Developing powerful hand-held drift tube ion mobility spectrometers (IMS) requires small, lightweight drift tubes with high analytical performance. In this work, we present an easy-to-manufacture, miniaturized drift tube ion mobility spectrometer, which is manufactured from polyether ether ketone, stainless steel foils and printed circuit boards. It is possible to operate the drift tube IMS with a radioactive 3 H ionization source or a non-radioactive X-ray ionization source with 3 kVacceleration voltage. The drift tube design provides high resolving power of R p = 63 at a drift length of just 40 mm, 15 mm × 15 mm in cross-section (outer dimensions) and a drift voltage of 2.5 kV. The limits of detection for less than one second of averaging are 40 ppt v for dimethylmethylphosphonate and 30 ppt v for methyl salicylate. For demonstration, the miniaturized drift tube IMS is integrated into a stand-alone battery-powered mobile device, including a closed gas-loop, high performance driver electronics and wireless data transmission. In a proof-of-concept study, this device was tested in an international field evaluation exercise to detect the release of a volatile, hazardous substance inside a large entry hall.
The drift voltage required for operating ion mobility spectrometers implies high voltage isolation of either the ion source or the detector. Typically, the detector is grounded due to the sensitivity of the small ion currents to interferences and thus higher requirements for signal integrity than the ion source. However, for certain ion sources, such as non-radioactive electron emitters or electrospray ionization sources, or for coupling with other instruments, such as gas or liquid chromatographs, a grounded ion source is beneficial. In this paper, we present an isolated data acquisition interface using a 16 bit, 250 kilosamples per second analog to digital converter and fiber optic transmitters and receivers. All spectra recorded via this new data acquisition interface and with a grounded ion source show the same peak shapes and noise when compared with a grounded detector, allowing additional freedom in design.
Due to their high sensitivity and compact design, ion mobility spectrometers are widely used to detect toxic industrial chemicals (TICs) in air. However, when analyzing complex gas mixtures, classical ion mobility spectrometry (IMS) suffers from false-positive rates due to limited resolving power or false-negative rates caused by competitive ion−molecule reactions and the resulting suppression of certain analyte ions. To overcome these limitations, high-kinetic energy IMS (HiKE-IMS) was introduced some years ago. In contrast to classical IMS, HiKE-IMS is operated at decreased pressures of 20•••60 mbar and high reduced electric field strengths E/N of up to 120 Td. Under these conditions, the influence of competitive ion−molecule reactions on the prevailing ion population should be less pronounced, thus reducing false negatives. Additionally, effects such as fragmentation and field-dependent ion mobility may help to reduce false positives. In this work, the capabilities and limitations of HiKE-IMS in the field of on-site detection of the volatile TICs NH 3 , HCN, H 2 S, HCl, NO 2 , Cl 2 , and SO 2 are evaluated for the first time. Based on the limits of detection and the extent of spectral and chemical cross-sensitivities in gas mixtures, the results obtained for HiKE-IMS are compared with those obtained for classical IMS. It is shown that HiKE-IMS is less sensitive in comparison to classical IMS. However, when used for TIC detection, the reduced sensitivity of HiKE-IMS is not a major drawback. With values around 1 ppm v , the achievable limits of detection for almost all TICs are below the AEGL-2 (4h) levels. Furthermore, in comparison to classical IMS, it is still striking that HiKE-IMS shows significantly less spectral and chemical cross-sensitivities and thus exhibits considerably lower false-positive and false-negative rates. Overall, it thus turns out that HiKE-IMS is a promising alternative to classical IMS in the field of on-site detection of TICs.
Ion 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. The dual field switching ion shutter allows significantly improved ion gating and ion accumulation due to improved shielding of the ionization region from the drift field. Equipped with two 75 mm long high-performance drift tubes, the dual IMS reaches high resolving power of R = 90 with detection limits in the lower pptv range for different ketones, chlorinated hydrocarbons and methyl salicylate that forms ions in both polarities.
