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PubMed2004

System for the generation of standard gas mixtures of volatile and semi-volatile organic compounds for calibrations of solid-phase microextraction and other sampling devices.

Standard gases are used for quality control and quality assurance, development of analysis methods and novel air sampling devices. The use of solid-phase microextraction (SPME) and other novel technologies for research in the area of air sampling and analysis requires systems/devices for reliable standard gas generation and sampling. In this paper we describe a new gas standard generating system for volatile organic compounds (VOCs) and semi-VOCs that was designed, built, and tested to facilitate fundamental and applications research with SPME. The system provided for the generation of a wide range of VOC/semi-VOC concentrations and mixing various standard gases, estimation of detection limits, testing the effects of sampling time, air temperature and relative humidity, testing the effects of air velocity and ozone on sampling/extractions. The system can be also used for calibrations of analytical instrumentation, quality control and quality assurance checks, and cross-validations of SPME with/and other sampling techniques.

Calibration↗
PubMed2006

Oxygen-induced concurrent ultrasonic degradation of volatile and non-volatile aromatic compounds.

Acoustic cavitation, induced by ultrasound, can be used to eliminate organic pollutants from water. This type of ultrasonic treatment of polluted water can be grouped with those generally referred to as advanced oxidative processes since it involves hydroxyl radicals. In this case these highly active species are generated from the dissociation of water and oxygen dissociation caused by cavitation bubble collapse. The cavitation induced degradation rates of organic compounds in water are mainly linked to their vapor pressure and solubility and here we will further explore these links by examining the degradation of a mixture of two materials with different physical properties, chlorobenzene and 4-chlorophenol. The results obtained when a dilute solution of a mixture of these compounds saturated with argon is subjected to sonication at 300 kHz, parallels previous observations achieved in an aerated aqueous medium at 500 kHz. The two compounds exhibit sequential degradation with the more volatile chlorobenzene entering the cavitation bubble and being destroyed first. The 4-chlorophenol degradation occurs subsequently only when the chlorobenzene has been completely destroyed. The two compounds exhibit different behavior when sonicated in water saturated with oxygen. Under these conditions the two compounds are degraded simultaneously, a remarkable result for which two explanations can be proposed, both of which are based on the formation of additional OH radical species: The ability to produce conditions for the simultaneous elimination of two organic compounds by the use of oxygen is of great importance in the developing field of ultrasonic water treatment.

Computer Simulation↗
PubMed1993

Absorption of volatile fatty acids from the rumen of lactating dairy cows as influenced by volatile fatty acid concentration, pH and rumen liquid volume.

The effect of rumen liquid volume, pH and concentration of volatile fatty acids (VFA) on the rates of absorption of acetic, propionic and butyric acids from the rumen was examined in lactating dairy cows. Experimental solutions introduced into the emptied, washed rumen comprised two different volumes (10 or 30 l), four levels of pH (4.5, 5.4, 6.3, 7.2) and three levels of individual VFA concentrations (20, 50 or 100 mM-acetic, propionic or butyric acid). All solutions contained a total of 170 mM-VFA and an osmotic value of 400 mOsmol/l. Absorption rates were calculated from the disappearance of VFA from the rumen corrected for passage with liquid phase to the omasum. An increase in initial fluid pH caused a reduction in fractional absorption rates of propionic and butyric acids. Increasing the initial pH from 4.5 to 7.2 reduced fractional absorption rates of acetic, propionic and butyric acids from 0.35, 0.67 and 0.85 to 0.21, 0.35 and 0.28/h respectively. The fractional absorption rates of all VFA were reduced (P < 0.05) by an increase in initial rumen volume. The fractional absorption rate of acetic acid was lower (P < 0.05) at an initial concentration of 20 mM than of 50 mM. The fractional absorption rate of propionic acid tended (P < 0.10) to decrease as the level of concentration increased while fractional absorption rate of butyric acid was not affected by butyric acid concentration. These results indicate that relative concentrations of VFA in rumen fluid might not represent relative production rates and that attempts to estimate individual VFA production from substrate digestion must take account of pH and VFA concentration.

Acetates↗
PubMedDate not supplied

Volatile, non-volatile and total N-nitroso compounds in bacon.

