Bonn-Rhine-Sieg University of Applied Sciences, Department of Applied Natural Sciences, von-liebig-str. 20, D Rheinbach, Germany,

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1 Application of pyrolysis-gas chromatography/mass spectrometry for the identification of polymeric materials in failure analysis in the automotive industry P. Kusch* 1, V. Obst 2, D. Schroeder-Obst 1, W. Fink 1, G. Knupp 1 and J. Steinhaus 1 1 Bonn-Rhine-Sieg University of Applied Sciences, Department of Applied Natural Sciences, von-liebig-str. 20, D Rheinbach, Germany, 2 Dr. Obst Technische Werkstoffe, von-wrangell-str. 8, D Rheinbach, Germany 1

2 1. Introduction Contents 2. Pyrolysis gas chromatography/mass spectrometry (Py-GC/MS) 3. Application examples of Py-GC/MS in failure analysis of hydraulic cylinders from the automotive industry - identification of fouling in the hydraulic cylinder - identification of fibers from the hydraulic cylinder - identification of a glue residue on the membrane from the hydraulic cylinder - identification of additives in nitril rubber membrane from the hydraulic cylinders 4. Conclusions 5. References 2

fouling in the hydraulic cylinder - identification of fibers from the hydraulic cylinder - identification of a glue residue

3 Pyrolysis gas chromatography/mass spectrometry apparatus (Py-GC/MS) (SGE/Agilent Technologies) 3

4 Pyrolysis gas chromatography/mass spectrometry apparatus (Py-GC/MS) (SGE/Thermo) Heizpilz Schematic view of the pyrolyzer 4

5 Fouling on the wall of the hydraulic cylinder 5

6 Pyrolysis-GC/MS chromatogram of fouling in the hydraulic cylinder 1 8 Peak Nr. RT (min) Pyrolysis product Butene/1,3-butadiene SBR Pyrolyzed material Pentene Mineral oil Hexene Mineral oil Benzene SBR Heptene Mineral oil Toluene SBR Octene Mineral oil Hexamethylocyclotrisiloxane PDMS Nonene Mineral oil Styrene SBR Octamethylocyclotetrasiloxane PDMS Decene Mineral oil Undecene Mineral oil Decamethylocyclopentasiloxane Dodecamethylocyclohexasiloxane PDMS PDMS Heavy n-alkanes Mineral oil 6

41 Hexamethylocyclotrisiloxane PDMS 9 15.84 1-Nonene Mineral oil 10 16.06 Styrene SBR 2 11 19.03 Octamethylocyclotetrasiloxane PDMS 4 6 12 19.

7 Pyrolysis-GC/MS chromatograms of fibers from the failed hydraulic cylinder 1 2 Fibers from the failed hydraulic cylinder PTFE Blister packing materialli (A) Guide rings (B) Blister packing material 7

failed hydraulic cylinder PTFE Blister packing

Pyrolysis-GC/MS chromatograms of rubber membranes from the hydraulic cylinder Peak Retention time (RT) [min] Pyrolysis products of the rubber membrane with glue coating at 700 C Pyrolyzed material 1

8 Pyrolysis-GC/MS chromatograms of rubber membranes from the hydraulic cylinder Peak Retention time (RT) [min] Pyrolysis products of the rubber membrane with glue coating at 700 C Pyrolyzed material Propene SBR, mineral oil Butene/1,3-Butadiene SBR, mineral oil Pentene Mineral oil Hexene Mineral oil Benzene SBR Heptene Mineral oil Methyl methacrylate PMMA ,4-Dimethyl-1,3-pentadiene SBR Toluene SBR Octene Mineral oil p-xylene SBR Nonene Mineral oil Styrene SBR Decene Mineral oil Trimethylbenzene SBR Indene SBR Undecene Mineral oil Dodecene Mineral oil Tridecene Mineral oil Tetradecene Mineral oil Heavy n-alkanes Mineral oil 8

94 Methyl methacrylate PMMA 8 11.00 2,4-Dimethyl-1,3-pentadiene SBR 9 12.04 Toluene SBR 10 12.26 1-Octene Mineral oil 11 13.84 p-xylene SBR 12 13.95 1-Nonene Mineral oil 13 14.22 Styrene SBR 14 15.

9 A b u n d a n c e 2. 6 e e T I C : P Y R O L Y S E D \ d a t a. m s Additives in NBR membrane 2. 4 e e e e e e e e e e e e e e Nitrile rubber membrane with additives 7 1 e N-phenyl-1,4-benzenediamine 8 Benzothiazole T i m e - - > A b u n d a n c e e e e e e e T I C : P Y R O L Y S E D \ d a t a. m s Nitrile rubber membrane without additives Peak RT (min) Compound ,3-Butadiene Acrylonitrile Methacrylonitrile Benzene Toluene Styrene Benzonitrile T i m e - - > Indene Toluonitrile Naphthalene

1 e + 0 7 1 2 4 Nitrile rubber membrane with additives 7 1 e + 0 7 9 0 0 0 0 0 0 8 0 0 0 0 0 0 7 0 0 0 0 0 0 6 0 0 0 0 0 0 5 0 0 0 0 0 0 4 0 0 0 0 0 0 3 6 N-phenyl-1,4-benzenediamine 8 Benzothiazole

10 Conclusions Analytical pyrolysis-gas chromatography/mass spectrometry has been proved as a valuable technique for analysis and identification of organic polymeric materials in the failure analysis in the automobile industry. This technique allows the direct analysis of very small sample amounts (5 200 µg) without the need of time-consuming sample preparation. The obtained analytical results were then used for troubleshooting and remedial action of the technological process. 10

This technique allows the direct analysis of very small sample amounts (5 200 µg) without the need of time-consuming

11 References P. Kusch, Pyrolysis gas chromatography/mass spectrometry of polymeric materials in Advanced Gas Chromatography - Progress in Agricultural, Biomedical and Industrial Applications, Ed. M. A. Mohd, InTech, Rijeka, Croatia, 2012, pp , ISBN ; P. Kusch, V. Obst, D. Schroeder-Obst, G. Knupp, W. Fink Einsatz der Pyrolyse - GC/MS zur Untersuchung von Polymeren Materialien in der Schadenanalyse in der Automobilindustrie, ANALYTIK NEWS Das Online- Magazin für Labor und Analytik, 44/2009, ; P. Kusch, V. Obst, D. Schroeder-Obst, G. Knupp, W. Fink Einsatz der Pyrolyse - Gaschromatographie/Massenspektrometrie zur Untersuchung von polymeren Materialien in der Schadenanalyse in der Automobilindustrie, LC GC AdS, July/August 2008, 5-11; 11

com/books/advanced-gas-chromatography-progressin-agricultural-biomedical-and-industrial-applications/pyrolysis-gaschromatography-mass-spectrometry-of-polymeric-materials P. Kusch, V. Obst, D.

12 Thank you for your attention! Dr. Peter Kusch Hochschule University of Applied Sciences Department of Applied Natural Sciences D Rheinbach Germany 12

Pyrolysis-Gas Chromatography/Mass Spectrometry of Polymeric Materials

16 Pyrolysis-Gas Chromatography/Mass Spectrometry of Polymeric Materials Peter Kusch Bonn-Rhine-Sieg University of Applied Sciences, Department of Applied Natural Sciences, Rheinbach, Germany 1. Introduction