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At least 1,171 records · Page 65Linked to original sources

PubMed2005

De- and rehydration behavior of alpha,alpha-trehalose dihydrate under humidity-controlled atmospheres.

Effects of humidity were investigated on de- and rehydration behavior of alpha,alpha-trehalose dihydrate (T(h)) throughout simultaneous measurements of differential scanning calorimetry and X-ray diffractometry (DSC-XRD) and simultaneous thermogravimetry and differential thermal analysis (TG-DTA). When T(h) was heated from room temperature under dry nitrogen atmosphere, a metastable anhydrous crystal (T(alpha)) was formed at 105 degrees C after dehydration of T(h). The resulting T(alpha) melted at 125 degrees C and became amorphous, followed by cold crystallization from 150 degrees C giving rise to a stable anhydrous crystal T(beta). Under a highly humid atmosphere, on the other hand, T(beta) was formed at 90 degrees C directly as a result of T(h) dehydration. T(alpha) was readily rehydrated and turned back to T(h) when nitrogen gas with low water vapor pressure of 2.1kPa was admitted, whereas high water vapor pressure up to 7.4kPa was required for rehydration of T(beta) into T(h). This study provided a picture of pathways that link various solid forms of trehalose, taking into account the effects of a humid environment.

Atmosphere↗

PubMed2006

Urban atmospheric pollution: personal exposure versus fixed monitoring station measurements.

We initiated the PETER (pedestrian environmental traffic pollutant exposure research) project to investigate pedestrians' exposure to traffic related atmospheric pollutants, based on data obtained with the collaboration of selected categories of pedestrian urban workers. We investigated relations between roadside personal exposure levels of volatile aromatic hydrocarbons (including benzene) and particulate matter <10 microm (PM10) among traffic police (n = 126) and parking wardens (n = 50) working in downtown Bologna, Italy. Data were collected from workshifts throughout four 1-week periods in different seasons of 2000-2001. For benzene and PM10, comparisons were made with measurements by fixed monitoring stations, and influence of localized traffic intensity and meteorological parameters was examined. Roadside personal exposure to benzene correlated more strongly with other volatile aromatic hydrocarbons (toluene, xylenes and ethylbenzene) than with PM10. Benzene and PM10 personal exposure levels were higher than fixed monitoring station values (both p<0.0001). At multivariate analysis, benzene and PM10 data from fixed monitoring stations both correlated with meteorological variables, and were also influenced by localized traffic intensity. Plausibly because of the downtown canyon-like streets, weather conditions (during a period of drought) only marginally affected benzene personal exposure, and moderately affected PM10 personal exposure. These findings reinforce the concept that urban atmospheric pollution data from fixed air monitoring stations cannot automatically be taken as indications of roadside exposures.

Air Pollution↗

PubMed2004

Determination of aldehydes and ketones using derivatization with 2,4-dinitrophenylhydrazine and liquid chromatography-atmospheric pressure photoionization-mass spectrometry.

Atmospheric pressure photoionization-mass spectrometry (APPI-MS) is used for the analysis of aldehydes and ketones after derivatization with 2,4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the [M - H]- pseudomolecular ions are most abundant for the carbonyls. Compared with the established atmospheric pressure chemical ionization (APCI)-MS, limits of detection are typically lower using similar conditions. Automobile exhaust and cigarette exhaust samples were analyzed with APPI-MS and APCI-MS in combination with an ion trap mass analyzer. Due to improved limits of detection, more of the less abundant long-chain carbonyls are detected with APPI-MS in real samples. While 2,4-dinitrophenylazide, a known reaction product of DNPH with nitrogen dioxide, is detected in APCI-MS due to dissociative electron capture, it is not observed at all in APPI-MS.

Aldehydes↗

PubMed2006

Determination of sugar compounds in atmospheric aerosols by liquid chromatography combined with positive electrospray ionization mass spectrometry.

