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Discrimination of Combustion Fuel Sources Using Gas Chromatography-Planar Field Asymmetric-Waveform Ion Mobility Spectrometry

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Discrimination of Combustion Fuel Sources Using Gas Chromatography-Planar Field Asymmetric-Waveform Ion Mobility Spectrometry J. Sep. Sci. 2003, 26, 585–593 Eiceman, Tarassov, Funk, Hughs, Nazarov, Miller 585 Gary A. Eicemana), Discrimination of combustion fuel sources using Alexander Tarassova, 1), Paul A. Funkb), gas chromatography-planar field asymmetric- S. Edgar Hughsb) , waveform ion mobility spectrometry Erkinjon G. Nazarovc), c) Raanan A. Miller Smoke plumes from cotton, paper, grass, and cigarettes and emissions from a gas- oline engine were sampled using solid-phase microextraction (SPME) and samples a) Department of Chemistry were analyzed for volatile organic compounds (VOC) using gas chromatography- and Biochemistry mass spectrometry (GC-MS). Chemical compositions were sufficiently distinct to ([email protected]), allow source identification. Unfortunately, advanced smoke detectors based on GC- New Mexico State University, MS would be too slow and expensive for most applications. Direct sampling of smoke Las Cruces, NM 88003 b) USDA-ARS-SW Cotton by atmospheric pressure chemical ionization-mass spectrometry produced a complex Ginning Research Lab response, demonstrating that VOC in smoke were suitable for gas phase chemical ([email protected]), 300 E. ionization. The complexity also indicated the necessity of chromatographic prefractio- College Drive, PO Box 578, nation. Planar Field Asymmetric-waveform Ion Mobility Spectrometry (PFAIMS) as a Mesilla Park, NM 88047 capillary GC detector generated chemical information orthogonal to GC retention c) SIONEX Corporation times. The combination of SPME preconcentration and the additional information pro- ([email protected]), vided by the PFAIMS detector yielded unique patterns from smoke from each fuel. 300 Second Ave., Waltham, Reconstructed ion chromatograms extracted from the PFAIMS scans indicated suffi- MA 02451 cient resolution of chemical constituents could be completed in less than five minutes with little loss of analytical information. These first measurements suggest that a GC- PFAIMS instrument operating at ambient pressure in air might result in a compact and convenient fuel specific smoke alarm at a reasonable cost. Key Words: Gas chromatography; Ion mobility spectrometry; Volatile organic com- pounds; Smoke detector; Received: July 1, 2002; accepted: September 9, 2002 1 Introduction quently, present detectors can not discriminate between smoke sources. The benefits of smoke detectors for protection of human In some instances a false positive alarm is harmless. In life and property have been known for decades. These others, repeated false alarms can cause a loss in confi- detectors are now widely used in domestic, commercial, dence and/or reaction time. Examples of this include false and industrial structures. Two technologies of measure- alarms from diesel engine emissions in mine safety [1–3] ment are employed in modern consumer grade smoke and in certain naval ships [4–6]. False positives are the detectors. One measures ion flux from an alpha source focus of this work. False negatives have been addressed with a Faraday plate collector and the other measures by the addition of a gaseous CO sensor to a standard photon flux from a light-emitting diode with a photocell. In smoke detector since carbon monoxide is generated in both technologies, the diffusion of particles borne on most fires [7]. ambient air between the source and the Faraday plate or Original Paper the photocell is the basis for a positive alarm. Airborne One strategy to bring specificity to smoke detectors is particles interrupt the collection of ions or photons. Conse- modification of existing technologies. An example is the desensitization of CO sensors using nitric oxide to sup- Correspondence: Paul A. Funk, USDA-ARS-SW Cotton press response to carbon monoxide that arises from die- Ginning Research Lab, 300 E. College Drive, PO Box 578, sel engines in atmospheres of underground mines [3]. Mesilla Park, NM 88047, USA. Phone: +1 505 526 6381. Thus, the relatively low CO levels from diesel engines did Fax: +1 505 525 1076. E-mail: [email protected]. not trigger the alarm and only CO produced at high levels Abbreviations: APCI, Atmospheric Pressure Chemical Ioni- from fires exceeded the response threshold. zation; FID, Flame Ionization Detector; IMS, Ion Mobility Spectrometer; PFAIMS, Planar Field Asymmetric-waveform The other approach to bring specificity to smoke detectors Ion Mobility Spectrometer; SPME, Solid-phase Microextrac- has been to develop emerging technologies for the detec- tion; VOC, Volatile Organic Compound(s). tion of volatile organic constituents in smoke. Fires pro- 1) Presently in Pittsburgh, PA. duce a large number of organic compounds in complex i 2003 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim 1615-9306/2003/0605–0585$17.50+.50/0 586 Eiceman, Tarassov, Funk, Hughs, Nazarov, Miller J. Sep. Sci. 2003, 26, 585–593 mixtures in the vapor phase as seen in fires from synthetic pendicular to ion transport. Unlike the behavior of ions in polymers [8, 9], cigarettes [10–12], and