Separation by gas chromatography

DichIoro-l,3-butadiene [1653-19-6] M 123.0, b 41-43 /85mm, 98 /760mm. Crystd from pentane to constant melting point about -40°. A mixture of meso and d,l forms was separated by gas chromatography on an 8m stainless steel column (8mm i.d.) with 20% DECS (diethyleneglycolsilyl chloride) on Chromosorb W (60-80 mesh) at 60° and 80mL He/min. [Su and Ache J Phys Chem 80 659 1976.]... 

High performance liquid chromatography is used for the separation and quantitative analysis of a wide variety of mixtures, especially those in which the components are insufficiently volatile and/or thermally stable to be separated by gas chromatography. This is illustrated by the following method which may be used for the quantitative determination of aspirin and caffeine in the common analgesic tablets, using phenacetin as internal standard where APC tablets are available the phenacetin can also be determined by this procedure. 

The combination of chromatography and mass spectrometry (MS) is a subject that has attracted much interest over the last forty years or so. The combination of gas chromatography (GC) with mass spectrometry (GC-MS) was first reported in 1958 and made available commercially in 1967. Since then, it has become increasingly utilized and is probably the most widely used hyphenated or tandem technique, as such combinations are often known. The acceptance of GC-MS as a routine technique has in no small part been due to the fact that interfaces have been available for both packed and capillary columns which allow the vast majority of compounds amenable to separation by gas chromatography to be transferred efficiently to the mass spectrometer. Compounds amenable to analysis by GC need to be both volatile, at the temperatures used to achieve separation, and thermally stable, i.e. the same requirements needed to produce mass spectra from an analyte using either electron (El) or chemical ionization (Cl) (see Chapter 3). In simple terms, therefore, virtually all compounds that pass through a GC column can be ionized and the full analytical capabilities of the mass spectrometer utilized. 

Several methods are available for the analysis of trichloroethylene in biological media. The method of choice depends on the nature of the sample matrix cost of analysis required precision, accuracy, and detection limit and turnaround time of the method. The main analytical method used to analyze for the presence of trichloroethylene and its metabolites, trichloroethanol and TCA, in biological samples is separation by gas chromatography (GC) combined with detection by mass spectrometry (MS) or electron capture detection (ECD). Trichloroethylene and/or its metabolites have been detected in exhaled air, blood, urine, breast milk, and tissues. Details on sample preparation, analytical method, and sensitivity and accuracy of selected methods are provided in Table 6-1. 

Reliable analytical methods are available for determination of many volatile nitrosamines at concentrations of 0.1 to 10 ppb in a variety of environmental and biological samples. Most methods employ distillation, extraction, an optional cleanup step, concentration, and final separation by gas chromatography (GC). Use of the highly specific Thermal Energy Analyzer (TEA) as a GC detector affords simplification of sample handling and cleanup without sacrifice of selectivity or sensitivity. Mass spectrometry (MS) is usually employed to confirm the identity of nitrosamines. Utilization of the mass spectrometer s capability to provide quantitative data affords additional confirmatory evidence and quantitative confirmation should be a required criterion of environmental sample analysis. Artifactual formation of nitrosamines continues to be a problem, especially at low levels (0.1 to 1 ppb), and precautions must be taken, such as addition of sulfamic acid or other nitrosation inhibitors. The efficacy of measures for prevention of artifactual nitrosamine formation should be evaluated in each type of sample examined. 

Characterization of various types of damage to DNA by oxygen-derived species can be achieved by the technique of gas chromatography-mass spectrometry (GC-MS), which may be applied to DNA itself or to DNA-protein complexes such as chromatin (Dizdaroglu, 1991). For GC-MS, the DNA or chromatin is hydrolysed (usually by heating with formic acid) and the products are converted to volatile derivatives, which are separated by gas chromatography and conclusively identified by the structural evidence provided by a mass spectrometer. Stable isotope-labelled bases may be used as internal standards... 

An important application of carbon-skeleton gas chromatography is the simplification of the analysis of complex samples such as polychlorinated biphenyls, polybrominated biphenyls and polychloroalkanes [709-711], These complex mixtures of halogenated isomers produce multiple peaks when separated by gas chromatography, making quantitation difficult. The isomers have identical carbon skeletons, resulting in a very simple chromatogram after hydrodechlorination. 

Isotopes of hydrogen. Three isotopes of hydrogen are known H, 2H (deuterium or D), 3H (tritium or T). Isotope effects are greater for hydrogen than for any other elements (and this may by a justification for the different names), but practically the chemical properties of H, D and T are nearly identical except in matters such as rates and equilibrium constants of reactions (see Tables 5.1a and 5.1b). Molecular H2 and D2 have two forms, ortho and para forms in which the nuclear spins are aligned or opposed, respectively. This results in very slight differences in bulk physical properties the two forms can be separated by gas chromatography. 

Bruhin and Jenny 72) recently prepared the [2.2] (2,5)pyridinophanes 50a—50d by Hofmann elimination the compounds were separated by gas chromatography. Their 1H—NMR spectra provide clear structural... 

The extension of the ideas presented in Sections 5.8 and 5.10 to the theoretical treatment of isotope separation by gas chromatography is straightforward. The isotope effects observed in chromatography are governed by the isotopic ratio of Henry s Law constants (for gas-liquid separations), or adsorption constants (for... 

This particular demonstration module only incorporates decisions involving analysis of volatile and semivolatile organic compounds from water. These compounds are, by definition, volatile enough to be separated by gas chromatography (GC). The complete expert system will incorporate decisions based upon any type of chemical in any type of matrix and will also be capable of providing advice specifically for selected EPA methods commonly in use, i.e., EPA Methods 624, 625, 1624, 1625, the various non-mass spectrometric 600 Methods, etc. (Figure 1). 

Since the compound(s) you are analyzing are sufficiently volatile to be separated by gas chromatography, I am assuming that you will use a GC for your separations. Here are the detector choices we have to consider a = Mass spectrometer (general purpose)... 

In modern combustion analysers, a tiny sample (about 2 mg) is accurately weighed and oxidised at a high temperature in an oxygen atmosphere. The product mixture of CO, HjO, Nj and SO is separated by gas chromatography and the mass of each component is measured using a thermal conductivity detector. From these product masses, the mass of each of the elements C, H, N and S in the sample can... 

Spectra of these tautomers were obtained on samples separated by gas chromatography from thioketo-thioenol mixtures. Trithioacetone pyrolysate was passed through a DC 200 silicone oil on Gas Chrom Z packed column. As the appropriate sample eluted from the column, it was condensed on a sodium chloride plate cooled to —100° C and its spectrum immediately determined. The very low temperature employed prevented loss of thioenol by tautomerization and of thioketo by polymerization. 

An earlier paper on the thermal cyclodimerization of 3 (R1 = F R2 = Ph) also reported the formation of a cis/trans mixture which was separated by gas chromatography.3 This structure contradicted an earlier assignment of the head-to-tail structure for this dimer.4... 

Gas-liquid chromatographic analysis with a 1 S-m 5% SE-30 column at 13S° b Could not be separated by gas chromatography... 

The analysis of essential fatty acids involves hydrolysis of the ester bonds and subsequent formation of the fatty acid methyl esters, which can be separated by gas chromatography (GC) [10]. By accident, the plasmalogens are hydrolysed in the same reaction and the methylation reaction transforms them into dimethylacetals, which appear in the GC run of the fatty acid methyl esters [4]. 

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