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At least 289 records · Page 16Linked to original sources
PubMed2002

Selectivity enhancement for high-speed GC analysis of volatile organic compounds with portable instruments designed for vacuum-outlet and atmospheric-pressure inlet operation using air as the carrier gas.

A tandem ensemble of two 4.5-m-long x 0.25-mm-i.d. capillary columns with the first using a 0.50-microm film of nonpolar dimethyl polysiloxane and the second using a 0.25-microm film of polar trifluoropropylmethyl polysiloxane is operated with atmospheric pressure air as the carrier gas and an outlet pressure of 50.5 kPa established using a small vacuum pump. A thicker stationary-phase film is used in the first column to increase retention for very volatile compounds. This significantly increases the resolution of these compounds. The thicker film in the first (nonpolar) column decreases the polarity of the tandem column ensemble and, thus, changes its selectivity. A low-dead-volume valve, connected between the column junction point and a source of atmospheric pressure air, is used to obtain pulsed modulation of the carrier gas flow through the column ensemble. When the valve is open, the ensemble inlet pressure and the junction-point pressure are nearly the same, and carrier gas flow nearly stops in the first column, and flow in the second column increases. Enhanced resolution of a component pair that is separated by the first column but coelutes from the column ensemble can be obtained if the valve is opened for a few seconds after one of the components has crossed the junction and is in the second column, but the other component is still in the first column. A sequence of appropriately timed pulses is used to obtain enhanced resolution of several pairs of components that coelute from the column ensemble. These methods enabled the complete separation of an 18-component vapor mixture of common solvents in air in 3.5 min.

Air↗
PubMed2003

The influence of atmospheric pressure on landfill methane emissions.

Landfills are the largest source of anthropogenic methane (CH4) emissions to the atmosphere in the United States. However, few measurements of whole landfill CH4 emissions have been reported. Here, we present the results of a multi-season study of whole landfill CH4 emissions using atmospheric tracer methods at the Nashua, New Hampshire Municipal landfill in the northeastern United States. The measurement data include 12 individual emission tests, each test consisting of 5-8 plume measurements. Measured emissions were negatively correlated with surface atmospheric pressure and ranged from 7.3 to 26.5 m3 CH4 min(-1). A simple regression model of our results was used to calculate an annual emission rate of 8.4 x 10(6) m3 CH4 year(-1). These data, along with CH4 oxidation estimates based on emitted landfill gas isotopic characteristics and gas collection data, were used to estimate annual CH4 generation at this landfill. A reported gas collection rate of 7.1 x 10(6) m3 CH4 year(-1) and an estimated annual rate of CH4 oxidation by cover soils of 1.2 x 10(6) m3 CH4 year(-1) resulted in a calculated annual CH4 generation rate of 16.7 x 10(6) m3 CH4 year(-1). These results underscore the necessity of understanding a landfill's dynamic environment before assessing long-term emissions potential.

Atmospheric Pressure↗
PubMed2004

Determination of atractyloside in Callilepis laureola using solid-phase extraction and liquid chromatography-atmospheric pressure ionisation mass spectrometry.

A selective analytical method based on high-performance liquid chromatography, combined with atmospheric pressure ionisation mass spectrometry, was developed for the detection of atractyloside. The analysis was performed on an Xterra Phenyl column utilising a gradient elution profile and a mobile phase consisting of 10 mM aqueous ammonium acetate buffer-methanol-acetonitrile. The calibration curve of the method (1 ng/ml-160 microg/ml) was best described by a second order polynomial function (r2 = 0.998) but displayed good linearity in the range of 100 ng/ml-1 microg/ml (r2 = 0.999). The limit of detection for the atractyloside standard was determined and found to be 100 pg/ml and the limit of quantification of atractyloside in tuber matrix was found to be 250 pg/ml. The relative standard deviation of the method was on average below 5% (n = 8). The method was successfully applied to the analysis of Callilepis laureola tubers and unknown powdered samples for the presence of atractyloside.

