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Mass Spectrometry: Pyrolysis
(2019)
Analysis of Synthetic Polymers and Copolymers by Pyrolysis- Gas Chromatography/Mass Spectrometry
(2005)
Structural analysis and the study of degradation properties are important in order to understand and improve performance characteristics of synthetic polymers and copolymers in many industrial applications. Polymers/copolymers are inherently difficult to analyze because of their high molecular weight and lack of volatility. Traditionally, various analytical techniques are used to characterize polymers/copolymers including physical testing (rheological testing), thermogravimetric analysis (TGA), electron microscopy, Fourier transform infrared (FTIR) spectroscopy, size-exclusion chromatography (SEC)/gel permeation chromatography (GPC), and mass spectrometry (MS). Often, time consuming sample preparation, including hydrolysis, dissolution, or derivatization is needed before analysis.
Gas chromatography with flame-ionization detection (FID) and gas chromatography-mass spectrometry (GC/MS) has been used for structure elucidation of long-chain primary n-alkyl amines after derivatization with trifluoroacetic anhydride (TFAA). Electron impact ionization- (EI) and positive chemical ionization- (PCI) mass spectra of trifluoroacetylated derivatives of the identified nalkyl amines are presented. The corrosion inhibiting n-alkyl amines were applied in the investigation of a new anticorrosive and antifouling formulation for water-steam circuit of energy systems in the power industry. The presented results are part of an EU-funded international collaboration with partners from research institutes and industry from Poland, Lithuania, Romania, France and Germany (EUREKA project BOILTREAT E!2426).
Gas chromatography with simultaneous flame-ionization detection (FID) and a nitrogen-phosphorus detection (NPD) as well as gas chromatography-mass spectrometry (GC/MS) has been used to characterize some long-chain primary alkyl amines and alkyl diamines after derivatization with trifluoroacetic anhydride (TFAA).
Gas chromatography with flame-ionization detection (FID) and gas chromatography-mass spectrometry (GC/MS) with electron impact ionization (EI) and chemical ionization (PCI and NCI) were successfully used for separation and identification of commercially available longchain primary alkyl amines. The investigated compounds were used as corrosion inhibiting and antifouling agents in a water-steam circuit of energy systems in the power industry. Solidphase extraction (SPE) with octadecyl bonded silica (C18) sorbents followed by gas chromatography were used for quantification of the investigated Primene JM-T™ alkyl amines in boiler water, condensate and superheated steam samples from the power plant. Amine formulations from Kotamina group favor formation of protective layers on internal surfaces and keep them free from corrosion and scale. Alkyl amines contained in those formulations both render the environment alkaline and limit the corrosion impact of ionic and gaseous impurities by formation of protective layers. Moreover, alkyl amines limit scaling on heating surfaces of boilers and in turbine, ensuring failure-free operation. Application of alkyl amine formulation enhances heat exchange during boiling and condensation processes. Alkyl amines with branched structure are more thermally stable than linear alkyl amines, exhibit better adsorption and effectiveness of surface shielding. As a result, application of thermostable long-chain branched alkyl amines increases the efficiency of anti-corrosive protection. Moreover, the concentration of ammonia content in water and in steam was also considerably decreased.
This book chapter describes application examples of gas chromatography/mass spectrometry and pyrolysis – gas chromatography/mass spectrometry in failure analysis for the identification of chemical materials like mineral oils and nitrile rubber gaskets. Furthermore, failure cases demanding identification of polymers/copolymers in fouling on the compressor wall of a car air conditioner and identification of fouling on the surface of a bearing race from the automotive industry are demonstrated. The obtained analytical results were then used for troubleshooting and remedial action of the technological process.
Solid-Phase Microextraction (SPME) is a very simple and efficient, solventless sample preparation method, invented by Pawliszyn and coworkers at the University of Waterloo (Canada) in 1989. This method has been widely used in different fields of analytical chemistry since its first applications to environmental and food analysis. SPME integrates sampling, extraction, concentration and sample introduction into a single solvent-free step. The method saves preparation time, disposal costs and can improve detection limits. It has been routinely used in combination with gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS) and successfully applied to a wide variety of ompounds, especially for the extraction of volatile and semi-volatile organic compounds from environmental, biological and food samples.
Since the last twenty years, SPME in headspace (HS) mode is used as a valuable sample preparation technique for identifying degradation products in polymers and for determination of rest monomers and other light-boiling substances in polymeric materials. For more than ten years, our laboratory has been involved in projects focused on the application of HS-SPME-GC/MS for the characterization of polymeric materials from many branches of manufacturing and building industries. This book chapter describes the application examples of this technique for identifying volatile organic compounds (VOCs), additives and degradation products in industrial plastics, rubber, and packaging materials.
According to the International Union of Pure and Applied Chemistry (IUPAC) recommendation, analytical pyrolysis (Py) is defined as the characterization in an inert atmosphere of a material or a chemical process by a chemical degradation reaction(s) induced by thermal energy [1]. Thermal degradation under controlled conditions is often used as a part of an analytical procedure, either to render a sample into a suitable form for subsequent analysis by gas chromatography (GC), mass spectrometry (MS), gas chromatography coupled with the mass spectrometry (GC/MS), with the Fourier-transform infrared spectroscopy (GC/FTIR), or by direct monitoring as an analytical technique in its own right [2].
Gas chromatography (GC) is a type of chromatography. According to the International Union of Pure and Applied Chemistry (IUPAC) recommendation, gas chromatography is defined as a separation technique in which the mobile phase is a gas. Gas chromatography is always carried out in a column [1]. GC is a separation and detection method for sample mixtures, whose components can be volatilized without thermal decomposition.
A method for the identification of polymeric residues in recycled aluminium by using analytical pyrolysis at 700°C hyphenated to gas chromatography-mass spectrometry (Py-GC/MS) was presented for the first time. The polymeric residues in recycled aluminium were identified as a mixture of polyethylene, polystyrene, and phenolic resin. The described method could be useful for the aluminium industry as a part of the quality control of the recycled aluminium production.