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The indoor air of living rooms which are located above commercially used rooms can exhibit traces of volatile organic substances. These substances were enriched with passive samplers and gas-chromatographically determined.
The paper reports on the performance of chromium or/and copper supported on H-ZSM-5(Si/Al = 240) modified with silicon tetrachloride (Cr1.5/SiCl4-Z, Cu1.5/SiCl4-Z and Cr1.0Cu0.5/SiCl4-Z) as catalysts in the combustion of chlorinated VOCs (Cl-VOCs). A reactor operated at a gas hourly space velocity (GHSV) of 32,000 h(-1), a temperature between 100 and 500 degrees C with 2500 ppm of dichloromethane (DCM), trichloromethane (TCM) and trichloroethylene (TCE) is used for activity studies. The deactivation study is conducted at a GHSV of 3800 h(-1), at 400 degrees C for up to 12 h with a feed concentration of 35,000 ppm. Treatment with silicon tetrachloride improves the chemical resistance of H-ZSM-5 against hydrogen chloride. TCM is more reactive compared to DCM but it produces more by-products due to its high chlorine content. The stabilization of TCE is attributed to resonance effects. Water vapor increases the carbon dioxide yield through its role as hydrolysis agent forming reactive carbocations and acting as hydrogen-supplying agent to suppress chlorine-transfer reactions. The deactivation of Cr1.0Cu0.5/SiCl4-Z is mainly due to the chlorination of its metal species, especially with higher Cl/H feed. Coking is limited, particularly with DCM and TCM. In accordance with the Mars-van Krevelen model, the weakening of overall metal reducibility due to chlorination leads to a loss of catalytic activity.
Literature values of the in vivo distribution (BB) of drugs from blood, plasma, or serum to rat brain have been assembled for 207 compounds (233 data points). We find that data on in vivo distribution from blood, plasma, and serum to rat brain can all be combined. Application of our general linear free energy relationship (LFER) to the 207 compounds yields an equation in log BB, with R2=0.75 and a standard deviation, SD, of 0.33 log units. An equation for a training set predicts the test set of data with a standard deviation of 0.31 log units. We further find that the in vivo data cannot simply be combined with in vitro data on volatile organic and inorganic compounds, because there is a systematic difference between the two sets of data. Use of an indicator variable allows the two sets to be combined, leading to a LFER equation for 302 compounds (328 data points) with R2=0.75 and SD=0.30 log units. A training equation was then used to predict a test set with SD=0.25 log units.
Micropatterned polymeric diffraction gratings have been fabricated and evaluated as volatile organic chemical sensors. When operated under nonresonant conditions, sensor elements were found to respond in a rapid (response time 5-15 s) and reproducible fashion to each analyte investigated. Relative response magnitudes were found to be in qualitative agreement with those obtained via surface acoustic wave techniques. Preliminary limits of detection as determined by investigations with micropatterned polyepichlorohydrin, polyisobutylene, and polybutadiene gratings, respectively, were found to be 8, 11, and 7 ppm for toluene, 25, 258; and 72 ppm for methyl ethyl ketone; 41, 102, and 34 ppm for chloroform; and 460, 60, and 59 ppm for hexane. While generally less than 1 order of magnitude higher than those observed for identical polymer/analyte combinations in SAW studies, the observed limits of detection were at or below governmental standards (OSHA-PEL and NIOSH-REL) for each analyte evaluated. These diffraction-based sensors show promise for integration into an array-based sensor system, providing simultaneous identification and quantification of unknown analytes and simple analyte mixtures.