Atmospheric Pressure↗
PubMed2004

Atmospheric pressure photoionization-mass spectrometry with a microchip heated nebulizer.

A novel, microfabricated heated nebulizer chip for atmospheric pressure photoionization-mass spectrometry (APPI-MS) is presented. The chip consists of fluidic and gas inlets, a mixer, and a nozzle etched onto silicon wafer that is anodically bonded to a Pyrex glass wafer, on which an aluminum heater is sputtered. A krypton discharge lamp is used as the source for 10-eV photons to initiate the photoionization process. Dopant, delivered as part of the sample solution, is used to achieve efficient ionization. The use of the microfabricated heated nebulizer with APPI in the analysis of four analytes is demonstrated, and the spectra are compared to those obtained with a conventional APPI source. Ionization in positive and negative ion modes was successfully achieved and the spectra were mainly similar to those obtained with conventional APPI, indicating that the ionization in microfabricated and conventional APPI sources takes place by the same mechanisms. The flow rates with conventional APPI are approximately 100 muL/min, whereas the microchip heated nebulizer allows the use of flow rates 0.05-5 muL/min, thus being compatible with microfluidic separation systems or micro- and nano-LC. A stable signal was demonstrated throughout a 5-h measurement, which proved the excellent stability of the micro-APPI. The same heated nebulizer chip can be used for weeks.

Atmospheric Pressure↗
PubMed1998

Rapid target analysis of microcontaminants in water by on-line single-short-column liquid chromatography combined with atmospheric pressure chemical ionization ion-trap mass spectrometry.

The applicability of trace enrichment and separation of microcontaminants on a single 10 x 2 mm I.D. high-pressure-packed liquid chromatography (LC) column, combined on-line with an atmospheric pressure chemical ionization (APCI)-ion-trap tandem mass spectrometry (MS-MS) instrument was studied for the target analysis of herbicides in river water. The total analysis time was 15-20 min. With the on-line short-column LC-MS-MS method, detection limits of 0.1-1 microgram/l can be achieved using only 4 ml of river water. However, the results obtained for a mixture of six triazines were considerably better than those for a mixture of eight phenylureas. An attempt is made to explain this difference on the basis of various processes that occur within the ion trap and the measurement procedure itself.

Atmospheric Pressure↗
PubMed2000

Monitoring of priority pesticides and other organic pollutants in river water from portugal by gas chromatography-mass spectrometry and liquid chromatography-atmospheric pressure chemical ionization mass spectrometry.

Gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-atmospheric pressure chemical ionization mass spectrometry (LC-APCI-MS) were optimized and applied for the trace-level determination of 42 priority pesticides and 33 priority organic pollutants from European Union Directive EC 76/464. First, off-line solid-phase extraction of 200 ml of river water using an OASIS solid-phase extraction cartridge, followed by GC-MS was used. Next, selected samples that were positive to GC-MS were analyzed by LC-APCI-MS in order to detect further polar byproducts or to improve the determination of previously detected polar analytes. The transformation products of triazine pesticides like deethylatrazine (DEA) and deisopropylatrazine (DIA) and compounds such as diuron and several chlorophenols were positively identified by LC-APCI-MS. The present methodology has also been used for searching for new analytes not included in the EC 76/464 list, like Irgarol, DEA and DIA. In addition it was applied to target pollutants in 43 river water samples from Portugal during a pilot survey from April to July 1999. Atrazine followed by simazine and 2,4,6-trichlorophenol were the most ubiquitous compounds detected in this area. The levels detected of the different compounds were in the range of: 0.01-2.73 microg/l, 0.05-0.74 microg/l, 0.02-1.65 microg/l, 0.02-5.43 microg/l, 0.01-0.40 microg/l, 0.01-0.26 microg/l, 0.02-0.61 microg/l, 0.01-3.90 microg/l, 0.01-1.24 microg/l, 0.02-2.3 microg/l, 0.01-0.13 microg/l and 0.01-0.5 microg/l for atrazine, simazine, terbuthylazine, alachlor, metolachlor, Irgarol, propanil; tributhylphosphate, diuron, 2,4,6-trichlorophenol, deisopropylatrazine and deethylatrazine, respectively.

