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Results for “Journal of Chromatographic Science”

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USGS1977

An automated glass capillary gas chromatographic system for routine quantitative analysis

A steel capillary gas chromatographic system, based on the Hewlett-Packard (HP) Model 5711A gas chromatograph and HP model 3354A laboratory data system, was converted to an automated glass capillary system suitable for routine quantitative analysis of trace levels of hydrocarbons. Two instrument modifications, which were required for a fully automated system, are described. The system was tested with two different column installation methods. The HP recommended method of column installation showed much less discrimination against high molecular weight compounds than did a simpler column installation technique that introduced excessive dead volume (unswept by the carrier gas) into the HP Model 18740A glass capillary inlet system. Discrimination against high molecular weight compounds was shown to adversely affect their quantification. Data on the accuracy and precision of quantitative analyses of 18 hydrocarbons covering a wide range of boiling points and polarities are presented for both column installation techniques. Retention time reproducibiiity data for the same 18 compounds are also included.

Journal of Chromatographic Science↗
USGS1971

Isotope fractionation during gas chromatographic separations

Physical interaction between the sample and stationary phase during GC separations may result in severe isotopic fractionation of the effluent, making it essential to collect it totally in order to obtain quantitative results. When carbon dioxide was eluted through a Porapak column the front portions of the elution peak was enriched in 13 C. When methane was eluted through molecular sieve, both the heavier species were eluted faster than the lighter ones. However, when the carbon dioxide was eluted through silica gel the first CO 2 eluted was enriched in 13 C and the last CO 2 eluted was enriched in 18 O. This behavior of the isotopes probably indicates the presence of two different interaction mechanisms.

Journal of Chromatographic Science↗
USGS2002

Liquid chromatographic determination of florfenicol in the plasma of multiple species of fish

A simple method was developed for determining florfenicol concentration in a small volume (250 μl) of plasma from five phylogenetically diverse species of freshwater fish. Florfenicol was isolated from the plasma matrix through C 18 solid-phase extraction and quantified by reversed-phase high-performance liquid chromatography with UV detection. The accuracy (84–104%), precision (%RSD⩽8), and sensitivity (quantitation limit <30 ng/ml) of the method indicate its usefulness for conducting pharmacokinetic studies on a variety of freshwater fish.

Journal of Chromatography B: Analytical Technologi↗
USGS2007

An automated approach to detecting signals in electroantennogram data

Coupled gas chromatography/electroantennographic detection (GC-EAD) is a widely used method for identifying insect olfactory stimulants present in mixtures of volatiles, and it can greatly accelerate the identification of insect semiochemicals. In GC-EAD, voltage changes across an insect's antenna are measured while the antenna is exposed to compounds eluting from a gas chromatograph. The antenna thus serves as a selective GC detector whose output can be compared to that of a "general" GC detector, commonly a flame ionization detector. Appropriate interpretation of GC-EAD results requires that olfaction-related voltage changes in the antenna be distinguishable from background noise that arises inevitably from antennal preparations and the GC-EAD-associated hardware. In this paper, we describe and compare mathematical algorithms for discriminating olfaction-generated signals in an EAD trace from background noise. The algorithms amplify signals by recognizing their characteristic shape and wavelength while suppressing unstructured noise. We have found these algorithms to be both powerful and highly discriminatory even when applied to noisy traces where the signals would be difficult to discriminate by eye. This new methodology removes operator bias as a factor in signal identification, can improve realized sensitivity of the EAD system, and reduces the number of runs required to confirm the identity of an olfactory stimulant. ?? 2007 Springer Science+Business Media, LLC.

Journal of Chemical Ecology↗
USGS1990

Selenium speciation methods and application to soil saturation extracts from San Joaquin Valley, California

Methods to determine soluble concentrations of selenite, selenate, and organic Se were evaluated on saturation extracts of soil samples collected from three sites on the Panoche Creek alluvial fan in the western San Joaquin Valley, California. The methods were used in combination with hydride-generation atomic-absorption spectrometry for detection of Se, and included a selective chemical-digestion method and three chromatographic methods using XAD-8 resin, Sep-Pak C 18 cartridge, and a combination of XAD-8 resin and activated charcoal. The chromatography methods isolate dissolved organic matter that can inhibit Se detection by hydride-generation atomic-absorption spectrometry. Isolation of hydrophobic organic matter with XAD-8 did not affect concentrations of selenite and selenate, and the isolated organic matter represents a minimal estimation of organic Se. Ninety-eight percent of the Se in the extracts was selenate and about 100% of the isolated organic Se was associated with the humic acid fraction of dissolved organic matter. The depth distribution of Se species in the soil saturation extracts support a hypothesis that the distribution of soluble Se and salinity in these soils is the result of evaporation from a shallow water table and leaching by irrigation water low in Se and salinity.

California↗
USGS2003

Formation and loss of humic substances during decomposition in a pine forest floor

Since twice as much C is sequestered in soils as is contained in the atmosphere, the factors controlling the decomposition rate of soil C are important to the assessment of the effects of climatic change. The formation of chemically resistant humic substances might be an important process controlling recycling of CO 2 to the atmosphere. Our objectives were to measure the rate of formation and loss of humic substances during 13 yr of litter decomposition . We placed nets on the floor of a white pine (Pinus strobus) forest to separate each annual layer of litter for 13 yr and measured humic substance concentration using NaOH extraction followed by chromatographic fractionation. The humic acid fraction increased from 2.1% of the C in litterfall to 15.7% after 1 yr. On a grams per square meter (g m -2 ) basis the humic substance fraction increased during the first year and then declined, with a half decay time (t 1/2 ) of 5.1 yr, which was significantly slower than the bulk litter (t 1/2 = 3.9 yr). The carboxylic C concentration estimated from 13 C nuclear magnetic resonance (NMR) increased in the litter over time, though total mass of carboxylic acid C in the forest floor also declined over the 13-yr period (t 1/2 = 4.6 yr). While humic substances in the forest floor decomposed at a somewhat slower rate than bulk litter during Years 1 to 13, they decomposed much faster than has been calculated from 14 C dating of the refractory fraction of organic matter in the mineral soil.

Soil Science Society of America Journal↗
USGS1982

A rapid high-performance liquid-chromatographic method for simultaneously determining the concentrations of TFM and Bayer 73 in water during lampricide treatments

The high-performance liquid-chromatography (HPLC) procedure requires only minutes per sample, is specific, and is relatively sensitive (limit of detection < 0.005 mg/L for both chemicals). A combined buffer (pH 4) and internal standard (3-chlorodiphenylamine) reagent is added to the water sample, which is injected through a Sep Pak C 18 disposable cartridge. The cartridge adsorbs and retains both the lampricides and the internal standard. The quantitative elution of the three chemicals from the cartridge with a small volume of methanol effectively concentrates the sample and provides sample cleanup. The methanol extract is then analyzed directly by HPLC on an MCH 10 reverse phase column by using a methanol:0.01 mol/L acetate buffer (87:13, v:v) as the mobile phase at 2 mL/min and detected by ultraviolet spectrophotometry at 330 (or 254) nm. A microprocessor data system further facilitates the procedure by quantifying off-scale peaks and yielding results directly in units of concentration (mg/L).

Canadian Journal of Fisheries and Aquatic Sciences↗