Ion mobility spectrometers (IMS) are able to detect pptV-level concentrations of substances in gasses and in liquids within seconds. Due to the continuous increase in analytical performance and reduction of the instrument size, IMS are established nowadays in a variety of analytical field applications. In order to reduce the manufacturing effort and further enhance their widespread use, we have developed a simple manufacturing process for drift tubes based on a composite material. This composite material consists of alternating layers of metal sheets and insulator material, which are connected to each other in a mechanically stable and gastight manner. Furthermore, this approach allows the production of ion drift tubes in just a few steps from a single piece of material, thus reducing the manufacturing costs and efforts. Here, a drift tube ion mobility spectrometer based on such a composite material is presented. Although its outer dimensions are just 15 mm × 15 mm in cross section and 57 mm in length, it has high resolving power of Rp = 62 and detection limits in the pptV-range, demonstrated for ethanol and 1,2,3-trichloropropane.
A growing demand for low-cost gas sensors capable of detecting the smallest amounts of highly toxic substances in air, including chemical warfare agents (CWAs) and toxic industrial chemicals (TICs), has emerged in recent years. Ion mobility spectrometers (IMS) are particularly suitable for this application due to their high sensitivity and fast response times. In view of the preferred mobile use of such devices, miniaturized ion drift tubes are required as the core of IMS-based lightweight, low-cost, hand-held gas detectors. Thus, we evaluate the suitability of a miniaturized ion mobility spectrometer featuring an ion drift tube length of just 40 mm and a high resolving power of R p = 60 for the detection of various CWAs, such as nerve agents sarin (GB), tabun (GA), soman (GD), and cyclosarin (GF), as well as the blister agent sulfur mustard (HD), the blood agent hydrogen cyanide (AC) and the choking agent chlorine (CL). We report on the limits of detection reaching minimum concentration levels of, for instance, 29 pptv for sarin (GB) within an averaging time of only 1 s. Furthermore, we investigate the effects of precursors, simulants, and other common interfering substances on false positive alarms.
Split-ring resonators (SRR) are simple electrical circuits that show a significant shift in resonance frequency even with the smallest changes in split capacitance, and thus in permittivity, electric conductivity, and dielectric losses of the split capacitor’s dielectric. Usually, the resonance frequency is derived from the frequency response, but recording the frequency spectrum takes a certain amount of time. Here, we present a new capillary split-ring resonator CaSRR with fast readout for liquid chromatography (LC), which is capable of accurately detecting very fast changes in split capacity. The proposed method is based on the detection of the transmitted signal at a single frequency that is analyzed by demodulation. The demodulated signal changes its amplitude depending on the shift of the resonance frequency. Our simple low-cost electronics enables an average sampling rate of 42 Hz with 128 averages of the demodulated signal and has a frequency stability of 840 mHz. Thus, a minimum change in permittivity of Δεr,min = 11.26 × 10−3 can be detected. Finally, a chromatogram of one sugar (glucose) and one sugar alcohol (xylitol) is recorded using the SRR and is compared to a standard refractive index detector.
Ion mobility spectrometers (IMS) are well suited for detecting trace gases down to levels at ppb v and even ppt v 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. Contained within this effort, we present an alternative approach for detecting both ion polarities using one single drift tube that can switch the polarity of the drift tube within 12 ms. This technique allows for generating one positive and one negative ion mobility spectrum, each with a drift time range of 13 ms (minimum reduced ion mobility of K 0 = 0.72 cm 2 V −1 s −1 ), within a total experiment time of 50 ms. Additionally, ions are continuously generated in the ionization region during both the polarity switching and the analysis of one of the polarities, which allows for an effective ionization/reaction time of 25 ms. Comparable to the performance of similar instrument designs we reported previously, the presented device has a high resolving power of R P = 70 with a drift length of 51 mm. The limits of detection are for the monomers between 70 and 370 ppt v and for the dimers between 450 and 800 ppt v for 1 s of averaging for various ketones, methyl salicylate, and chlorinated hydrocarbons. Although this work focuses on applying ultra-fast polarity switching to an existing IMS, the techniques shown here may be applied to other IMS implementations for different applications.
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