Atmospheric Pressure↗
PubMedDate not supplied

The potential for use of steam at atmospheric pressure to decontaminate or sterilize parenteral filling lines incorporating barrier isolation technology.

Barrier isolators that enclose aseptic filling equipment are being proposed as a means of: (1) assisting in achieving a 10(-6) sterility assurance level (SAL) in the filling area and (2) minimizing the clean environment required in the manufacturing area. The need for operator and maintenance access to the interior of the barrier isolators presents difficulties in achieving the above goals. Several methods are available for reducing the microbial level inside the isolation barrier. If the objective is the decontamination of all surfaces inside the enclosure, saturated steam at atmospheric pressure can be used. If the objective is to sterilize the inside of the enclosure, saturated steam at atmospheric pressure with added H2O2 can be used. Test data and practical interface considerations relative to various methodologies will be reviewed.

Air Pressure↗
PubMed2002

Identification of nitrate ester explosives by liquid chromatography-electrospray ionization and atmospheric pressure chemical ionization mass spectrometry.

Liquid chromatography-mass spectrometry (LC-MS) with electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI), in the negative-ion mode, was investigated for the analyses of three widely used nitrate ester explosives, pentaerythritol tetranitrate, nitroglycerin and ethylene glycol dinitrate, as well as six additional nitrate esters, using post-column additives. In ESI, ammonium nitrate, sodium nitrite, propionic acid and ammonium chloride promoted formation of characteristic adduct ions of the respective nitrate esters. In APCI, chlorinated agents, dichloromethane, chloroform, carbon tetrachloride and ammonium chloride, were employed, fanning chloride attachment adduct ions. Three forensic samples, Booster DYNO, Semtex and Smokeless Powder, were analyzed to demonstrate the validity of the developed LC-MS methods.

Atmospheric Pressure↗
PubMed2001

Triacylglycerol analysis of potential margarine base stocks by high-performance liquid chromatography with atmospheric pressure chemical ionization mass spectrometry and flame ionization detection.

Several margarine base stock candidates have previously been prepared for the purpose of finding better, more oxidatively stable food components: high-saturate vegetable oils, randomized vegetable oils, vegetable oil-hard stock blends, and interesterified vegetable oil-hard stock blends. Here are reported the triacylglycerol compositions of these products, determined using reverse-phase high-performance liquid chromatography (HPLC) coupled with a flame ionization detector or a quadrupole mass spectrometer with an atmospheric pressure chemical ionization source. Triacylglycerol percent composition results for samples of known composition (randomized and interesterified samples) exhibited less average error by HPLC coupled with a quadrupole mass spectrometer with an atmospheric pressure chemical ionization source, after application of response factors, than the results by HPLC coupled with a flame ionization detector. The fatty acid compositions calculated from the mass spectrometric data exhibited less average error than the fatty acid compositions resulting from the flame ionization detector data. The average error of the fatty acid compositions by the mass spectrometer was lowest for interesterified blend samples, next lowest for randomized samples, then followed by high-saturated fatty acid oils, normal oils, and blends. Analysis of the vegetable oil-hard stock blends by mass spectrometer required special treatment for calculation of response factors.

Chromatography, High Pressure Liquid↗
PubMed2003

Observation of different ceramide species from crude cellular extracts by normal-phase high-performance liquid chromatography coupled to atmospheric pressure chemical ionization mass spectrometry.

