Angela M. Zapata

Detection of biological and chemical agents using differential mobility spectrometry (DMS) technology

With international concern growing over the potential for chemical and biological terrorism, there is an urgent need for a sensor that can quickly and accurately detect chemical and biological agents. Such a sensor needs to be portable, robust, and sensitive, with fast sample analysis time. We will demonstrate the use of a micromachined differential mobility spectrometer (DMS) with these characteristics that can detect multiple agents simultaneously on a time scale of seconds. In this study, we have demonstrated the ability of the DMS to detect Bacillus subtilis spores, a surrogate for Bacillus anthracis spores, the causative agent of anthrax. Pyrolysis was used as the sample introduction method to volatilize the spores before introducing material into the DMS. Additionally, we examined the effect of pyrolysis on B. subtilis spores suspended in sterile water using SDS-PAGE. These experiments showed that the spores must be heated at 650/spl deg/C or greater for 5 s or at 550/spl deg/C for at least 10 s to be fragmented into particles considerably smaller than 10 kDa, which the DMS can detect. Several major biomarkers can be easily distinguished above the background of the sterile water in which the spores are suspended, and we hypothesize that additional biomarkers could be liberated by further optimizing conditions. The DMS also has shown promise as a detector for chemical weapon agents, and we have demonstrated the ability of the DMS to detect nerve and blister agent simulants at clinically relevant levels.

Fluid damping in resonant flexural plate wave device

Fluid damping models are developed for resonant (standing wave) flexural plate wave (FPW) devices, which are rectangular plates or diaphragms with structural layers, a piezoelectric layer, and interdigitated conducting combs for driving and sensing. This configuration is often used in micromechanical chemical, biological, or nonvolatile residue sensors. Where much of the previous work on fluid effects in FPW devices focused on delay lines, this effort investigates resonant devices both analytically and experimentally. The fluid model is based on closed-form solution of a wide beam vibrating into a semi-infinite fluid volume and is mated directly into the beam equation. While the fluids pressure versus wave motion solution has been reported previously, the application to the resonant FPW is mathematically rigorous and leads to a greater understanding of the FPW damping regimes. Frequency responses of FPW devices constructed from silicon with deposited piezoelectric aluminum nitride and operating in water and alcohol compared well with analytic results with some discrepancies noted.

Micro-machined planar field asymmetric ion mobility spectrometer as a gas chromatographic detector.

A planar high field asymmetric waveform ion mobility spectrometer (PFAIMS) with a micro-machined drift tube was characterized as a detector for capillary gas chromatography. The performance of the PFAIMS was compared directly to that of a flame ionization detector (FID) for the separation of a ketone mixture from butanone to decanone. Effluent from the column was continuously sampled by the detector and mobility scans could be obtained throughout the chromatographic analysis providing chemical inforrmation in mobility scans orthogonal to retention time. Limits of detection were approximately I ng for measurement of positive ions and were comparable or slightly better than those for the FID. Direct comparison of calibration curves for the FAIMS and the FID was possible over four orders of magnitude with a semi-log plot. The concentration dependence of the PFAIMS mobility scans showed the dependence between ion intensity and ion clustering, evident in other mobility spectrometers and atmospheric pressure ionization technologies. Ions were identified using mass spectrometry as the protonated monomer and the proton bound dimer of the ketones. Residence time for column effluent in the PFAIMS was calculated as approximately 1 ms and a 36% increase in extra-column broadening versus the FID occurred with the PFAIMS.

Micromachined silicon plates for sensing molecular interactions

A micromachined surface stress sensor based on a thin suspended crystalline silicon circular plate measures differential surface stress changes associated with vapor phase chemisorption of an alkanethiol self-assembled monolayer. The isolated face of the suspended silicon plate serves as the sensing surface treated with a receptor layer sensitive to a target molecule, in this case Au(111). Chemisorption of an alkanethiol on the gold coated silicon surfaces results in plate bending. Plate displacements, measured with a phase scanning interferometer, indicate a differential surface stress change

High Performance Micromachined Planar Field-Asymmetric Ion Mobility Spectrometers for Chemical and Biological Compound Detection

\Delta \sigma_s

A micromachined surface stress sensor with electronic readout

=-0.72 +/- 0.02 N m(-1) for 1-dodecanethiol.

Systems for differential ion mobility analysis

The micromachined Planar High Field Asymmetric Waveform Ion Mobility Spectrometer (PFAIMS) is a novel detector for chemical and biological sensing applications. This detector fills an unmet market need, providing spectrometer capabilities and extremely high sensitivity, at a cost comparable to stand-alone sensors. The PFAIMS is quantitative, and has detection limits down to the parts-per-trillion. The performance of the PFAIMS in a number of applications ranging from industrial to biomedical, where it is used as both a stand alone sensor, and as a gas chromatographic detector are demonstrated. These applications include the detection of xylene isomers and non-invasive medical diagnosis through breath analysis.

Non-invasive breath analysis using field asymmetric ion mobility spectrometry

A micromachined surface stress sensor has been fabricated and integrated off chip with a low-noise, differential capacitance, electronic readout circuit. The differential capacitance signal is modulated with a high frequency carrier signal, and the output signal is synchronously demodulated and filtered resulting in a dc output voltage proportional to the change in differential surface stress. The differential surface stress change of the Au(111) coated silicon sensors due to chemisorbed alkanethiols is Deltasigma(s) approximately -0.42+/-0.0028 N m(-1) for 1-dodecanethiol (DT) and Deltasigma(s) approximately -0.14+/-0.0028 N m(-1) for 1-butanethiol (BT). The estimated measurement resolution (1 Hz bandwidth) is approximately 0.12 mN m(-1) (DT: 0.2 pg mm(-2) and BT: 0.8 pg mm(-2)) and as high as approximately 3.82 microN m(-1) (DT: 8 fg mm(-2) and BT: 24 fg mm(-2)) with system optimization.