Solvent gas chromatography

The crude material also contains some pol)oneric material and traces of solvent. Gas chromatography indicates that the phenyl /-butyl ether is 60-70% pure at this point. 

Several techniques are used to determine purity of solvents. Gas chromatography is the most common and tins and other methods are discussed first followed by oflier analytical methods which include instrumental and simple methods. The aim of these tests is to determine flie concentration of flie main component but more frequently qualitative and quantitative determination of admixtures. Some mefliods have already been discussed in Sections 15.1.1,15.1.5,15.1.8,15.1.9,15.1.18,15.1.20 and 15.1.23. 

Some techniques have been described that are based on the concept of flame ionization used in gas chromatography. The results are generally unsatisfactory because it is necessary to evaporate the solvent prior to introducing the mixture into the detector. 

Instmmental methods of analysis provide information about the specific composition and purity of the amines. QuaUtative information about the identity of the product (functional groups present) and quantitative analysis (amount of various components such as nitrile, amide, acid, and deterruination of unsaturation) can be obtained by infrared analysis. Gas chromatography (gc), with a Hquid phase of either Apiezon grease or Carbowax, and high performance Hquid chromatography (hplc), using siHca columns and solvent systems such as isooctane, methyl tert-huty ether, tetrahydrofuran, and methanol, are used for quantitative analysis of fatty amine mixtures. Nuclear magnetic resonance spectroscopy (nmr), both proton ( H) and carbon-13 ( C), which can be used for quaHtative and quantitative analysis, is an important method used to analyze fatty amines (8,81). 

Analytical Techniques. Sorbic acid and potassium sorbate are assayed titrimetricaHy (51). The quantitative analysis of sorbic acid in food or beverages, which may require solvent extraction or steam distillation (52,53), employs various techniques. The two classical methods are both spectrophotometric (54—56). In the ultraviolet method, the prepared sample is acidified and the sorbic acid is measured at 250 260 nm. In the colorimetric method, the sorbic acid in the prepared sample is oxidized and then reacts with thiobarbituric acid the complex is measured at - 530 nm. Chromatographic techniques are also used for the analysis of sorbic acid. High pressure Hquid chromatography with ultraviolet detection is used to separate and quantify sorbic acid from other ultraviolet-absorbing species (57—59). Sorbic acid in food extracts is deterrnined by gas chromatography with flame ionization detection (60—62). 

The acetyl content of cellulose acetate may be calculated by difference from the hydroxyl content, which is usually determined by carbanilation of the ester hydroxy groups in pyridine solvent with phenyl isocyanate [103-71-9J, followed by measurement of uv absorption of the combined carbanilate. Methods for determining cellulose ester hydroxyl content by near-infrared spectroscopy (111) and acid content by nmr spectroscopy (112) and pyrolysis gas chromatography (113) have been reported. 

Polymerization-grade chloroprene is typically at least 99.5% pure, excluding inert solvents that may be present. It must be substantially free of peroxides, polymer [9010-98-4], and inhibitors. A low, controlled concentration of inhibitor is sometimes specified. It must also be free of impurities that are acidic or that will generate additional acidity during emulsion polymerization. Typical impurities are 1-chlorobutadiene [627-22-5] and traces of chlorobutenes (from dehydrochlorination of dichlorobutanes produced from butenes in butadiene [106-99-0]), 3,4-dichlorobutene [760-23-6], and dimers of both chloroprene and butadiene. Gas chromatography is used for analysis of volatile impurities. Dissolved polymer can be detected by turbidity after precipitation with alcohol or determined gravimetrically. Inhibitors and dimers can interfere with quantitative determination of polymer either by precipitation or evaporation if significant amounts are present. 

GAS CHROMATOGRAPHY DETERMINATION FOR SMALL QUANTITIES OF WATER IN ORGANIC SOLVENTS... 

Determination of water of different materials is one of the important tasks of the analytical chemistry. For water determination in organic solvents physical-chemical methods use side by side with the classic titration method by Karl Fisher. In particular, gas chromatography (GC), distinguished its universality and selectivity, is used. However, GC usually used for determination of relatively large quantity of water. 

Charcoal adsorbent tubes with solvent desorption and gas chromatography... 

Chlorinated hydrocarbon solvent vapours in air Lab method using pumped charcoal adsorption tubes, solvent desorption and gas chromatography 28... 

Ethylene dibromide Lab method with pumped Tenax absorbent tubes, solvent desorption and electron capture gas chromatography 45... 

Lab method using charcoal diffusive samplers, solvent desorption and gas chromatography (using Drager ORSA monitor) 64... 

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