High voltage pulser for ion shutters in ion mobility spectrometry based on an optocoupler.

A novel high voltage pulser for an ion shutter used in drift-tube ion-mobility spectrometers is described. The simple design suitable for the in-house construction of these spectrometers relies on a special optocoupler to isolate the triggering circuitry from the high voltage at the ion shutter. The device was tested with an electrospray-ionization ion-mobility device with a 10 cm drift tube operated at 4 kV into which a standard test mixture of four tetraalkylamines was injected with a negative going gating pulse of about 50 V on top of 4 kV. A fall time of 15.7 µs and a rise time of 2.0 µs were determined for the pulse, which was adequate for the required injection pulse width of 450 µs. Resolving powers between 61 and 81 were determined for the four quaternary amines, which were found to be comparable to the performance obtained with a previously reported pulser circuitry of a different design used as a reference.

Determination of tobramycin in eye drops with an open-source hardware ion mobility spectrometer.

The analysis of tobramycin was demonstrated successfully as an example for electrospray ionization on an open-source hardware ion mobility spectrometer. This instrument was assembled inexpensively in-house, and required only very few purpose-made components. The quantitative determination of tobramycin required 20 s for a reading. The calibration curve for the range from 50 to 200 µM was found to be linear with a correlation coefficient of r = 0.9994. A good reproducibility was obtained (3% relative standard deviation) and the limit of detection was determined as 8 µM. As the concentration of the active ingredient in the eye drops (ophthalmic solutions) is too high for the sensitivity of the instrument, the samples had to be diluted appropriately.

Ambient ionization source based on a dielectric barrier discharge for direct testing of pharmaceuticals using ion mobility spectrometry.

The instrument is based on a miniature plasma source mounted at an oblique angle close to the injection gate of the ion mobility spectrometer. The plasma torch consists of two 5 mm wide external cylindrical electrodes, 10 mm apart, which are placed coaxially around a fused silica tube (1.5 mm i.d. and 3.0 mm o.d.). A small helium plasma is created by applying a alternating voltage of 8 kV at 28 kHz and employed for the direct desorption and ionization of solid or liquid samples, which are placed on an electrically isolated support. The separation section of the ion mobility spectrometer has a drift tube of 10 cm length and an applied high voltage of 4 kV. The instrument was built in-house at low cost and can easily be duplicated. Its usefulness was demonstrated by the rapid identification of five different pharmaceutical drugs, namely acetaminophen, loratadine, norfloxacin, tadalafil, thiamine as well as caffeine in ground coffee beans.

Development of simple drift tube design for ion mobility spectrometry based on flexible printed circuit board material.

A study on the use of flexible printed circuit board material for the construction of drift tubes for ion mobility spectrometry is reported. This is significantly less complicated than the conventional approach based on stacked electrode and insulator rings, as the material can simply be rolled up to obtain a string of circular electrodes. The size and spacing of the electrodes was found to have a strong effect on the resolving power. For an optimized geometry with electrodes of 1.5 mm width at a pitch of 3.5 mm resolving powers of up to 80 were achieved for quaternary amines introduced by electrospray ionization into a drift tube of 10 cm length and an applied voltage of 4200 V. This performance was found to be comparable to that of a conventional drift tube based on stacked rings with otherwise identical geometry and operating conditions. The entire instrument was constructed in-house. Its utility was demonstrated with the determination of the C12, C14 and C16 benzalkonium ions in several commercial cleaning products with limits of detection of 20, 25, and 38 µg L-1, respectively.

Contactless conductivity sensor employing moist paper as absorbent for in-situ detection of generated carbon dioxide gas.