cellulose-based traditional IMS drift tubes, ion separation in this drift tube materials such as wood [13]. This approach might in prin- occurs according to ion mobility dependence on electric ciple provide sufficient analytical information for selective field strength. The PFAIMS drift tube can be connected to detection of fires through measures of the chemical com- a capillary column and mobility scans can be obtained position of emissions. However, the analytical perfor- throughout the chromatographic analysis. This provides mance (resolution or selectivity and detection limits) chemical information in mobility scans orthogonal to reten- needed for a practical detector has always been too tion time. The small size of the miniature mobility analyzer demanding and complex for most uses. allows ion residence times of ca. 1 ms, so scan times are 1 s or less. Sensors whose response is based on solubility and absorptivity of organic compounds on coated surfaces In a direct comparison between a PFAIMS and a flame have been examined as replacements for smoke detec- ionization detector (FID) a slight broadening in the peak tors. These include surface acoustic wave (SAW) shape was observed that could be attributed to additional devices [6] and a polymer-based sensor [5]. The advan- column length from connections between the analytical tage of these sensors is the comparatively low cost and column and the detector. Apart from this small technical size. Results have shown improved discrimination over effect, the PFAIMS detector provided low cost detection conventional smoke detectors for vapors from some with advanced analytical information for a capillary GC materials. The disadvantage of these sensors is that analysis [20]. selectivity is based upon principles of general solubility or In this study, smoke from combustion of cotton, paper, surface adsorption, thus limiting specificity. A solution to grass, tobacco, and gasoline (in an internal combustion the limited selectivity of such sensors is an array of such engine) were sampled by solid-phase micro-extraction sensors with various polymers or coatings. The response (SPME) and the samples were screened using a GC- then is a complex pattern which can be interpreted using PFAIMS. A particular interest was to learn whether this artificial intelligence [4], improving selectivity. technology had sufficient analytical performance to discri- minate between these materials as a first step in equip- Although a gas chromatograph-mass spectrometer (GC- ping cotton warehouses with advanced smoke detectors. MS) would provide the specificity needed for complex mix- Since cotton may smolder for extended periods and spon- tures of organic compounds, cost and maintenance are taneously ignite [21], detecting cotton smoke at very low prohibitive. Between the performance/cost ratio of a SAW levels regardless of background combustion byproducts sensor and that of a GC-MS lies ion mobility spectrometry may facilitate the removal of smoldering material before a (IMS) technology. Recently, IMS was suggested for use fire spreads. Under such conditions, speed is not as criti- as a smoke alarm [14]. Unfortunately, drift tubes in tradi- cal as sensitivity and specificity. Details sought in these tional IMS can be costly [15]. Comparatively low cost drift studies included: a measure of the chemical vapor compo- tubes have become possible with IMS technology [16– sition of several materials using GC-MS; the discrimina- 20] with micro-machined planar drift tubes of rectangular tion of vapor profiles from cotton over those from other cel- dimensions 25 mm long65 mm wide60.5 mm deep. lulose materials by GC-PFAIMS; the identification of che- These drift tubes have been operated using non-tradi- mical markers specific to the burning of a particular mate- tional approaches to ion characterization with planar field rial; and what further enhancement of technology should asymmetric waveform (PFAIMS) dependent mobility be undertaken to reduce response time and cost. methods [16–20]. A limitation commonly encountered with miniature drift tubes is loss in detection limits. This was not observed with the PFAIMS. Detection limits in the range of 0.1 to 1 ng have been obtained [18, 19]. Thus, 2 Materials and methods the most expensive part of an IMS analyzer, the drift tube, now can be mass-produced with concomitant low cost of 2.1 Equipment such analyzers. The size of the analyzer and supporting electronics suggests that this design may be attractive as A model 5880 gas chromatograph (GC) (Hewlett-Packard a detector for a fast gas chromatograph. This may be an Co., Avondale PA) was equipped with a HP splitless injec- affordable replacement for smoke detectors with the tor, 25 m SP 2300 capillary column (Supelco, Bellefonte, added benefit that combustion source material can be PA), a flame ionization detector, and a PFAIMS detector identified. [16–20]. The carrier gas was nitrogen (99.99%) scrubbed over a molecular sieve bed. Pressure on the splitless In a high field asymmetric waveform-operated drift tube injector was 10 psig with a split ratio of 50:1. Other experi- such as PFAIMS, ions are transported through the planar mental parameters for the GC included: initial tempera- drift region by a gas flow.
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