We here report a method for the determination of sugar compounds of known presence in atmospheric aerosols using liquid chromatography (LC) combined with positive electrospray ionization mass spectrometry (MS). The target analytes include C(3)-C(6) monosaccharide alcohols (glycerol, erythritol, xylitol, mannitol), C(5)-C(6) monosaccharides (xylose, glucose, and levoglucosan), a disaccharide (sucrose), and a trisaccharide (melezitose). A mobile phase consisting of 20% 10 mM aqueous ammonium acetate, 8% methanol, and 72% water was found to provide abundant [M+NH(4)](+) adduct ions when coupled with electrospray ionization. Use of a polymer-based amino analytical column resolved the target compounds from the bulk solvent and provided limited separation among the target compounds. The target analytes were quantified using their [M+NH(4)](+) ions. Sample pretreatment was greatly simplified in comparison with the more commonly used gas chromatographic methods. It involved extraction of aerosol filters in methanol, evaporation of the solvent, and reconstitution with 5 mM ammonium acetate in water prior to the LC-MS analysis. The analyte recoveries were measured at the levels of 100, 500 and 1000 microg/L to be in the range of 78-102%, 94-112%, and 92-110%, respectively. The detection limits were lower than 10 pmol/injection for the tested target compounds except for xylose. Xylose had a detection limit of 95 pmol/injection. The method was applied to analyze 30 atmospheric aerosol samples to demonstrate its feasibility. The LC-MS method made possible the detection of trisaccharides as aerosol constituents for the first time.

Aerosols↗

PubMed2006

Atmospheric pressure photoionization mass spectrometry for analysis of fatty acid and acylglycerol lipids.

In this work, we optimize parameters and conditions for analysis of fatty acid ester and acylglycerol lipids by atmospheric pressure photoionization-mass spectrometry (APPI-MS). The investigated parameters include atmospheric pressure chemical ionization (APCI) nebulizer/vaporizer physical orientation and APPI lamp face position, solvent selections, mobile phase compositions and flow rates, cone voltages and probe temperatures. APPI sensitivity is found to be highly dependent on mobile phase compositions. Normal phase solvents offer much higher sensitivity and better peak shape than reversed phase for nonpolar lipids. Hexane and isooctane are found to be two solvents generating highest S/N for eicosapentaenoic acid (EPA) methyl ester. The effects of mobile phase flow rates on sensitivity are found to be target analytes and target ions specific. However, the flow rate changes do not significantly affect the sensitivity of three out of four tested analytes under normal phase conditions over tested flow rates of 50-500muL/min. Cone voltage is found to be one of key parameters affecting sensitivity. Optimum probe temperature is found to be more dependent on mobile phase compositions than on the specific target analytes. Aqueous reversed-phase mobile phase requires higher probe temperature than normal phase for better sensitivity. More volatile mobile phase solvents require lower probe temperature for analyte desolvation. APPI offers four to five decades of linear ranges under normal phase condition. Full scan mass spectra of individual lipid standards, custom lipid mixtures and natural fish oil show that APPI spectra are clean and very easy to interpret. APPI also gives stable, reproducible peak responses with good peak shape. Limits of detection (LODs) by FIA (S/N=3) are estimated to be 12pg for EPA methyl ester and monoarachidin, 19pg for diarachidin and 7pg for trielaidin. LODs on-column are estimated to be 94pg for EPA methyl ester, 90pg for monoarachidin and diarachidin and 24pg for trielaidin.

Atmospheric Pressure↗

PubMed2005

Atmospheric bulk deposition to the Lagoon of Venice Part II. Source apportionment analysis near the industrial zone of Porto Marghera, Italy.

Multivariate statistical analyses were applied to measurements of atmospheric deposition of total particulate (TSP), inorganic elements (Al, Ca, Na, K, Mg, Si, Mn, Fe, Zn, Ni, Cr, Cu, Pb, Cd, As, Hg, V and S) and organic compounds (PAH, PCB, HCB and PCDD/F) collected in four stations, all located in the Lagoon of Venice. Aerosols at the scale of the basin (i.e., within a distance of 20 km) were mainly characterised by two end-members, one natural (composed of mineral particulate and marine spray) and one anthropogenic (with at least two different source components), affecting the sites in various ways. Variability at the two distant (>20 km) sites (Valle Dogà, Valle Figheri) was mainly due to natural components, whereas the other two stations (city of Venice, Dogaletto, approximately 5 km) were mainly impacted by industrial (and urban) sources. Total annual inputs were compared with the limits recently set by law (maximum allowed discharge=MAD). In the year of study, MAD values were exceeded for total As, Cd, Hg, Pb, dissolved Zn, PAH and PCDD/F. These results indicate that industrial sources gave rise to a quasi-permanent compositional (background) effect near the industrial area. The risk associated with atmospheric deposition should be quantified within the DSPIR framework to avoid future negative consequences in populations living in the vicinity of Porto Marghera.

Atmosphere↗

PubMed2004

Investigating the occurrence of persistent organic pollutants (POPs) in the arctic: their atmospheric behaviour and interaction with the seasonal snow pack.