Normal-phase high-performance liquid chromatography (NP-HPLC) coupled to atmospheric pressure chemical ionization mass spectrometry (APCI-MS) allows qualitative analysis of endogenous ceramide and dihydroceramide species from crude lipid extracts utilizing chromatographic methods readily adaptable from commonly used thin layer chromatography (TLC) conditions. Qualitative information for the species comes from observation of differences in chromatographic and mass spectrometric behavior between species. Application to the analysis of ceramide and dihydroceramide from various cell lines is demonstrated. The results show the species profile in each cell line to be unique despite growth under identical conditions. The results from APCI-MS analysis corroborate and enhance information acquired from use of the diacylglycerol kinase assay for total ceramide measurement. This technique readily allows the previously difficult distinction between ceramide and dihydroceramide species.

Atmospheric Pressure↗
PubMed2005

Investigations of taxoids by electrospray and atmospheric pressure chemical ionization with tandem mass spectrometry.

The fragmentation behavior of taxoids was studied using electrospray (ESI) and atmospheric pressure chemical ionization (APCI) sources with multi-stage tandem mass spectrometry. In the positive ion mode taxoids gave prominent [M+Na]+ and [M+K]+ ions with the ESI source, and [M+NH4]+ or [M+H]+ ions with the APCI source. The MS/MS fragmentations of ions produced by APCI and ESI sources were very similar. For both sources, the presence of cinnamoyl or benzoyl groups could be characterized by initial losses of 148 or 122 u, respectively, from molecular adduct ions. However, the elimination of cinnamic acid was relatively difficult for the molecular adduct ions formed by APCI, and was comparable in importance to the loss of acetic acid. The other fragments involved losses of CH2CO, CO, and H2O. The 5/7/6 type taxoids underwent characteristic losses of 58 or 118 u from ions produced by both APCI and ESI sources. The fragmentation behavior was remarkably influenced by substitution locations. The elimination of the C-10 benzoyl group was usually the first fragmentation step, while that of the C-2 benzoyl group was relatively difficult. The acetoxyl group at C-7 was more active than those at C-2, C-9, and C-10, which in turn were more active than that at C-4. These fragmentation rules could facilitate the rapid screening and structural characterization of taxoids in plant extracts by high-performance liquid chromatography/mass spectrometry (HPLC/MS).

Atmospheric Pressure↗
PubMed1999

Atmospheric pressure changes and outdoor temperature changes in relation to spontaneous pneumothorax.

STUDY AIMS: To examine the influence of atmospheric pressure (AP) and temperature changes on the incidence of idiopathic spontaneous pneumothorax (SP). METHODS: From December 1991 through November 1993, 115 consecutive SP cases were selected. Patients were included after being in Amsterdam at least 1 full day before contracting the SP. Differences in air temperature and AP (provided hourly by the national weather bureau) for the days of the SP occurrence and the days previous to it were recorded to measure influences of air temperature and AP. The correlation between days with lightning and SP and clustering of SP was evaluated. RESULTS: SP occurred on 14.7% of the days in the 2-year period. There was no relationship between SP and a rise or fall in AP (Poisson regression). There was an average temperature rise of 0.57 degrees C from the day prior to the day of the SP, compared with a 0.08 degrees C fall on the days without SP. This difference is statistically significant and was consistent over the four seasons and both years. Seventy-three percent of the SP cases were clustered. A relationship between SP and thunderstorms was found. CONCLUSIONS: AP differences do not seem to influence the chance of developing SP. SP occurs in clusters, and more often 1 to 2 days after thunderstorms. Whether the identified temperature rise prior to the SP is a causative factor is unlikely; coexisting weather phenomena might explain this unexpected finding and should be studied in the future.

Adult↗
PubMed2002

Impact of surface heterogeneity on mercury uptake by carbonaceous sorbents under UHV and atmospheric pressure.

