A new, rapid air sampling/sample preparation methodology was investigated using adsorptive solid-phase microextraction (SPME) fiber coatings and nonequilibrium conditions for volatile organic compounds (VOCs). This method is the fastest extraction technique for air sampling at typical airborne VOC concentrations. A theoretical model for the extraction was formulated based on the diffusion through the interface between the sampled (bulk) air and the SPME coating. Parameters that affect the extraction process including sampling time, air velocity, air temperature, and relative humidity were investigated with the porous (solid) PDMS/DVB and Carboxen/PDMS coatings. Very short sampling times from 5 s to 1 min were used to minimize the effects of competitive adsorption and to calibrate the extraction process in the initial linear extraction region. The predicted amounts of extracted mass compared well with the measured amounts of target VOCs. Findings presented in this study extend the existing fundamental knowledge related to sampling/sample preparation with SPME, thereby enabling the development of new sampling devices for the rapid sampling of air, headspace, water, and soil.
The Geological Survey of Norway (NGU) has produced new aeromagnetic and gravity maps from Norway and adjacent areas, compiled from ground, airborne and satellite data. Petrophysical measurements on core samples, hand specimens and on in situ bedrock exposures are essential for the interpretation of these maps. Onshore, the most prominent gravity and magnetic anomalies are attributed to lower crustal rocks that have been brought closer to the surface. The asymmetry of the gravity anomalies along the Lapland Granulite Belt and Kongsberg–Bamble Complex, combined with the steep gradient, points to the overthrusted high-density granulites as being the main source of the observed anomalies. The Kongsberg–Bamble anomaly can be traced southwards through the Kattegat to southern Sweden. This concept of gravity field modelling can also be applied to the Mid-Norwegian continental shelf and could partially explain the observed high-density rocks occurring below the Møre and Vøring basins and in the Lofoten area. Extrapolations of Late-Caledonian detachment structures occurring on the mainland can be traced on aeromagnetic and gravimetric images towards the NW across the continental margin. Subcropping Late Palaeozoic to Cenozoic sedimentary units along the mid-Norwegian coast produce a conspicuous magnetic anomaly pattern. The asymmetry of the low-amplitude anomalies, with a steep gradient and a negative anomaly to the east and a gentler gradient to the west, relates the anomalies to gently westward dipping strata. Recent aeromagnetic surveys in the Barents Sea have revealed negative magnetic anomalies associated with shallow salt diapirs. Buried Quaternary channels partly filled with gravel and boulders of crystalline rocks generate magnetic anomalies in the North Sea. The new maps also show that the opening of the Norwegian–Greenland Sea occurred along stable continental margins without offsets across minor fracture zones, or involving jumps in the spreading axis. A triple junction formed at 48 Ma between the Lofoten and Norway Basins.
Odor profiling efforts were directed at applying to high-density livestock operations some of the lessons learned in resolving past, highly diverse, odor-focused investigations in the consumer product industry. Solid-phase microextraction (SPME) was used for field air sampling of odorous air near and downwind of a beef cattle feedyard and a swine finisher barn in Texas. Multidimensional gas chromatography-olfactometry (MDGC-O) was utilized in an attempt to define and prioritize the basic building blocks of odor character associated with these livestock operations. Although scores of potential odorant volatiles have been previously identified in high-density livestock operations, the odor profile results developed herein suggest that only a very few of these may constitute the preponderance of the odor complaints associated with these environments. This appeared to be especially true for the case of increasing distance from both cattle feedyard and swine barn facilities, with p-cresol consistently taking on the dominant odor impact role with ever increasing distance. In contrast, at- or near-site odor profiles were shown to be much more complex, with many of the well-known lower tier odorant compounds rising in relative significance. For the cattle feedyard at- or near-site odor profiles, trimethylamine was shown to represent a significantly greater individual odor impact relative to the more often cited livestock odorants such as hydrogen sulfide, the organic sulfides, and volatile fatty acids. This study demonstrates that SPME combined with a MDGC-O-mass spectrometry system can be used for the sampling, identification, and prioritization of odors associated with livestock.
