these species exist in equilibrium.
View Article and Find Full Text PDFEfficient ionization of analyte molecules is a crucial step for the outstanding sensitivity of ion mobility spectrometers (IMS) used for trace gas detection. Here, we present a new ion source that combines the previously published extended field switching ion shutter with two switchable ionization sources and an optimized sample gas flow that leads to a focused laminar stream through the reaction region of the ion source. The X-ray ionization source allows for chemical gas phase ionization of analyte molecules, while the UV ionization source allows for direct ionization of analyte molecules.
View Article and Find Full Text PDFHigh Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) chemically ionize gaseous samples via reactant ions and separate the generated ions by their motion in a neutral gas under the influence of an electric field. Operation at reduced pressures of 10-40 mbar allows for reaching high reduced electric field strengths (/) of up to 120 Td. At these high /, the generated ions gain the namesake high kinetic energies, leading to a decrease in cluster size of the reactant ions by increasing the reaction rate of collision-induced cluster dissociation of hydrates.
View Article and Find Full Text PDFIon mobility spectrometers (IMS) are well suited for detecting trace gases down to levels at ppb and even ppt within 1 s of analysis time when using chemical ionization. The measuring principle is based on the separation and detection of the ionized constituents of a sample. Depending on the sample composition, certain ionization sources create both positive and negative analyte ions, but the simultaneous detection of both ion polarities usually requires two drift tubes.
View Article and Find Full Text PDFIons are separated in ion mobility spectrometry (IMS) by their characteristic motion through a gas-filled drift tube with a static electric field present. Chemical dynamics, such as clustering and declustering of chemically reactive systems, and physical parameters, as, for example, the electric field strength or background gas temperature, impact on the observed ion mobility. In high kinetic energy IMS (HiKE-IMS), the reduced electric field strength is up to 120 Td in both the reaction region and drift region of the instrument.
View Article and Find Full Text PDFClassical ion mobility spectrometers (IMS) operated at ambient pressure, often use atmospheric pressure chemical ionization (APCI) sources to ionize organic compounds. In APCI, reactant ions ionize neutral analyte molecules via gas-phase ion-molecule reactions. The positively charged reactant ions in purified, dry air are HO, NO, and O.
View Article and Find Full Text PDFIn a previous work, we explored zone broadening and the achievable plate numbers in linear drift tube ion mobility-mass spectrometry through developing a plate-height model [1]. On the basis of these findings, the present theoretical study extends the model by exploring peak-to-peak resolution and peak capacity in ion mobility separations. The first part provides a critical overview of chromatography-influenced resolution equations, including refinement of existing formulae.
View Article and Find Full Text PDFPrinted circuit board (PCB) based drift tube ion mobility spectrometers enable the use of state-of-the-art production techniques to manufacture compact devices with excellent performance at minimum cost. The new PCB ion mobility spectrometer (PCB-IMS) presented here is equipped with either a 140 MBq tritium or a 95 MBq nickel-63 ionization source and consists of a combination of horizontally arranged 6-layer PCBs for the drift and reaction regions and vertically arranged PCBs for interfacing the ionization source, ion shutter, and detector. The design allows the reproducible manufacturing and thus comparison of different IMS topologies.
View Article and Find Full Text PDFIon mobility spectrometry is a powerful detection method widely used in various applications. Particularly in field applications, ion mobility spectrometers (IMSs) are useful because of their extremely low detection limits at short measuring periods and their compact and robust design. However, especially small IMSs suffer from the consequences of low resolving power when compared to laboratory systems.
View Article and Find Full Text PDFIon mobility spectrometers (IMS) separate ions mainly by ion-neutral collision cross section and to a lesser extent by ion mass and effective temperature. When investigating isotopologues, the difference in collision cross section can be assumed negligible. Since the mobility shift of isotopologues is thus mainly caused by their difference in mass and effective temperature, the investigation of isotopologues can provide important insights into the theory of ion mobility.