Twenty-five smoked and unsmoked fried bacon samples have been analysed by a group selective procedure to measure the concentration of apparent total N-nitroso compounds (ATNC). The levels of a range of individual N-nitroso compounds, including simple volatile N-nitrosamines, N-nitrosothiazolidines, N-nitrosamino acids and N-nitrosothiazolidine carboxylic acids have also been examined. Concentrations of ATNC varied from 430 to 6800 micrograms(N-NO)/kg with a mean of 2700 micrograms(N-NO)/kg. Protein-bound N-nitrosoproline was the most abundant compound detected in unsmoked bacon, mean 260 micrograms/kg, and on average accounted for 4% of the ATNC concentration. For smoked bacon, bound N-nitrosoproline was detected in levels of up to 890 micrograms/kg and contributed 5% to the ATNC total. The most abundant compound present in smoked bacon was N-nitrosothiazolidine-4-carboxylic acid, mean 660 micrograms/kg, and this accounted for 6% of the ATNC. N-Nitrosothiazolidine, mean 340 micrograms/kg, and 2-(hydroxymethyl)-3-nitrosothiazolidine-4-carboxylic acid, mean 180 micrograms/kg, were the next most prominent compounds detected in smoked bacon. The combined sum of all the individual N-nitroso compounds measured accounted for, on average, 16% of the total ATNC. The identities of the N-nitroso compounds comprising the majority of the ATNC in bacon remain unknown.

Animals↗
PubMed1976

Volatile fatty acid metabolism in sheep. 1. Average daily volatile fatty acid production in the rumen of sheep fed lucerne hay.

Changes in the total concentration of the volatile fatty acid (VFA) pool in the rumen were followed over a 24 hour period in 2 groups of sheep, 1 fed at 08h00 and the other twice daily at 08h00 and 20h00. Although similar maximum (143 and 147 meq/1) and average (100, 3 and 102, 1 meq/1) levels were found in the 12 and 24 h groups respectively, the twice daily feeding regimen resulted in a lower variation (S.D.=17, 0 meq/1 and 28, 9 meq/1 respectively). It was concluded from changes in the percentage molar composition of the VFA pool over the same period that the other of VFA absorption from the rumen was propionate greater than acetate greater than butyrate for both groups, but that the differences were less marked for the twice daily fed sheep. Long term infusions of 14C labelled acetic, propionic and butyric acids into the rumen of sheep fed a total of 1 600 g lucerne hay twice daily (08h00 and 20h00), gave an average net total VFA production rate of 4,52+/-1,01 moles/800 g/12 hours irrespective of the acid infused. The net individual turnover rates for acetic (2,81 moles/12 h), propionic acid (0,82 moles/12 h) and butyric acid (0,55 moles/12 h), derived by the subtraction of the inter-conversion factors from the gross production rates of the acids, and expressed as the percentage contribution of each acid to the total net VFA turnover (acetic=62%, propionic=18% and butyric=12%) closely resembled the percentage molar composition of the VFA pool in the rumen (acetic=60%, propionic=23% and butyric=12%). The total net VFA production was found to be directly proportional to the total VFA concentration in the rumen (correlation coefficient=0,83), and the relationships can be described by the equation y=0,034 x + 0,16 where y=VFA production in moles/12 hour and x=VFA concentration in meq/1. A specific VFA production rate of 0,85 moles per 100 g digestible organic matter was calculated from the average daily VFA production rate and the composition of the lucerne hay.

Acetates↗
PubMed2006

Air sampling with Empore solid phase extraction membranes and online single-channel desorption/liquid chromatography/mass spectrometry analysis: determination of volatile and semi-volatile organophosphate esters.

A method for determining organophosphate esters in air samples using C8 Empore solid phase extraction (SPE) membranes has been developed. After the sampling the analytes trapped in the membrane are completely desorbed with methanol, using an extraction cell connected online to the organic modifier channel of a HPLC gradient pump. The addition of water to the mobile phase prior to analytical chromatography ensures that the analytes are refocused and efficiently separated. Sampling with Empore SPE membranes enables the collection of analytes in both the vapour phase and particulate matter. During the air sampling procedure no losses were observed after 24 h of sampling, yielding a total volume of 14.4 m3, even for the most volatile compound used in this investigation (trimethylphosphate). Complete desorption was observed for all the organophosphate esters and recoveries were greater than 95%, with a relative standard deviation of less than 8%. The limits of detection ranged between 0.4 and 19 pg/m3. The effect of particulate matter on the extraction efficiency was investigated in detail by spiking the membranes with reference standard material. It was also found that the SPE membranes could be stored for at least 5 days at room temperature without any evidence of loss. The efficacy of the method was verified using real samples from different common indoor environments. Interestingly, significant quantities of several phosphate esters were found in a NIST standard reference material (urban dust, SRM 1649a).