Lingshuang Cai, postdoctoral research associate of ABE; Jacek A. Koziel*, assistant professor of ABE; Yin-Cheung Lo, M.S. of ABE; Steven J. Hoff, professor of ABE Summary and Implications Swine operations can affect air quality by emissions of odor, volatile organic compounds (VOCs) and other gases, and particulate matter (PM). Particulate matter has been proposed to be an important pathway for carrying odor. In this research, continuous PM sampling was conducted simultaneously with three collocated TEOM (tapered element oscicllating microbalance) analyzers inside a 1000head swine finish barn located in central Iowa. Each TEOM was fitted with total suspended particulate (TSP), PM-10, PM-2.5 and PM-1 preseparators. Used filters were stored in 40 mL vials and transported to the laboratory. Carboxen/polydimethylsiloxane (PDMS) 85 μm solid phase microextraction (SPME) fibers were used to extract VOCs. Simultaneous chemical and olfactometry analyses of VOCs and odor associated with swine PM were completed using a gas chromatography-mass spectrometer-olfactometry (GC-MS-O) system. Fifty VOCs categorized into nine chemical function groups were identified and confirmed with standards. Five of them are classified as hazardous air pollutants. VOCs were characterized with a wide range of molecular weight, boiling points, vapor pressures, water solubilities, odor detection thresholds, and atmospheric reactivities. All characteristic swine VOCs and odorants were present in PM and their abundance was proportional to PM size. However, the majority of VOCs and characteristic swine odorants were preferentially bound to smaller-size PM. The findings indicate that a significant fraction of swine odor can be carried by PM.
Odorous gases associated with livestock operations are complex mixtures of hundreds if not thousands of compounds. Research is needed to know how best to sample and analyze these compounds. The main objective of this research was to compare recoveries of a standard gas mixture of 11 odorous compounds from the Carboxen/PDMS 75-m solid-phase microextraction fibers, polyvinyl fluoride (PVF; Tedlar), fluorinated ethylene propylene copolymer (FEP; Teflon), foil, and polyethylene terephthalate (PET; Melinex) air sampling bags, sorbent 2,b-diphenylene-oxide polymer resin (Tenax TA) tubes, and standard 6-L Stabilizer sampling canisters after sample storage for 0.5, 24, and 120 (for sorbent tubes only) hrs at room temperature. The standard gas mixture consisted of 7 volatile fatty acids (VFAs) from acetic to hexanoic, and 4 semivolatile organic compounds including p-cresol, indole, 4-ethylphenol, and 2Ј-aminoacetophenone with concentrations ranging from 5.1 ppb for indole to 1270 ppb for acetic acid. On average, SPME had the highest mean recovery for all 11 gases of 106.2%, and 98.3% for 0.5-and 24-hr sample storage time, respectively. This was followed by the Tenax TA sorbent tubes (94.8% and 88.3%) for 24 and 120 hr, respectively; PET bags (71.7% and 47.2%), FEP bags (75.4% and 39.4%), commercial Tedlar bags (67.6% and 22.7%), in-house-made Tedlar bags (47.3% and 37.4%), foil bags (16.4% and 4.3%), and canisters (4.2% and 0.5%), for 0.5 and 24 hr, respectively. VFAs had higher recoveries than semivolatile organic compounds for all of the bags and canisters. New FEP bags and new foil bags had the lowest and the highest amounts of chemical impurities, respectively. New commercial Tedlar bags had measurable concentrations of N,N-dimethyl acetamide and phenol. Foil bags had measurable concentrations of acetic, propionic, butyric, valeric, and hexanoic acids.
Solid phase microextraction (SPME) presents many advantages over conventional analytical methods by combining sampling, preconcentration, and direct transfer of
Homeowners, small fruit growers, and wine makers are concerned with noxious compounds released by multicolored Asian ladybird beetles (Harmonia axyridis, Coleoptera: Coccinellidae). A new method based on headspace solid-phase microextraction (HS-SPME) coupled with multidimensional gas chromatography-mass spectrometry-olfactometry (MDGC-MS-O) system was developed for extraction, isolation and simultaneous identification of compounds responsible for the characteristic odor of live H. axyridis. Four methoxypyrazines (MPs) were identified in headspace volatiles of live H. axyridis as those responsible for the characteristic odor: 2,5-dimethyl-3-methoxypyrazine (DMMP), 2-isopropyl-3-methoxypyrazine (IPMP), 2-sec-butyl-3-methoxypyrazine (SBMP), and 2-isobutyl-3-methoxypyrazine (IBMP). To the best of our knowledge this is the first report of H. axyridis releasing DMMP and the first report of this compound being a component of the H. axyridis characteristic odor. Besides the MPs, 34 additional compounds were also identified. Quantification of three MPs (IPMP, SBMP and IBMP) emitted from live H. axyridis were performed using external calibration with HS-SPME and direct injections. A linear relationship (R(2)>0.9951 for all 3 MPs) between MS response and concentration of a standard was observed over a concentration range from 0.1 ng L(-1) to 0.05 microg L(-1) for HS-SPME-GC-MS. The method detection limits (MDL) based on multidimensional GC-MS with narrow heart-cut approach for three MPs were estimated to be between 0.020 and 0.022 ng L(-1). This represents a 38.9-52.4% improvement in sensitivity compared to GC-MS with full heart-cut method. This methodology is applicable for in vivo determination of odor-causing chemicals associated with emissions of volatiles from insects.
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