View Article and Find Full Text PDFIn High Kinetic Energy Ion Mobility Spectrometry (HiKE-IMS), ions are formed in a reaction region and separated in a drift region, which is similar to classical drift tube ion mobility spectrometers (IMS) operated at ambient pressure. However, in contrast to the latter, the HiKE-IMS is operated at a decreased background pressure of 10-40 mbar and achieves high reduced electric field strengths of up to 120 Td in both the reaction and the drift region. Thus, the HiKE-IMS allows insights into the chemical kinetics of ion-bound water cluster systems at effective ion temperatures exceeding 1000 K, although it is operated at the low absolute temperature of 45 °C.
View Article and Find Full Text PDFIon mobility spectrometers (IMS) with field switching ion shutters are an excellent choice for trace gas detection, being extremely sensitive while having fast response times. However, as different target molecules may form positive, negative, or even ions of both polarities, it is beneficial to simultaneously detect both ion polarities. Here, we present a dual drift tube IMS with a new dual field switching ion shutter for gating both ion polarities and an X-ray ionization source in orthogonal configuration.
View Article and Find Full Text PDFIn the past decade, ion mobility spectrometry (IMS) in combination with mass spectrometry (IM-MS) became a widely employed technique for the separation and structural characterization of ionic species in the gas phase. Similarly to chromatography, where studies on the mechanism of band broadening and adequate plate-height equations have been aiding method development and promoting advancements in column technology, a suitable resolving power theory of drift tube ion mobility-mass spectrometry (DTIM-MS) is essential to stimulate further progress in this emerging field of separation science. In the present study, therefore, we explore dispersion processes in detail and present a plate-height model of ion mobility-mass spectrometry.
View Article and Find Full Text PDFJ Am Soc Mass Spectrom
September 2020
Due to the operation at background pressures between 10-40 mbar and high reduced electric field strengths of up to 120 Td, the ion-molecule reactions in High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) differ from those in classical ambient pressure IMS. In the positive ion polarity mode, the reactant ions H(HO), O(HO), and NO(HO) are observed in the HiKE-IMS. The relative abundances of these reactant ion species significantly depend on the reduced electric field strength in the reaction region, the operating pressure, and the water concentration in the reaction region.
View Article and Find Full Text PDFJ Am Soc Mass Spectrom
July 2020
High Kinetic Energy Ion Mobility Spectrometers (HiKE-IMS) are usually operated at an absolute pressure of 20 mbar reaching high reduced electric field strengths of up to 125 Td for controlled reaction kinetics. This significantly increases the linear range and limits chemical cross sensitivities. Furthermore, HiKE-IMS enables the ionization of compounds normally not detectable in ambient pressure IMS, such as benzene, due to new reaction pathways and the inhibition of clustering reactions.
View Article and Find Full Text PDFIn contrast to classical Ion Mobility Spectrometers (IMS) operating at ambient pressure, the High Kinetic Energy Ion Mobility Spectrometer (HiKE-IMS) is operated at reduced pressures of between 10 and 40 mbar and higher reduced electric field strengths of up to 120 Td. Thus, the ion-molecule reactions occurring in the HiKE-IMS can significantly differ from those in classical ambient pressure IMS. In order to predict the ionization pathways of specific analyte molecules, profound knowledge of the reactant ion species generated in HiKE-IMS and their dependence on the ionization conditions is essential.
View Article and Find Full Text PDFIn contrast to classical ion mobility spectrometers (IMS) operating at ambient pressure, the high kinetic energy ion mobility spectrometer (HiKE-IMS) is operated at reduced pressures between 10-40 mbar. In HiKE-IMS, ions are generated in a reaction region before they are separated in a drift region. Due to the operation at reduced pressure, it is possible to reach high reduced electric field strengths up to 120 Td in both the reaction as well as drift region, resulting in a pronounced decrease in chemical cross sensitivities and a significant enhancement of the dynamic range.
View Article and Find Full Text PDF