The U.S. Environmental Protection Agency and the California Air Resources Board studied the exposures of 51 residents of Los Angeles, California, to 25 volatile organic chemicals (VOCs) in air and drinking water in 1987. A major goal of the study was to measure personal, indoor, and outdoor air concentrations, and breath concentrations of VOCs in persons living in households that had previously been measured in 1984. Other goals were to confirm the marked day-night and seasonal differences observed in 1984; to determine room-to-room variability within homes; to determine source emission rates by measuring air exchange rates in each home; and to extend the coverage of chemicals by employing additional sampling and analysis methods. A total of 51 homes were visited in February of 1987, and 43 of these were revisited in July of 1987. The results confirmed previous TEAM Study findings of higher personal and indoor air concentrations than outdoor concentrations of all prevalent chemicals (except carbon tetrachloride); higher personal, indoor, and outdoor air concentrations in winter than in summer; and (in winter only) higher outdoor concentrations at night than in the daytime. New findings included the following: (1) room-to-room variability of 12-hour average concentrations was very small, indicating that a single monitor may be adequate for estimating indoor concentrations over this time span; (2) "whole-house" source emission rates were relatively constant during both seasons, with higher rates for odorous chemicals such as p-dichlorobenzene and limonene (often used in room air fresheners) than for other classes of chemicals; (3) breath concentrations measured during morning and evening were similar for most participants, suggesting the suitability of breath measurements for estimating exposure in the home; (4) limited data obtained on two additional chemicals-toluene and methylene chloride-indicated that both were prevalent at fairly high concentrations and that indoor air concentrations exceeded outdoor concentrations by a factor of about three.
A prototype mid-infrared sensor system for the determination of volatile organic pollutants in groundwater was developed and tested under real-world conditions. The sensor comprises a portable Fourier transform infrared spectrometer, coupled to the sensor head via mid-infrared transparent silver halide fiber-optic cables. A 10 cm unclad middle section of the 6-m-long fiber is coated with ethylene propylene copolymer in order to enrich the analytes within the penetration depth of the evanescent field protruding from the fiber sensor head. A mixture of tetrachloroethylene, dichlorobenzene, diethyl phthalate, and xylene isomers at concentrations in the low ppm region was investigated qualitatively and quantitatively in an artificial aquifer system filled with Munich gravel. This simulated real-world site at a pilot scale enables in situ studies of the sensor response and spreading of the pollutants injected into the system with controlled groundwater flow. The sensor head was immersed into a monitoring well of the aquifer system at a distance of 1 m downstream of the sample inlet and at a depth of 30 cm. Within one hour, the analytes were clearly identified in the fingerprint region of the IR spectrum (1300 to 700 cm(-1)). The results have been validated by head-space gas chromatography, using samples collected during the field measurement. Five out of six analytes could be discriminated simultaneously; for two of the analytes the quantitative results are in agreement with the reference analysis.
The US EPA and the California Air Resources Board studied the exposures of 51 residents of Los Angeles, CA to 25 volatile organic chemicals in air and drinking water in February and July of 1987. Participants carried a personal air monitor consisting of a Tenax cartridge and a small sampling pump for two consecutive 12-hour periods. Concurrently, outdoor air samples were collected in the back yards and indoor air samples were collected in the kitchen and living room. Breath samples were collected at the beginning, middle, and end of the 24-hour monitoring period using a vanmounted spirometer employing Tedlar bags followed by collection on Tenax cartridges. All analyses were by GC/MS. Air exchange measurements were made at all homes using the perfluorotracer method. For most chemicals, personal air concentrations were greater than indoor air levels, which were in turn greater than outdoor air concentrations. Breath concentrations were more stable than air exposures and were significantly correlated with previous exposure. Using the air exchange measurements, whole-house source strengths were estimated to range between approximately zero for carbon tetrachloride to 10,000 micrograms/h for para-dichlorobenzene. Ambient concentrations in February were two-three times those in July, perhaps due to strong inversions.