POPs in the Arctic are the focus of international concern due to their occurrence and accumulation in Arctic food webs. This paper presents an overview of the major pathways into the Arctic and details contemporary studies that have focused on the occurrence and transfer of POPs between the major Arctic compartments, highlighting areas where there is a lack of quantitative information. The behaviour of these chemicals in the Arctic atmosphere is scrutinised with respect to long-term trends and seasonal behaviour. Subtle differences between the PCBs and OC pesticides are demonstrated and related to sources outside of the Arctic as well as environmental processes within the Arctic. Unlike temperate regions, contaminant fate is strongly affected by the presence of snow and ice. A description of the high Arctic snow pack is given and the physical characteristics that determine chemical fate, namely the specific surface area of snow and wind driven ventilation, are discussed. Using a well-characterised fresh snow event observed at Alert (Canadian high Arctic) [Atmos. Environ. 36(2002) 2767] the flux of gamma-HCH out of the snow is predicted following snow ageing. Under conditions of wind (10 m/s) it is estimated that approximately 75% of the chemical may be re-emitted to the atmosphere within 24 h following snowfall, compared with just approximately 5% under conditions of no wind. The implications of this are raised and areas of further research suggested.

Air Pollutants↗

PubMed2006

Diversity and seasonal variation of viable algal particles in the atmosphere of a subtropical city in India.

To characterize the airborne algal diversity in a populous subtropical urban environment, sampling was done at a height of 2.5m, the normal human breathing zone. Results indicated that airborne algae are the permanent constituent of Varanasi city atmosphere. The nature, composition, and relative ratio of constituting groups differed among sampling sites. Cyanobacteria, possibly due to their broad ecological distribution, dominate the fluctuating climates of subtropical regions such as Varanasi. The majority of the airborne algae were of local origin, indicating short-distance transport of the algae. Soilborne algae constituted the bulk of aeroalgal flora. This might be due to their ability to withstand the dehydrating effect of the atmosphere. Composition of the aeroalgal community also exhibited seasonal variation along with the change in climatic condition of the area. Thus, the physiological ability of an algal group to tolerate different types of abiotic stresses and the climatic conditions of the area appeared to be the two major factors responsible for regulating the structure of the aeroalgal community in the air.

Atmosphere↗

PubMed2004

Analytical investigations in a death case by suffocation in an argon atmosphere.

A 31-year-old engineer was found dead in a reaction vessel (diameter 0.8 m, height 1.8 m) of a bulb factory some minutes after he had entered it for repair work. Resuscitation attempts with artificial respiration were unsuccessful. Despite autopsy and usual toxicological analyses, no cause of death could be found. Since in the normal production process, argon was used as a protecting gas, the possibility of suffocation in an argon atmosphere was investigated. This was rendered more difficult because of the natural content of 0.93 vol.% argon in air and since the excessive argon could have been removed by the resuscitation attempts. Gas samples from larynx, esophagus, bronchi, and stomach, separated blood samples from both ventricles of the heart and from the vena iliaca externa as well as tissue samples from lung and liver were collected during autopsy into headspace vials in such a way that the loss of gas and a dilution by surrounding air was avoided as far as possible. The samples were analyzed by headspace GC-MS. The abundance of Ar+ (m/z = 40) was used for quantification with N2(2+) (m/z = 14) as internal standard. The following argon concentrations were measured (mean values, case under investigation/comparison cases): gas from larynx 1.79/0.96 vol.%, stomach gas 1.58/0.89 vol.%, heart blood (left ventricle) 7.2/2.7 microg/mL, heart blood (right ventricle) 5.8/2.7 microg/mL, blood from vena iliaca externa 3.6/2.7 microg/mL. A clearly increased concentration was also found in lung tissue, whereas in liver tissue no significant difference in comparison to other cases was measured. From the results, it follows that the deceased inhaled an increased amount of argon a short time before death. The concentrations are consistent with asphyxia and subsequent resuscitation attempts. They cannot be explained by a long-term inhalation of an atmosphere enriched with argon before the incident as it is likely to have occurred in this factory hall.

Administration, Inhalation↗

PubMed2006

Determination of gambogic acid in human plasma by liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

A high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS) method was established for the determination of gambogic acid (GA) in human plasma using ursolic acid as the internal standard (I.S.). Plasma samples were extracted with ethyl acetate and separated on a Hanbon Lichrospher 5-C18 column with a mobile phase of acetonitrile-tetrahydrofuran-water (70:23:7, v/v). Gambogic acid was determined by using atmospheric pressure chemical ionization (APCI) in a single quadrupole mass spectrometer. HPLC-APCI-MS was performed in the selected ion monitoring (SIM) mode using target ions at [M-H](-)m/z 627.4 for gambogic acid and [M-H](-)m/z 455.4 for the I.S. Calibration curve was linear over the range of 3.108-4144 microg/L. The lower limit of quantification was 3.108 microg/L. The intra- and inter-run precisions were less than 12.3 and 14.1%, respectively. The method has been successfully applied to study the pharmacokinetics of gambogic acid in patients with malignant tumour.

