A novel gas chromatograph-mass spectrometer (GC-MS) based on a miniature toroidal ion trap mass analyzer (TMS) and a low thermal mass GC is described. The TMS system has an effective mass/charge (m/z) range of 50-442 with mass resolution at full-width half-maximum (FWHM) of 0.55 at m/z 91 and 0.80 at m/z 222. A solid-phase microextraction (SPME) fiber mounted in a simple syringe-style holder is used for sample collection and introduction into a specially designed low thermal mass GC injection port. This portable GC-TMS system weighs <13 kg (28 lb), including batteries and helium carrier gas cartridge, and is totally self-contained within dimensions of 47 X 36 X 18 em (18.5 X 14 X 7 in.). System start-up takes about 3 min and sample analysis with library matching typically takes about 5 min, including time for column cool-down. Peak power consumption during sample analysis is about 80 W. Battery power and helium supply cartridges allow 50 and 100 consecutive analyses, respectively. Both can be easily replaced. An on-board library of target analytes is used to provide detection and identification of chemical compounds based on their characteristic retention times and mass spectra. The GC-TMS can detect 200 pg of methyl salicylate on-column. n-Butylbenzene and naphthalene can be detected at a concentration of 100 ppt in water from solid-phase microextraction (SPME) analysis of the headspace. The GC-TMS system has been designed to easily make measurements in a variety of complex and harsh environments. and toxic industrial chemicals (TICs), is a concern, the ability to rapidly detect and accurately identify such chemicals in harsh environments is of great utility. There is a need for field-portable, selective, and sensitive detectors for military and emergency first-responder operations and for on-site environmental contamination measurement, to mention only a couple of key applications. The development of fieldportable devices directed toward fast, on-site analysis is one of the most active research areas in analytical chemistry.Currently, several approaches for detection of CWAs and TICs are utilized by military personnel, first responders, and environmental scientists. They include dye solubility (detection paper), enzymatic reaction,
The U.S. Environmental Protection Agency is promoting the development and application of sampling methods for the semicontinuous determination of fine particulate matter (PM 2.5 , particles with an aerodynamic diameter Ͻ2.5 m) mass and chemical composition. Data obtained with these methods will significantly improve the understanding of the primary sources, chemical conversion processes, and meteorological atmospheric processes that lead to observed PM 2.5 concentrations and will aid in the understanding of the etiology of PM 2.5 -related health effects. During January and February 2007, several semicontinuous particulate matter (PM) monitoring systems were compared at the Utah State Lindon Air Quality Sampling site. Semicontinuous monitors included instruments to measure total PM 2.5 mass (filter dynamic measurement system [FDMS] tapered element oscillating microbalance [TEOM], GRIMM), nonvolatile PM 2.5 mass (TEOM), sulfate and nitrate (two PM 2.5 and one PM 10 [PM with an aerodynamic diameter Ͻ10 m] ionchromatographic-based samplers), and black carbon (aethalometer). PM 10 semicontinuous mass measurements were made with GRIMM and TEOM instruments. These measurements were all made on a 1-hr average basis. Source apportionment analysis indicated that sources impacting the site were mainly urban sources and included mobile sources (gasoline and diesel) and residential burning of wood, with some elevated concentrations because of the effect of winter inversions. The FDMS TEOM and GRIMM instruments were in good agreement, but TEOM monitor measurements were low because of the presence of significant semi-volatile material. Semi-volatile mass was present dominantly in the PM 2.5 mass.
A state-of-the-art, rapid laser-heating technique, referred to as the laser-driven thermal reactor, was used to characterize National Institute of Standards and Technology Standard Reference Material (SRM) diesel and biodiesel fuels, as well as a prototype biodiesel fuel. Also described are the various issues associated with carrying out these measurements under different operating conditions (i.e., temperature, pressure, heating rate, and sample mass). The technique provides measurement of various relevant thermochemical characteristics; for this investigation the focus was on the sample endothermic/exothermic behavior, specific heat release rate and total specific heat release. The experimental apparatus consists of a copper sphere-shaped reactor mounted within a vacuum chamber, along with integrated optical, gas-supply, and computer-controlled data-acquisition subsystems. At the center of the reactor, the sample rests on a thermocouple. The reactor is heated from opposing sides by a near-infrared laser to achieve nearly uniform sample temperature. The change in sample temperature with time (i.e., thermogram) is recorded and compared to a baseline (no sample) thermogram obtained prior to the experiment. Then processed (using an equation for thermal energy conservation) for the thermochemical information of interest. Results indicated that the modification of the baseline is attributed to residue remaining after completion of reactions and a change in the oxide layer of the reactor sphere outer surface. Thus, the sphere must be pre-oxidized in air using the laser prior to any sample or baseline measurement. This investigation provides preliminary evaluation of SRM biodiesel fuels, with the results being consistent with distillation curve work reported in the literature.
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