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The development and operational evaluation of a calibration gas generator for the analysis of volatile or ganic compounds (VOC) in air is described. Details of the construction, as well as of the evaluation of the apparatus are presented here. The performance of the test gas generator is validated both by on-line GC analysis of the calibration gas produced and by off-line analysis of adsorptive samples taken from the generated calibration gas. Both, active and passive sampling have been used, and the results demonstrate the excellent accuracy and precision of the generated test gas atmosphere: For the 11 investigated organic compounds (aromatic and halogenated compounds), the found values were in most cases within 5% of the target value with a reproducibility of better than 3% RSD (as determined by the analysis of the sampled adsorbent tubes). Custom made adsorbent tubes were used for active and passive sampling and in both cases were analysed by thermal-desorption GC. Particularly the combination of passive sampling and thermodesorption-GC analysis offers significant advantages over the commonly used active sampling on activated charcoal, followed by CS2 desorption in terms of avoidance of hazardous solvents, potential for automation and improved detection limits. Both sampling techniques are capable for monitoring VOCs at concentrations and under conditions relevant for workplace monitoring.
Catabolism of a (14)C-labelled volatile monoterpene compound (geraniol) to (14)CO(2) was investigated in soils taken from the rhizosphere at distances up to 200 cm from the trunks of three small Populus tremula trees growing at different sites in Slovenia. Emissions of limonene of up to 18 microg m(-2) h(-1) were detected from the soil surface at each site. Evolution of (14)C-labelled CO(2) was measured as a product of catabolism of (14)C-labelled geraniol introduced into the soil samples. Indigenous soil microorganisms degraded the geraniol rapidly. There was a significant difference in relative lag times and rates of catabolism along the gradient from the tree trunks, with relatively longer lag times and lower rates occurring in soil samples from the farthest point from the tree.
A system and methodology were developed for the nondestructive qualitative and quantitative analysis of volatile emissions from hydroponically grown 'Waldmann's Green' leaf lettuce (Lactuca sativa L.). Photosynthetic photon flux (PPF), photoperiod, and temperature were automatically controlled and monitored in a growth chamber modified for the collection of plant volatiles. The lipoxygenase pathway products (Z)-3-hexenal, (Z)-3-hexenol, and (Z)-3-hexenyl acetate were emitted by lettuce plants after the transition from the light period to the dark period. The volatile collection system developed in this study enabled measurements of volatiles emitted by intact plants, from planting to harvest, under controlled environmental conditions.
Estimates of dermal dose from exposures to toxic chemicals are typically derived using models that assume instantaneous establishment of steady-state dermal mass flux. However, dermal absorption theory indicates that this assumption is invalid for short-term exposures to volatile organic chemicals (VOCs). A generalized distributed parameter physiologically-based pharmacokinetic model (DP-PBPK), which describes unsteady state dermal mass flux via a partial differential equation (Fickian diffusion), has been developed for inhalation and dermal absorption of VOCs. In the present study, the DP-PBPK model has been parameterized for chloroform, and compared with two simpler PBPK models of chloroform. The latter are lumped parameter models, employing ordinary differential equations, that do not account for the dermal absorption time lag associated with the accumulation of permeant chemical in tissue represented by permeability coefficients. All three models were evaluated by comparing simulated post-exposure exhaled breath concentration profiles with measured concentrations following environmental chloroform exposures. The DP-PBPK model predicted a time-lag in the exhaled breath concentration profile, consistent with the experimental data. The DP-PBPK model also predicted significant volatilization of chloroform, for a simulated dermal exposure scenario. The end-exposure dermal dose predicted by the DP-PBPK model is similar to that predicted by the EPA recommended method for short-term exposures, and is significantly greater than the end-exposure dose predicted by the lumped parameter models. However, the net dermal dose predicted by the DP-PBPK model is substantially less than that predicted by the EPA method, due to the post-exposure volatilization predicted by the DP-PBPK model. Moreover, the net dermal dose of chloroform predicted by all three models was nearly the same, even though the lumped parameter models did not predict substantial volatilization.
