Determination of glycolic ether linkages in poly(ethylene terephthalate)

Gaskill, David R.; Chasar, Andrew G.; Lucchesi, Claude A.

doi:10.1021/ac60245a005

Cited by 20 publications

(5 citation statements)

References 3 publications

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“…During synthesis of PET, diethylene glycol (DEG) is produced as a byproduct, due to the undesirable dimerization of ethylene glycol. 14,15 Considerable effort is aimed at reducing the amount of DEG, because once produced and incorporated in the polymer chain, it adversely affects the T g , crystallinity, and melting behavior of PET. Because the formation of DEG is acid catalyzed, it is produced during the initial esterification reaction rather than during polyesterification.…”

Section: Synthesis Of High-performance Polyester Containing 44-biphementioning

confidence: 99%

Synthesis and properties of 4,4?-biphenyldicarboxylic acid and 2,6-naphthalenedicarboxylic acid

Asrar

1999

J. Polym. Sci. A Polym. Chem.

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This article describes the synthesis and the properties of polyesters and copolyesters prepared from ethylene glycol, terephthalic acid, 4,4′ biphenyldicarboxylic acid (BDA), and 2,6‐naphthlenedicarboxylic acid (NDA). The effect of incorporating varying levels of BDA and NDA on polyethylene terephthalate (PET) is described. Depending on the concentration, incorporation of BDA into PET leads to an improvement in glass transition temperature (Tg), strength, modulus, and barrier properties. Copolymers of PET containing up to about 50% BDA derived units are clear and have Tg's ranging from 85 to 105°C, making them suitable for applications where a high Tg along with clarity is important. Copolymers with higher BDA concentration are highly crystalline, with high rates of crystallization from the melt. Copolymerization of NDA with oligoethyleneterephthalate leads to copolymers that are generally amorphous. Crystallinity can be developed in copolymers with low concentration of NDA by thermal annealing. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3139–3146, 1999

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Section: Synthesis Of High-performance Polyester Containing 44-biphementioning

confidence: 99%

Synthesis and properties of 4,4?-biphenyldicarboxylic acid and 2,6-naphthalenedicarboxylic acid

Asrar

1999

J. Polym. Sci. A Polym. Chem.

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“…Once the pyridine-4-aldehyde is formed, it is easily analyzed via reaction with 3-methyl-2-benzothiazolinone hydrozone (MBTH) (1). With this modified procedure, the molar absorptivity for hydrogen peroxide is 36,500, which is somewhat higher than the molar absorptivities obtained with other methods available for the analysis of hydrogen peroxide (3,4).…”

Section: Acknowledgmentmentioning

confidence: 61%

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

Ponder¹

1968

Anal. Chem.

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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.

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“…There have been numerous studies reported in the literature where isomer identification and distribution have been accomplished by gas chromatographic techniques. However, in the majority of these studies, product identification was made possible by comparing their retention times with known compounds, i.e., the analysis of isomeric diaminotoluenes with the IV-trifluoroacetyl derivatives (3), the separation of mono and dichloroaniline isomers (4), the identification of isomeric toluidines (5) and the separation and identification of seven chlorinated derivatives of toluene (6).…”

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

Anal. Chem.

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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.

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Determination of glycolic ether linkages in poly(ethylene terephthalate)

Cited by 20 publications

References 3 publications

Synthesis and properties of 4,4?-biphenyldicarboxylic acid and 2,6-naphthalenedicarboxylic acid

Synthesis and properties of 4,4?-biphenyldicarboxylic acid and 2,6-naphthalenedicarboxylic acid

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

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

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