Chemical and morphological heterogeneities of carbon sorbents play important roles in gas-phase adsorption. However, the specific chemical complexes and topological structures of carbon that favor or impede elemental mercury uptake are not well understood and are the subject of this study. Temperature programmed desorption (TPD) with a model carbonaceous material (highly oriented pyrolytic graphite, HOPG) under ultrahigh vacuum (UHV) conditions and fixed bed adsorption by activated carbon (BPL) at atmospheric pressure were combined to investigate the effects of chemical and morphological heterogeneities on mercury adsorption by carbonaceous surfaces. TPD results show that mercury adsorption at 100 K onto HOPG surfaces with and without chemical functional groups and topological heterogeneity created by plasma oxidation occurs through physisorption. The removal of chemical functionalities from the HOPG surface enhances mercury physisorption. Plasma-oxidation of HOPG provides additional surface area for mercury adsorption. However, the pits created by plasma oxidation are more than 10 nm in diameter and do not simulate microporosity that predominates in activated carbons. Mercury adsorption by activated carbon at atmospheric pressure occurs through two distinct mechanisms. Physisorption governs mercury adsorption at lower temperatures (i.e., below 348 K), while chemisorption predominates at high adsorption temperatures (i.e., above 348 K). Presence of water on activated carbon surface enhances mercury uptake by both physisorption and chemisorption. Oxygen containing functional groups reduce mercury uptake by physisorption by blocking access to the micropores. No significant impact of oxygen functionalities was observed in the chemisorption regime. The key findings of this study open the possibility to apply scientific information obtained from the studies with simple surfaces such as HOPG under ideal conditions (UHV) to industrial sorbents under realistic process conditions.

Adsorption↗
PubMed2005

Spectroscopic characterization of two different microwave (2.45 GHz) induced argon plasmas at atmospheric pressure.

A surface-wave-sustained discharge created by using a surfatron device in a tube open to the atmosphere can be used to maintain a microwave (2.45 GHz) plasma at atmospheric pressure at powers of less than 300 W. The TIA (Torche a Injection Axiale) is a device also producing a plasma that, moreover, permits us to work at high power (higher than 200 W and up to 1000 W). A study of the departure from the thermodynamic equilibrium existing in the argon plasmas created by both devices has been done by using optical emission spectroscopy techniques in order to characterize them and to evaluate their possible advantages when they are used for applied purposes.

Argon↗
PubMed2001

Characterisation of humic substances using atmospheric pressure chemical ionisation and electrospray ionisation mass spectrometry combined with size-exclusion chromatography.

Humic substances were analysed by atmospheric pressure chemical ionisation (APCI) and electrospray ionisation (ESI) mass spectrometry in positive and negative modes. Using APCI the average m/z range of humic substances was reduced 5-fold compared to ESI. High-resolution time-of-flight mass spectrometry revealed the formation of multiply charged molecules in the ESI mode. Moreover, it was possible to obtain daughter ion mass spectra of humic substances by nanospray tandem mass spectrometry. The size-exclusion chromatography elution profile of humic substances was highly influenced by the pH of the analyte solution. By contrast, the pH had no significant influence on the observed mass spectra of humic substances.

Atmospheric Pressure↗
PubMed2003

Evaluation of an atmospheric pressure chemical ionization interface for capillary electrophoresis-mass spectrometry.

A simple and inexpensive approach to modify a commercial atmospheric pressure chemical ionization (APCI) interface was proposed for capillary electrophoresis-mass spectrometry (CE-MS). In order to accommodate lower flow rates in the range 1-10 microl/min, both sheath liquid and nebulizing gas were coaxially supplied to the nebulizer as an arrangement of pneumatically assisted electrospray interface. Since this paper focused on the primary study of the modified APCI interface, the performance of the interface was first evaluated by the direct infusion of a reserpine solution. Optimization of several APCI parameters, such as temperature of APCI vaporizer, nebulizing gas flow and APCI corona discharge current, were accomplished. The orifice dimension for the nebulizing gas flow was largely independent of the MS sensitivity when the nebulizing gas flow rate was ca. 0.4 l/min. A successful CE-APCI-MS separation is obtained using the modified APCI interface.

Atmospheric Pressure↗