Determination of polymer additives using analytical pyrolysis

Jansson, Karen D.; Zawodny, Charles; Wampler, Thomas P.

doi:10.1016/j.jaap.2006.12.009

Cited by 47 publications

(34 citation statements)

References 5 publications

(5 reference statements)

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“…More recent publications underline that a temperature program should be applied during pyrolysis. This increases the analysis time, but significantly reduces the interference of different substances [33]. This approach has to be considered (at least for lower temperature steps) as TDS with all its associated challenges in quantification.…”

Section: Direct Methods For the Analysis Of Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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Polymeric materials are complex samples, as they contain various groups of additives, compounding ingredients, and fillers. An important group of additives are stabilizers. Efficient stabilization is essential especially for polypropylene, as it is sensitive to oxidation and radical attack due to the numerous tertiary carbon atoms in its structure. How long a polymer will be sufficiently stabilized can be deduced from the contained amount of intact stabilizer. Different approaches for the analysis of stabilizers in polyolefins are available, which include sample preparation with subsequent chromatographic separation as well as direct analysis techniques. In round-robin tests, stabilizer concentrations obtained varied strongly. This shows the demand for reliable and robust methods. Stabilizers get consumed while protecting the polymer and are then present as degradation products. They were observed while quantifying intact stabilizers, in migration studies, and - if volatile - in emission studies of polymers. Furthermore, e.g. interactions with other polymer ingredients or irradiation degraded stabilizers. The identification of degradation products provides a better insight into the reactions associated with stabilization. Their quantitation makes it possible to deduce the original level of stabilization. Furthermore, polymer ingredients degrading stabilizers can be identified. Knowledge on these interactions contributes significantly to improved polymer stabilization.

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Section: Direct Methods For the Analysis Of Stabilizersmentioning

confidence: 99%

Analysis of polyolefin stabilizers and their degradation products

Reingruber

Buchberger

2010

J of Separation Science

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“…One such method is pyrolysis-GC/MS, in which a piece of sample is heated to a high temperature under inert gas atmosphere and volatile components together with pyrolysis fragments of larger molecules are separated and identified with a GC/MS system [4][5][6]. As already mentioned, most of the additives used today have a high molecular weight and are not volatile.…”

Section: Introductionmentioning

confidence: 99%

Quantitative Analysis of Polymer Additives with MALDI-TOF MS Using an Internal Standard Approach

Schwarzinger

Gabriel

Beißmann

et al. 2012

J. Am. Soc. Mass Spectrom.

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MALDI-TOF MS is used for the qualitative analysis of seven different polymer additives directly from the polymer without tedious sample pretreatment. Additionally, by using a solid sample preparation technique, which avoids the concentration gradient problems known to occur with dried droplets and by adding tetraphenylporphyrine as an internal standard to the matrix, it is possible to perform quantitative analysis of additives directly from the polymer sample.

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“…Several studies have been published about polymer and additive analysis using the pyrolysis technique [5][6][7][8][9][10] . Typically, the analytical techniques used to identify the fragments from pyrolysis are gas chromatography (GC) and mass spectrometry (MS).…”

mentioning

confidence: 99%

Characterization of Additives Typically Employed in EPDM Formulations by using FT-IR of Gaseous Pyrolyzates

Sanches¹,

Cassu²,

Diniz³

et al. 2014

Polímeros

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Abstract:In this study, Fourier transform infrared spectroscopy (FT-IR) was employed to investigate the gaseous pyrolysis products of ethylene-propylene-diene rubber (EPDM). The objective was to evaluate the potential of FT-IR analysis of gaseous pyrolyzates (PY-G/FT-IR) for characterization of EPDM additives. Two EPDM formulations, containing additives typically employed in EPDM rubbers, were analyzed. Initially, gaseous pyrolysis products from paraffin oil, stearic acid, 2,2,4-trimethyl-1,2-dihydroquinoline, tetramethylthiuram monosulfide (TMTM), tetramethylthiuram disulfide (TMTD), and 2-mercaptobenzothiazole (MBT) were characterized separately, and their main absorptions were identified. Subsequently, the gaseous pyrolysis products of raw, unvulcanized, and vulcanized EPDM formulations were analyzed. The similarities observed in the FT-IR spectra of unvulcanized and vulcanized EPDM show that the vulcanization process does not interfere with the pyrolysis products. The identification of the functional groups of the studied additives was possible in both unvulcanized and vulcanized EPDM samples, without solvent extraction. Results also demonstrate that the PY-G/FT-IR technique can identify additives containing sulfur in concentrations as low as 1.4 phr (1.26%) in both unvulcanized and vulcanized EPDM. However, the method showed some limitation due to overlapping and to similarities of TMTM and TMTD PY-G/FT-IR spectra, which could not be distinguished from each other. The PY-G/FT-IR technique is a faster and cheaper alternative to the sophisticated techniques usually applied to detection of additives in rubbers.

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Determination of polymer additives using analytical pyrolysis

Cited by 47 publications

References 5 publications

Analysis of polyolefin stabilizers and their degradation products

Analysis of polyolefin stabilizers and their degradation products

Quantitative Analysis of Polymer Additives with MALDI-TOF MS Using an Internal Standard Approach

Characterization of Additives Typically Employed in EPDM Formulations by using FT-IR of Gaseous Pyrolyzates

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