This work presents an unconventional use of capacitively coupled contactless conductivity detector (C4D) for detection of gas absorption by moist paper with potential application for chemical analysis. To be suitable for measuring conductivity of moist paper absorbent, the C4D sensor was therefore designed in planar configuration. A layer of dry filter paper, only 20 mm × 25 mm in size, was placed on the C4D sensor and the device installed inside a specifically designed vaporization chamber. A vial (16 mm i.d., 8 mm high) containing a 150-µL solution of sodium bicarbonate was placed alongside. The filter paper was loaded with 110 µL of deionized water through an injection hole in the cover lid. A 100-µL aliquot of 2 M hydrochloric acid solution was directly dispensed into the vial through a second hole in the lid to generate CO2 gas from the bicarbonate solution. It was observed that the C4D sensor gave real-time response that corresponded to the absorption of the gas and subsequent production of H+ and HCO3- in the moist paper. The monitored signal reached a constant value at 160 s after the addition of the acid. Chemistry of the absorption process and equivalent circuit for the C4D are proposed. Direct measurement of cement powder was chosen to demonstrate the potential use of this device for quantifying the CaCO3 content of the cement. The calibration curve for 0.5-3 mg CaCO3 was linear for signals recorded at 160 s: Vdc = (0.172 ± 0.005) · (mg CaCO3) + (0.016 ± 0.009), with coefficient of determination of 0.9965. Linear calibrations were also observed when the signals were monitored at various time less than 160 s. The limit of quantitation (3 SD of intercept/slope) was 0.17 mg CaCO3. The method provided acceptable precision with %RSD of 4.6 (2 mg CaCO3, n = 10).

Contactless conductivity detector from printed circuit board for paper-based analytical systems.

This work presents a capacitively coupled contactless conductivity detector (C4D) etched out from a printed circuit board (PCB) as potential sensor for paper-based analytical systems. Two lines of any desirable pattern forming 35-µm thick planar copper electrodes were produced on a PCB plate (40 mm × 60 mm) by photolithography. The final PCB plate was covered with polypropylene film to serve as the insulating layer for the C4D detector. The film also protected the copper electrodes from corrosion. Electrodes made in this planar geometry make the PCB-C4D suitable as sensor for flat devices such as paper-based analytical devices. For this work, plain paper strips were employed as sample reservoir and as fluidic channel without hydrophobic pattern. A dried paper strip was first placed over the sensor, followed by dispensing a fixed volume of the liquid sample onto the paper. Entrapment of the liquid sample in the paper strip leads to reproducible size and position of the detection zone of the sample liquid for the capacitive coupling effect. High precision was obtained with %RSD ≤1% (n = 18) for standard solutions of KCl. Soil suspensions could be analyzed without prior filtration by placing a drop onto the paper strip extending away from the detector zone. The paper strip filtered out soil particles at the surface of the paper. Therefore, only soil filtrate moved towards the detection zone by lateral flow. The C4D detection using paper strip showed high tolerance to soil suspension with turbidity up to 6657 NTU, offering direct analysis of soil salinity. Cleaning with moist tissue paper between samples is adequate even for dirty samples such as soil suspension. We also monitored conductivity of acid-base reaction in the microfluidic paper channels, which was later applied to the quantification of bicarbonate in water and in antacid tablet ("Soda Mint Tablet").

Temperature-dependent schlieren effect in liquid flow for chemical analysis.

In flow analysis, such as flow injection analysis, liquid lens is formed at the boundary between two adjacent liquid media which have different refractive indices. Light refraction at the liquid interface gives the so-called 'schlieren signal'. Schlieren effect is both concentration-dependent and temperature-dependent. In this work, the schlieren signal from temperature difference was quantitatively investigated for application in enthalpimetric measurement. The schlieren phenomena was then exploited for chemical analysis. A thermal insulated single flow line manifold was constructed using deionized water at 23 °C as the carrier. Deionized water at various temperatures in the range of 5-85 °C was injected into the carrier flow. A correlation between the schlieren signal and sample temperature was observed. A heat exchanger unit (HEU), consisting of a small volume glass-reaction chamber with a surrounding water jacket, was constructed. The unit was thermally insulated in a double layer cylindrical PVC unit. For demonstrating the applicability of temperature-dependent schlieren effect in chemical analysis, the exothermic oxidation reaction between acid dichromate and ethanol or ascorbic acid was employed with heat transferring to the surrounding water layer. When an aliquot of water from the HEU is injected into the constant temperature flow line the observed schlieren signal was dependent on the analyte concentration. Linear calibration (r2 > 0.99) were obtained covering the concentration range of ethanol and ascorbic acid as found in samples. The developed flow system provides good precision (RSD < 5%) with sample throughput of 4 sample h-1. The system were applied to the determination of ethanol in Thai white spirit and ascorbic acid in vitamin C tablets, respectively. The quantitative results obtained from the schlieren method were in agreement with the comparative methods.