Atmospheric Pressure↗

PubMed2005

222Rn as indicator of atmospheric turbulence: measurements at Lake Maggiore and on the pre-Alps.

Radon concentration measurements in atmosphere were taken in years from 1997 to 1999 in Milan and at pre-alpine sites located north of Lombardy. In this paper the results of measuring campaigns and a comparison of radon levels observed in the hilly area north of the town and on the pre-Alps are reported. The general criteria of the measurements and the interpretative models of radon concentration are presented. The Lake Maggiore area shows evidence of a great nocturnal stability and frequent formation of Nocturnal Stable Layer. The peculiar findings in the high altitude stations confirm the use of radon as an indicator of atmospheric dispersion of pollutants in an area with complex orography. The afternoon minimum values are concordant for the different stations: this implies a remixing in afternoon hours over the whole area investigated.

Air Pollutants, Radioactive↗

PubMed2006

Atmospheric deposition of 137Cs between 1994 and 2002 at Cienfuegos, Cuba.

Levels of 137Cs in total atmospheric deposition have been measured in the Cienfuegos region (Cuba) between 1994 and 2002. Samples were collected every three months, evaporated to dryness to obtain residual samples, and measured by gamma spectrometry. The 137Cs mean concentration in total deposition was 0.24 Bq m(-2) and data ranged between < 0.05 and 0.62 Bq m(-2). Precipitation rates and raintime have proved to be the most important factors controlling the concentration and depositional flux of 137Cs in the atmosphere over Cienfuegos, showing a high correlation coefficient (R = 0.93).

Air Pollutants, Radioactive↗

PubMed2005

Estimating direct and episodic atmospheric nitrogen deposition to a coastal waterbody.

Direct deposition of atmospheric nitrogen to shallow coastal embayments is usually estimated, since insufficient field measurements are available. Using Waquoit Bay (Cape Cod, MA. USA) as a case study, and a recent review of literature, we determined reasonable bounds on wet and dry inputs of inorganic and organic N. Since precipitation and wind vary daily, we explored the potential of episodic events to stimulate phytoplankton blooms. Many coastal waterbodies like Waquoit Bay are small relative to their watersheds. Nevertheless, direct deposition of NH(3), NO(3)(-), and HNO(3) is significant in the loading budget. For Waquoit Bay, direct deposition was calculated to be 7-15.5 kg total N ha(-1)yr(-1), representing 70-150% of the atmospheric N reported to reach the bay via the watershed, and 20-45% of the total N reaching the bay from all land-based sources. Episodic events were estimated to deliver up to 65 mg N m(-2)day(-1), representing a phytoplankton stock of 12.3 mg Chl m(-2), an amount unlikely to stimulate dense blooms in shallow coastal waters in the northeastern United States.

Atmosphere↗

PubMed2005

Atmospheric entry simulations of Mars lander bioload--experiments in support of Beagle 2.

Simulations of the temperature and vacuum effects of Martian atmospheric entry upon Bacillus atrophaeus (formerly Bacillus subtilis var niger; 8058; NCIMB) endospores were carried out inside a purpose-built vacuum chamber. The work formed part of the study in support of planetary protection for the Beagle 2 Mars lander and investigated to what extent the outer surface of the lander's back heat shield would be sterilised during Mars atmospheric entry. The spores were heated to peak temperatures up to 300 degrees C over 30 s under vacuum conditions (10(-3) mbar). There was no effect on spore viability until peak temperatures reached 180-200 degrees C (12-15 s of heat exposure). Spore viability then fell rapidly with increasing temperature. Once peak temperatures exceeded 300 degrees C, no further spore viability was detected. The average heating rate was rapid (10 degrees C s(-1)); thus spores were exposed to peak temperatures for less than a second. These data inform on the process of determining bioburden reduction and control steps necessary for external surfaces of spacecraft which are non-sterile at launch, as well as providing new information about the ability of a model resistant organism to survive rapid, short-duration heating.

Atmosphere↗

PubMed2004

Studies on neurosteroids XVII. Analysis of stress-induced changes in neurosteroid levels in rat brains using liquid chromatography-electron capture atmospheric pressure chemical ionization-mass spectrometry.