Static equilibrium headspace was diluted with a stream of nitrogen to study the stability of the volatile headspace concentration. The headspace dilution profile of 18 volatile compounds above aqueous and ethanolic solutions was measured in real time using atmospheric pressure chemical ionization-mass spectrometry. Under dynamic conditions the volatiles headspace concentration above water solutions decreased readily upon dilution. The presence of ethanol helped to maintain the volatile headspace concentration when the ethanol solution concentration was above 50 mL/L. This effect was such that under dynamic conditions the absolute volatile concentration above an ethanolic solution was higher than that above an aqueous solution, contrary to results observed in equilibrium studies. The ratio of the headspace concentration of volatiles above ethanolic 120 mL/L and water solutions was correlated to their air/water partition coefficient.
In 2001, Bacillus anthracis spores were delivered through the United States postal system in a series of bioterrorist acts. Controls proposed for this threat included sanitization with high-energy electrons. Solid phase microextraction was used with gas chromatography/mass spectrometry for field sampling and analysis of volatile compounds apparently produced from polymeric materials such as cellulose and plastics, immediately following processing of mail at a commercial irradiation facility. Solid phase microextraction and direct sampling of air into a cryogenically cooled temperature programmable inlet were used in the laboratory for gas chromatography/mass spectrometry analysis of air in contact with irradiated mail, envelopes only (packaged identically to mail), and air inside irradiated plastic mail packaging bags (with neither mail nor envelopes). Irradiated mail or envelope systems produced hydrocarbons such as propane, butane, pentane, hexane, heptane, methylpentanes, and benzene; and oxygen-containing compounds such as acetaldehyde, acrolein, propionaldehyde, furan, 2-methylfuran, methanol, acetone, 2-butanone, and ethanol. In addition to hydrocarbons, methyl and ethyl nitrate were detected in irradiated bags that contained only air, suggesting reactive nitrogen species formed from air irradiation reacted with hydroxy-containing compounds to give nitro esters. The similarities of volatile compounds in irradiated systems containing paper to those observed by researchers studying cellulose pyrolysis suggests common depolymerization and degradation mechanisms in each case. These similarities should guide additional work to examine irradiated mail for chemical compounds not detectable by methods used here.
A method compatible with radioactive samples, capable of detecting trace volatile components in a sample volume of ca. 1cm(3) of 2-[18F]-fluoro-2-deoxy-D-glucose solution is described. The approach, based on solid phase micro-extraction gas chromatography-mass spectrometry with a carboxen/polydimethylsiloxane based fibre, was optimised with respect to extraction time (10 min), extraction temperature (60 degrees C) and phase volume ratio (1). The analysis time, including extraction, was less than 20 min with linear responses for acetonitrile and ethanol over the ranges: 0.09-80 microg cm(-3) (22 degrees C, acetonitrile) and 0.78-79 microg cm(-3) (22 degrees C, ethanol). The detection limits were estimated to be ca. 0.78 microg cm(-3) for ethanol and 0.09 microg cm(-3) for acetonitrile. Stability studies indicated analyte losses of up to 75% over 24h and analysis of aged 2-[18F]FDG samples showed that levels of ethanol and acetonitrile were not less than 100 microg cm(-3), indicative of levels substantially greater than this in the original infusions given to human subjects.
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A commercial in-tube sorptive extraction device, known as solid-phase dynamic extraction (SPDE), has been evaluated for the extraction of non-polar volatile aromatic analytes from aqueous solutions in both headspace and liquid injection modes. An automated sampler is used with a gas-tight 2.5 ml syringe equipped with a special needle that is coated on the inside with a non-polar extraction phase. After absorption onto the phase, the analytes were thermally desorbed directly into a GC-MS system. The technique was evaluated for the determination of furan, benzene and toluene. The sensitivity for toluene was greatly improved on using SPDE compared to static headspace. A slight increase in sensitivity was observed for benzene but none for determination of furan. Estimated limits of detection ranged from 0.2 to 2 microg/l.