Identification of polyhydric alcohols in synthetic resins by programmed temperature gas chromatography

CONCLUSIONData presented show that the two-diameter column gives enhanced resolution of normally difficult separations for typical preparative and trace analyses. The two-diameter technique can be used for large samples without significantly increasing the time of analysis for both gases and liquids.This method may be applied to a combination gas chromatograph connected in series to a mass spectrometer. Frequently a trace component is too small to be identified by the mass spectrometer. The two-diameter column allows a much larger sample to be introduced into the gas chromatograph for a separation, without column overloading, and allows a satisfactory determination by the mass spectrometer. ACKNOWLEDGMENTThe author gratefully acknowledges the technical assistance of T. C. Harby in preparing the column used in these experiments.

Section: Acknowledgmentmentioning

confidence: 60%

Section: Acknowledgmentmentioning

confidence: 99%

See 1 more Smart Citation

Gas chromatographic determination of diethylene glycol in poly(ethylene terephthalate)

Ponder¹

1968

“…An examination of the literature revealed that only a few of these compounds had been identified and reported. Consequently, a synthesis of these isomers (there are a total of six isomers) was begun by an established procedure using potassium chlorate (2) and the commercially available 3-chloro-, 4-chloro-, 5-chloro-, and 6-chloro-2-methylanilines. As was soon discovered, these dichlorinated derivatives were exceedingly difficult to purify and identify for two reasons: isomer contamination and/or low melting points.…”

Section: Literature Citedmentioning

confidence: 99%

Quantitative hydrolysis-gas chromatographic methods for the determination of selected acids and glycols in polyesters

Allen¹,

Elsea²,

Keller³

et al. 1977

The objective of this work was to develop precise quantitative methods of analysis for determining repeat units of polyesters. These methods have In common an alkaline hydrolysis of polyesters followed by gas chromatographic determination of the glycols and acids produced from the hydrolyses. In order to obtain rapid chromatographic analyses, trimethylsllyl derivatives of the glycols and acids were formed by a reaction with /V,0-bis(trlmethylsllyl)trifluoracetamlde. The relative standard deviation varies from 0.8 % for the determination of 1,4-butanedlol to approximately 2% for 1,4-cyclohexanedlmethanol. For the determination of different concentrations of Isophthalic acid, the standard deviation varies from 0.7 to 2.4%. These methods provide rapid and precise determinations for selected acids and glycols In polyesters.Several methods have been described for determining the diethylene glycol content of poly(ethylene terephthalate) (PET) (1-3). These methods have in common the decomposition of the polyester through alkaline hydrolysis or hydrazinolysis followed by the determination of the diethylene glycol content by titration or gas chromatographic methods (4-8). However, none of these methods describe the quantitative determination of other glycol or acid content of polyesters. The objective of this work was to develop a precise, accurate method to determine the glycols and methyl ester end groups in PET and to develop a method for general use in determining glycols and acids in polyesters.

“…Reduction to a phenolic alcohol and analysis as an oxygenated compound (3,6,7,9,19) were also considered, but the manipulations were too involved for a good routine method; chlorination, bromination, or iodination were no improvement (10, SO). Other investigators converted fatty acids to methyl esters (6,12) to aid their movement on the gas chromatograph; still others converted barbiturates and acidic drugs to methyl esters (4, 23); or analyzed mono-and di-carboxylic acids in resinous substances as methyl ester (16,17); determined cyclic (14). phthalic (8,22), benzoic acids (9, 30), and mixtures of ethers of aromatic acids (18) as esters.…”

mentioning

confidence: 99%

Determination of Aspirin by Gas Chromatography.

Crippen¹,

Freimuth²

1964