Versatile injection system for gas chromatography
Evaporative injector system for capillary column gas chromatography for solutes in dilute solution
Donaldson, R.↗
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The determination of cyclohexylamine in aqueous solutions of sodium cyclamate by electron-capture gas chromatography.
A sensitive primary amine assay, capable of detecting 10 to the minus 11th g and utilizing the determination of the amine N-2,4-dinitrophenyl derivative by electron-capture gas chromatography is described. The method is exemplified by the determination of cyclohexylamine in sodium cyclamate.
Solomon, M. D.↗
Capillary gas chromatography with two new moderately high temperature phases.
Gas chromatography test results are presented for two new moderately high-temperature phases of Dexsil 400-GC with free hydroxyl end groups (uncapped) and with end groups covered by trimethyl silyl groups (capped). The two Dexsil 400-GC phases were tested for their ability to resolve N-TFA-DL-(+)-2-butyl esters and n-butyl esters, as well as fatty acid methyl esters and hydrocarbon standards. Generally the more polar uncapped phase was superior to the capped phase in all separation comparisons, except for the hydrocarbons.
Pollock, G. E.↗
"Dry-column" chromatography of plant pigments
Separation of plant pigments which can be accomplished on thin-layer silica plates with mixture of petroleum ether, halocarbon, acetone, and polar solvent can be readily translated into dry-column technique that yields reproducible chromatograms after elution in fashion of liquid chromatography with fluorimeter as detector. Best solvent system was found to be mixture of petroleum ether, dichloromethane, acetone, and ethyl acetate.
Woeller, F. H.↗
Soil moisture by extraction and gas chromatography
To determine moisture content of soils rapidly and conveniently extract moisture with methanol and determine water content of methanol extract by gas chromatography. Moisture content of sample is calculated from weight of water and methanol in aliquot and weight of methanol added to sample.
Merek, E. L.↗
Gas-liquid chromatography in lunar organic analysis.
Gas-liquid chromatography (GLC) is a powerful and sensitive method for the separation and detection of organic compounds at nanogram levels. The primary requirement for successful analyses is that the compounds of interest must be volatile under the chromatographic conditions employed. Nonvolatile organic compounds must be converted to volatile derivatives prior to analysis. The derivatives of choice must be both amenable to chromatographic separation and be relatively stable. The condition of volatility necessitates the development of efficient derivatization reactions for important groups of compounds as amino acids, carbohydrates, nucleosides, etc. Trimethylsilylation and trifluoroacetylation represent specific areas of recent prominence. Some relevant practical aspects of GLC are discussed.
Gehrke, C. W.↗
The determination of soil moisture by extraction and gas chromatography
Soil moisture content was determined by extracting soil with methanol and subsequently analyzing the extract for water by gas chromatography. With air-dried mineral soils, this method gave slightly higher moisture content values than those obtained by the oven-dry method. Moisture content was determined quantitatively in soils to which various amounts of water had been added. The complete procedure, including extraction and analysis, requires less than one hour and gives results that closely compare to the oven-dry method.
Merek, E. L.↗
An application of gas chromatography to planetary atmospheres
A gas chromatography developed for the Viking experiment is described. The instrument is designed to measure gases in planetary atmospheres and head space in a chamber. It is hoped that the chromatograph will also measure any biological activity present in these environments.
Oyama, V.↗
Analysis of benzo(a)pyrene in airborne particulates by gas chromatography
A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.
Luedecke, E.↗
Preparation of pure microbiological samples for pyrolysis gas-liquid chromatography studies
Bacterial samples were prepared for pyrolysis gas-liquid chromatography using cells grown on membrane filters. Pyrochromatograms were reproducible when cells harvested from the filters were pyrolyzed without being washed.
Oxborrow, G. S.↗
Hydrocarbon group type determination in jet fuels by high performance liquid chromatography
Thirty-two jet and diesel fuel samples of varying chemical composition and physical properties were prepared from oil shale and coal syncrudes. Hydrocarbon types in these samples were determined by a fluorescent indicator adsorption analysis, and the results from three laboratories are presented and compared. Two methods of rapid high performance liquid chromatography were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.
