Analysis of carboxylic esters using alkali fusion reaction gas chromatography

Frankoski, Stanley P.; Siggia, Sidney.

doi:10.1021/ac60311a052

Cited by 44 publications

(8 citation statements)

References 18 publications

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“…The thermocouple well in the cup served to support the pan on a central quartz spindle. Samples of rubber or gum, about 8 mg, were carefully weighed into the platinum pan and covered with 20 rng potassium hydroxide containing 1% sodium acetate freshly prepared according to the technique of Frankoski and Siggia [18]. Fresh preparations of this material are essential.…”

Section: Alkaline Pyrolysismentioning

confidence: 99%

Analysis and structure of dicumyl peroxide ultraviolet‐cured poly(dimethyl siloxane) rubber crosslinks

Barrall

Hawkins

Fukushima

et al. 1984

J. polym. sci., C Polym. symp.

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The alkaline fusion method for the analysis of the hydrocarbon portion of poly(dimethyl siloxane) gum stock containing pendant vinyl groups has been applied to systems crosslinked with dicumyl peroxide in the presence of near‐UV radiation. Crosslinks made of butyl and propyl chains both with and without aromatic residues were found. Under the conditions of this study the dicumyl peroxide efficiency as a crosslinking agent is slightly greater than one. Owing to the formation of three carbon‐containing crosslinks, the total chemical crosslink density of the system was greater than predicted from simple vinyl‐to‐vinyl addition.

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Section: Alkaline Pyrolysismentioning

confidence: 99%

Analysis and structure of dicumyl peroxide ultraviolet‐cured poly(dimethyl siloxane) rubber crosslinks

Barrall

Hawkins

Fukushima

et al. 1984

J. polym. sci., C Polym. symp.

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“…The procedure for its prep- 1 Present address, Biochemicals Department, E. I. du Pont de Nemours & Co., Inc., Wilmington, Del. 19898. aration has been described in detail elsewhere (30). Typically, the mixture melts around 110 °C.…”

mentioning

confidence: 99%

“…The exposed piece of tubing, which is loosely packed with quartz wool, is cooled in a liquid nitrogen-filled Dewar flask when concentrating the evolved products and heated with a 400 °C nichrome wire heater (30) when "injecting" the products into the gas chromatograph. Helium carrier gas flows (60 mL/min) through the reaction unit and cold trap before entering the chromatographic column.…”

mentioning

confidence: 99%

Analysis of polysiloxanes by alkali fusion reaction gas chromatography

Schlueter¹,

Siggia²

1977

Anal. Chem.

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The technique of alkali fusion reaction gas chromatography has been applied to the determination of alkyl and aryl groups in polysiloxanes. The method involves the quantitative cleavage of ail organic substituents bonded to silicon, producing the corresponding hydrocarbons. Reactions are driven to completion, with no apparent decomposition, in less than 10 minutes by fusing the sample with potassium hydroxide in an Inert atmosphere. After concentration of the volatile products, they are separated and determined by gas chromatography. Sample losses are minimized by performing the total analysis in a single piece of apparatus. Fluids, gum rubbers, and resins are handled with equal ease. The percent relative standard deviation of the method is 1.0%; the average deviation between experimental and theoretical or check method results Is 0.5% absolute.Polysiloxanes, also referred t o as silicones or polyorganosiloxanes, are commercially important because of unique properties resulting from their dual organic-inorganic composition. The analytical chemistry of this class of polymers has been reviewed in a recent monograph by Smith ( I ) .Spectrometric techniques, such as IR and NMR, are powerful tools for the qualitative and quantitative analysis of many functional groups in t h e intact polymer. Alternatively, these organic substituents can be cleaved from the polymer to produce simple compounds that can b e determined by chemical or instrumental techniques.Alkyl and aryl substituents are readily detected by t h e above approaches, b u t quantitative analyses of these groups may be difficult with existing methodology. Instrumental techniques such as N M R (2, 3 ) , IR (4-13), and UV (14-17) spectrometry are useful for analyzing methyl and/or phenyl groups in silicone polymers, but they are generally unable t o differentiate isomers or homologues. Chemical cleavage coupled with a separation technique is a more selective approach. Several reaction-based methods have been reported for t h e quantitative determination of alkyl and aryl groups

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“…EXPERIMENTAL Fusion Reagent. The preparation and storage of the alkali fusion reagent have been described in detail elsewhere (44,45).…”

mentioning

confidence: 99%

Determination of Imides, Aromatic, Polyimides, Polyamides, and Poly (Amide-Imides) by Alkali Fusion Reaction Gas Chromatography

Schlueter¹,

Siggia²

1977

Anal. Chem.

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Analysis of carboxylic esters using alkali fusion reaction gas chromatography

Cited by 44 publications

References 18 publications

Analysis and structure of dicumyl peroxide ultraviolet‐cured poly(dimethyl siloxane) rubber crosslinks

Analysis and structure of dicumyl peroxide ultraviolet‐cured poly(dimethyl siloxane) rubber crosslinks

Analysis of polysiloxanes by alkali fusion reaction gas chromatography

Determination of Imides, Aromatic, Polyimides, Polyamides, and Poly (Amide-Imides) by Alkali Fusion Reaction Gas Chromatography

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