The analysis of stress-induced changes in the brain neurosteroid levels by liquid chromatography (LC)-electron capture atmospheric pressure chemical ionization-mass spectrometry (ECAPCI-MS) is described. In the present method, neurosteroids were derivatized with a highly electron-affinitive reagent, 2-nitro-4-trifluoromethylphenylhydrazine (NFPH), to convert them to the corresponding hydrazones. The derivatized steroids showed over a 20-fold higher sensitivity in ECAPCI-MS than intact steroids measured by positive atmospheric pressure chemical ionization (APCI)-MS. Application of this method to the analysis of rat brain samples confirmed the significant increase in the levels of pregnenolone (PREG), progesterone (PROG), 5alpha-dihydroprogesterone (DHPROG), allopregnanolone (3alpha-hydroxy-5alpha-pregn-20-one; AP), and epiallopregnanolone (3beta-hydroxy-5alpha-pregn-20-one; EpiAP) in the fixated rats. The din stress, which we examined as a new short-term mental stress model, also elevated the brain neurosteroid levels. It is known that various types of stress lower the gamma-aminobutyric acid type A (GABA(A)) receptor function and induce the neuronal overexcitation. The increase in the brain level of AP, a potent positive modulator of GABA(A) receptors, may be the defensive response against acute stress. The increase in the brain concentration of its precursors, PREG, PROG, and DHPROG, may be associated with the acceleration of the AP synthesis. Thus, the present studies suggest that changes in the brain levels of neurosteroids may play an important role in the homeostatic mechanisms that counteract the inhibitory effect of stress on the GABA(A) receptor function.

Animals↗

PubMed2006

Passive landfill gas emission - Influence of atmospheric pressure and implications for the operation of methane-oxidising biofilters.

A passively vented landfill site in Northern Germany was monitored for gas emission dynamics through high resolution measurements of landfill gas pressure, flow rate and composition as well as atmospheric pressure and temperature. Landfill gas emission could be directly related to atmospheric pressure changes on all scales as induced by the autooscillation of air, diurnal variations and the passage of pressure highs and lows. Gas flux reversed every 20 h on average, with 50% of emission phases lasting only 10h or less. During gas emission phases, methane loads fed to a connected methane oxidising biofiltration unit varied between near zero and 247 g CH4 h(-1)m(-3) filter material. Emission dynamics not only influenced the amount of methane fed to the biofilter but also the establishment of gas composition profiles within the biofilter, thus being of high relevance for biofilter operation. The duration of the gas emission phase emerged as most significant variable for the distribution of landfill gas components within the biofilter.

Air Movements↗

PubMed2002

Atmospheric pressure photoionization liquid chromatographic-mass spectrometric determination of idoxifene and its metabolites in human plasma.

This paper describes a comparison between atmospheric pressure chemical ionization (APCI) and the recently introduced atmospheric pressure photoionization (APPI) interface for the LC-MS determination of idoxifene and its major metabolite, SB245419 (SB19), in human plasma. The results indicate that analyte response in APPI is highly dependent on the solvent composition, especially to water in the mobile phase. Other parameters investigated are the mobile phase flow-rate, the chemical noise, and signal suppression by matrix interferences. APPI appears to be six to eight times more sensitive than APCI for idoxifene and its SB245419 metabolite; the response for the SB245420 metabolite is considerably better than for APCI conditions, but still not sufficient for trace level pharmacokinetic determinations in human plasma. The LOQ for the parent drug and its major metabolite were 10 and 25 ng/ml, respectively, in human plasma. From post-column infusion experiments we conclude that there is little difference in matrix suppression between APCI and APPI. From these studies we suggest APPI may be an additional tool in pharmaceutical LC-MS applications.

Atmospheric Pressure↗

PubMed2003

"Cold" solid-phase microextraction method for the determination of volatile halocarbons present in the atmosphere at ultra-trace levels.

Anthropogenic volatile halocarbons are compounds of great enviromnental concern because of their involvement in global change phenomena. They are present in the atmosphere at concentration levels in the order of parts per trillion by volume. The chosen analytical method for their determination is capillary gas chromatography coupled to mass spectrometry, preceded by an enrichment step on suitable adsorbent resins. The method here presented makes use of the solid-phase microextraction as a pre-analytical technique, using sub-ambient temperature in order to enhance the retention capability of the fiber coating. The proposed method was evaluated in terms of extraction efficiency, linearity, reproducibility, andlimits of detection. Results obtained showed that trace atmospheric halocarbons are detectable even when enriching very small air sample volumes. A good chromatographic resolution is obtained as a consequence of the extremely low injection volume. Finally a standard GC-MS instrumentation equipped with a simple split-splitless injector was employed, thus avoiding the use of expensive dedicated apparatus. The method was also applied to the analysis of actual samples collected both in remote, and in semi-remote sites.

Air Pollutants↗