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For the last 20 years, solid-phase microextraction (SPME) in headspace (HS) mode has been used as a valuable sample preparation technique for identifying degradation products in polymers and the determination of residual monomers and other light-boiling substances in polymeric materials. For more than 10 years, our laboratory has been involved in projects focused on the application of HS-SPME-gas chromatography–mass spectrometry (GC–MS) for the characterization of polymeric materials from many branches of manufacturing and building industries. This article describes the application of this technique for identifying volatile organic compounds (VOCs), additives, and degradation products in industrial rubber, car labeling reflection foil, and bone cement materials. The obtained analytical results were then used for troubleshooting and remedial action of the technological processes as well as for the health protection of producers and users.
Mass Spectrometry: Pyrolysis
(2019)
The criteria for assessing the quality of rubber materials are the polymer or copolymer composition and the additives. These additives include plasticizers, extender oils, carbon black, inorganic fillers, antioxidants, heat and light stabilizers, processing aids, cross-linking agents, accelerators, retarders, adhesives, pigments, smoke and flame retardants, and others. Determination of additives in polymers or copolymers generally requires the extraction of these substances from the matrix as a first step, which can be challenging, and the subsequent analysis of the extracted additives by gas chromatography (GC), GC-mass spectrometry (MS), high performance liquid chromatography (HPLC), HPLC-MS, capillary electrophoresis, thin-layer chromatography, and other analytical techniques. In the present work, nitrile rubber materials were studied using direct analytical flash pyrolysis hyphenated to GC and electrospray ionization MS in both scan and selected ion monitoring modes to demonstrate that this technique is a good tool to identify the organic additives in nitrile rubber.
The criteria for assessing the quality of rubber materials are the polymer or copolymer composition and the additives. These additives include plasticizers, extender oils, carbon black, inorganic fillers, antioxidants, heat and light stabilizers, processing aids, cross-linking agents, accelerators, retarders, adhesives, pigments, smoke and flame retardants, and others. Determination of additives in polymers or copolymers generally requires the extraction of these substances from the matrix as a first step, which can be challenging, and the subsequent analysis of the extracted additives by gas chromatography (GC), GC–mass spectrometry (MS), high performance liquid chromatography (HPLC), HPLC–MS, capillary electrophoresis, thin-layer chromatography, and other analytical techniques. In the present work, nitrile rubber materials were studied using direct analytical flash pyrolysis hyphenated to GC and electrospray ionization MS in both scan and selected ion monitoring modes to demonstrate that this technique is a good tool to identify the organic additives in nitrile rubber.
Pyrolysis–Gas Chromatography
(2018)
The methodology of analytical pyrolysis-GC/MS has been known for several years, but is seldom used in research laboratories and process control in the chemical industry. This is due to the relative difficulty of interpreting the identified pyrolysis products as well as the variety of them. This book contains full identification of several classes of polymers/copolymers and biopolymers that can be very helpful to the user. In addition, the practical applications can encourage analytical chemists and engineers to use the techniques explored in this volume.
The structure and the functions of various types of pyrolyzers and the results of the pyrolysis–gas chromatographic–mass spectrometric identification of synthetic polymers/copolymers and biopolymers at 700°C are described. Practical applications of these techniques are also included, detailing the analysis of microplastics, failure analysis in the automotive industry and solutions for technological problems.
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.
Headspace-SPME-GC-MS identification of volatile organic compounds released from expanded polystyrene
(2004)
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).
Die analytische Pyrolyse ist eine universell einsetzbare Messtechnik zur Untersuchung von hoch molekularen organischen Verbindungen. Bei der Pyrolyse der hochmolekularen organischen Ver bindungen entstehen durch thermische Zersetzung bei 500-1400°C in einem Inertgasstrom nieder molekulare Verbindungen. Diese niedermolekularen Pyrolyse-Produkte werden dann den her kömmlichen Analyseverfahren wie GC-FID, GC/MS oder GC/FTIR unterworfen, die Rück schlüsse auf chemische Zusammensetzung und Struktur der Ausgangsstoffe erlauben. Die Festphasen mikroextraktion (SPME) ist eine lösungsmittelfreie Mikroextraktionstechnik. Im Headspace-Modus (HS) wurde SPME in den letzten Jahren für die Bestimmung von Rest mono meren und gesund heits gefährdenden, leichtflüchtigen organischen Verbindungen (VOCs) in Kunststoffen verwendet.
Der zunehmende Einsatz der Polymerwerkstoffe in der Automobilindustrie erfordert empfindliche und zuverlässige Methoden zur Analyse der verwendeten Stoffe. Bei Schadenanalysen an Komponenten in Kraftfahrzeugen stehen oftmals nur wenige Informationen über das Bauteil selbst, wie die chemische Zusammensetzung, die Temperaturbeständigkeit, mögliche Kontaminierungs stoffe oder mechanische Eigenschaften zur Verfügung. Der Schadensbereich ist meistens be grenzt und nicht immer homogen. Zur Klärung des Schadens stehen häufig nur kleine Proben mengen zur Verfügung, die jedoch für die Erkennung der Schadensursache von großer Bedeutung sein können.