Antoine, A. C.↗
Hydrocarbon group type determination in jet fuels by high performance liquid chromatography
Results are given for the analysis of some jet and diesel fuel samples which were prepared from oil shale and coal syncrudes. Thirty-two samples of varying chemical composition and physical properties were obtained. Hydrocarbon types in these samples were determined by fluorescent indicator adsorption (FIA) analysis, and the results from three laboratories are presented and compared. Recently, rapid high performance liquid chromatography (HPLC) methods have been proposed for hydrocarbon group type analysis, with some suggestion for their use as a replacement of the FIA technique. Two of these methods were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.
Antoine, A. C.↗
Chelate-modified polymers for atmospheric gas chromatography
Chromatographic materials were developed to serve as the stationary phase of columns used in the separation of atmospheric gases. These materials consist of a crosslinked porous polymer matrix, e.g., a divinylbenzene polymer, into which has been embedded an inorganic complexed ion such as N,N'-ethylene-bis-(acetylacetoniminato)-cobalt (2). Organic nitrogenous bases, such as pyridine, may be incorporated into the chelate polymer complexes to increase their chromatographic utility. With such materials, the process of gas chromatography is greatly simplified, especially in terms of time and quantity of material needed for a gas separation.
Christensen, W. W.↗
Thermal and oxidative degradation studies of formulated C-ethers by gel-permeation chromatography
Gel-permeation chromatography was used to analyze C-ether lubricant formulations from high-temperature bearing tests and from micro-oxidation tests. Three mu-styragel columns (one 500 and two 100 A) and a tetrahydrofuran mobile phase were found to adequately separate the C-ether degradation products. The micro-oxidation tests yielded degradation results qualitatively similar to those observed from the bearing tests. Micro-oxidation tests conducted in air yielded more degradation than did tests in nitrogen. No great differences were observed between the thermal-oxidative stabilities of the two C-ether formulations or between the catalytic degradation activities of silver and M-50 steel. C-ether formulation I did yield more degradation than did formulation II in 111- and 25-hour bearing tests, respectively.
Jones, W. R., Jr.↗
Quantitative separation of tetralin hydroperoxide from its decomposition products by high performance liquid chromatography
A method for the separation and analysis of tetralin hydroperoxide and its decomposition products by high pressure liquid chromatography has been developed. Elution with a single, mixed solvent from a micron-Porasil column was employed. Constant response factors (internal standard method) over large concentration ranges and reproducible retention parameters are reported.
Worstell, J. H.↗
Analysis of a MIL-L-27502 lubricant from a gas-turbine engine test by size-exclusion chromatography
Size exclusion chromatography was used to determine the chemical degradation of MIL-L-27502 oil samples from a gas turbine engine test run at a bulk oil temperature of 216 C. Results revealed a progressive loss of primary ester and additive depletion and the formation of higher molecular weight products with time. The high molecular weight products absorbed strongly in the ultraviolet indicating the presence of chromophoric groups.
Jones, W. R., Jr.↗
Mineral Separation in a CELSS by Ion-exchange Chromatography
Operational parameters pertinent to ion exchange chromatography separation were identified. The experiments were performed with 9 mm diameter ion exchange columns and conventional column accessories. The cation separation beds were packed with AG 50W-X2 strong acid cation exchange resin in H(+) form and 200-400 dry mesh particle size. The stripper beds used in some experiments were packed with AG 1-XB strong base cation exchange resin in OH(-) form and 200-400 dry mesh particle size.
Ballou, E. V.↗
Rapid estimation of concentration of aromatic classes in middistillate fuels by high-performance liquid chromatography
An high performance liquid chromatography (HPLC) method to estimate four aromatic classes in middistillate fuels is presented. Average refractive indices are used in a correlation to obtain the concentrations of each of the aromatic classes from HPLC data. The aromatic class concentrations can be obtained in about 15 min when the concentration of the aromatic group is known. Seven fuels with a wide range of compositions were used to test the method. Relative errors in the concentration of the two major aromatic classes were not over 10 percent. Absolute errors of the minor classes were all less than 0.3 percent. The data show that errors in group-type analyses using sulfuric acid derived standards are greater for fuels containing high concentrations of polycyclic aromatics. Corrections are based on the change in refractive index of the aromatic fraction which can occur when sulfuric acid and the fuel react. These corrections improved both the precision and the accuracy of the group-type results.
Otterson, D. A.↗