Air Pollutants↗
PubMed1989

Gas chromatographic determination of volatile anaesthetic agents in blood. Part 1. Preparation of standard gas mixtures of volatile anaesthetic agents.

A method for preparing standard gas mixtures of the volatile anaesthetics halothane, enflurane and isoflurane is described. Static mixtures of gases of known concentration can be prepared manometrically by measuring the required pressure of anaesthetic gas into a bulb and diluting to atmospheric pressure with air. Standard gas mixtures in the concentration range 0-4% V/V can be prepared with an accuracy of +/- 0.01% V/V, and the relative standard error of measurements of a single standard concentration is less than 0.8%. Significant adsorptive losses in the gas sampling valve were observed for gas standards prepared in the absence of any diluent gas. These losses were not detected for measurements of standards made up to atmospheric pressure in air. A comparison with calibration procedures currently in practice is presented.

Anesthetics↗
PubMed1985

Capillary gas chromatographic analysis of volatile and non-volatile organic acids from biological samples as the t-butyldimethylsilyl derivatives.

A quantitative procedure for the analysis of volatile organic acids and lactic acid in silage is described. The samples were extracted with diethyl ether, derivatized by t-butyldimethylsilylation, and then separated by capillary gas chromatography. The same procedure was useful for the identification by gas chromatography/mass spectrometry of organic acids in samples such as the metabolic fermentation products of anaerobic bacteria.

Acids↗
PubMed1980

Further studies on the occurrence of volatile and non-volatile nitrosamines in foods.

Approximately 250 samples of various foods, such as cured meat products, fried bacon, cooked-out bacon fats, baby foods containing meats, tomato products, cooked pizza, powdered and evaporated milk, mushrooms and different varieties of alcoholic beverages, were analysed by GLC-TEA for the presence of volatile nitrosamines. The levels detected in cured meat products (both cooked and uncooked) were very low, and both their incidence (at greater than 1 microgram/kg) and concentrations were much lower than those observed in a 1974 survey. The levels of N-nitrosopyrrolidine (NPYR) in fried bacon and cooked-out bacon fats were also somewhat lower than those observed at the end of 1976, but the decrease may not be significant. Traces (mean, 1.5 micrograms/kg) of N-nitrosodimethylamine (NDMA) were detected in 21 of 22 samples of beers and ales. Most of the remaining foods gave negative results, excepting the skim milk powders, which contained minute traces (mean, 0.4 micrograms/kg) of NDMA. An HPLC-TEA method was developed for the analysis of N-nitrosoproline (NPRO) and N-nitrososarcosine (NSAR) in raw and fried bacon. A study of the heat-induced decarboxylation of these nitrosamino acids suggests that these compounds are heat-labile and would not be expected to occur in fried foods at significant levels. Their presence, however, may lead to the formation of traces of NPYR and NDMA during frying at lower temperatures.

Beverages↗
PubMed2005

A chemical investigation by headspace SPME and GC-MS of volatile and semi-volatile terpenes in various olibanum samples.

Six different olibanum samples with certified botanical origin were analyzed by headspace SPME-GC/MS in order to define their mono-, sesqui- and diterpenic composition, as pertinent criteria of identification. Boswellia carteri and Boswellia sacra olibanum have quite similar chemical composition, with isoincensole acetate as the main diterpenic biomarker. Although Boswellia serrata olibanum also exhibits this biomarker, the presence of methylchavicol, methyleugenol and an unidentified oxygenated sesquiterpene distinguishes B. serrata olibanum from the two other species. The characteristic chemical compounds of Boswellia papyrifera are the diterpenic biomarkers incensole and its oxide and acetate derivatives, n-octanol and n-octyl acetate. Boswellia frereana olibanum is devoid of diterpenes of the incensole family but contains a high amount of many dimers of alpha-phellandrene. The chemical composition of olibanum, which is demonstrated to be different for each Boswellia species allowed the determination of the taxonomic origin of frankincense samples purchased on various markets in East Africa, in the Near East and in Yemen. Moreover, terpenic fingerprints allowed the botanical origin of olibanum used in traditional incense mixtures to be identified. Furthermore, this study gave us the opportunity to assign a botanical origin to an archaeological frankincense sample.

Boswellia↗