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Fourier transform infrared spectroscopy
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Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006933
EISBN: 978-1-62708-395-9
Abstract
This article reviews analytical techniques that are most often used in plastic component failure analysis. The description of the techniques is intended to familiarize the reader with the general principles and benefits of the methodologies, namely Fourier transform infrared spectroscopy, energy-dispersive x-ray spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and dynamic mechanical analysis. The article describes the methods for molecular weight assessment and mechanical testing to evaluate plastics and polymers. The descriptions of the analytical techniques are supplemented by a series of case studies to illustrate the significance of each method. The case studies also include pertinent visual examination results and the corresponding images that aided in the characterization of the failures.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c0090439
EISBN: 978-1-62708-220-4
Abstract
A section of clear polymeric tubing failed while in service. The failed sample had been used in a chemical transport application. The tubing had also been exposed to periods of elevated temperature as part of the operation. The tubing was specified to be a polyvinyl chloride (PVC) resin plasticized with trioctyl trimellitate. Investigation included visual inspection, micro-FTIR in the ATR mode, and thermogravimetric analysis. The spectrum on the failed tubing exhibited absorption bands indicative of a PVC resin containing an adipate-based plasticizer. Thermograms of the failed pieces and a reference sample of tubing that performed well showed that the reference material contained a trimellitate-based plasticizer and that the failed material contained an adipate-based material. The conclusion was that the failed tubing had been produced from a formulation that did not comply with the specified material and, as a result, was not as thermally stable as the reference material.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090466
EISBN: 978-1-62708-218-1
Abstract
A production lot of mechanical hinges used in an automotive application had failed during incoming quality-control routine actuation testing. A change in part supplier had taken place between the approval of the prototype parts that performed acceptably and the receipt of the first lot of production parts. The mechanical hinges were specified to be injection molded from an impact-modified, 13% glass-fiber-reinforced nylon 6/6 resin. Investigation of samples representing the failed components and the original prototype parts included visual inspection, 118x SEM images, micro-FTIR, DSC analysis, and TGA. It supported the conclusion that the hinge assemblies failed through brittle fracture associated with stress overload during the actuation of the parts. The failed part material was found to be degraded, most likely occurring during the compounding of the resin or during the actual molding of the parts. While resins for both failed and non-failed parts produced results characteristic of a 13% glass-fiber-reinforced, impact-modified nylon 6/6, the failed part material, contained a significantly lower level of rubber, which rendered the parts less impact resistant and subsequently lowered the ductility of the molded hinge assemblies. No recommendations were made.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c9001629
EISBN: 978-1-62708-235-8
Abstract
A large number of electropolished copper parts showed evidence of discoloration (tinting) after electropolishing. Because these parts are used in a high-vacuum application, even trace amounts of organic materials would be problematic. Scanning electron microscopy of nondiscolored and discolored areas both showed trace amounts of residue in the form of adherent deposits. EDS, FTIR spectroscopy, XPS, and secondary ion mass spectroscopy (SIMS) analyses indicated that the discoloration to the copper components was due to the development of CuO at localized regions. It was recommended that process changes be made to completely remove residual processing fluids from the part surfaces before electropolishing. The use of more aggressive detergents was suggested, and it was recommended also that a filtering and recirculating system be considered for use in the cleaning and electropolishing tanks.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.process.c9001626
EISBN: 978-1-62708-235-8
Abstract
A type 17-4PH stainless steel tube exhibited brown discoloration after a pickling operation. EDS analysis of the extracted substance revealed relatively high levels of iron and chromium, along with lower amounts of aluminum, silicon, sulfur, chlorine, calcium, manganese, and nickel. The iron, chromium, and nickel are likely in the form of dissolution products from the pickling solution. FTIR analysis revealed the presence of polypropylene and poly(ethylene:propylene). The EDS results showed that the discoloration of the tube was associated with oxidation products of the tube material, as well as adherent organic residue. Analysis by FTIR of the residue revealed detectable levels of two polymeric substances, which were later determined to be construction materials of the pickling tank. It was recommended that more frequent cleaning and/or replacement of the pickling solution be put into place and another type of tank material be considered.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c0090460
EISBN: 978-1-62708-234-1
Abstract
A component of a water filtration unit failed while being used in service for approximately eight months. The filter system had been installed in a commercial laboratory, where it was stated to have been used exclusively in conjunction with deionized water. The failed part had been injection molded from a 30% glass-fiber and mineral-reinforced nylon 12 resin. Investigation, including visual inspection, 118x SEM images, 9x micrographs, energy-dispersive x-ray spectroscopy, micro-FTIR in the ATR mode, and TGA, supported the conclusion that the filter component failed as a result of molecular degradation caused by the service conditions. Specifically, the part material had undergone severe chemical attack, including oxidation and hydrolysis, through contact with silver chloride. The source of the silver chloride was not established, but one potential source was photographic silver recovery.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.modes.c9001593
EISBN: 978-1-62708-234-1
Abstract
A failure analysis was conducted on a flow-sensing device that had cracked while in service. The polysulfone sensor body cracked radially, adjacent to a molded-in steel insert. This article describes the investigative methods used to conduct the failure analysis. The techniques utilized included scanning electron microscopy, Fourier transform infrared spectroscopy, differential scanning calorimetry, thermomechanical analysis, and melt flow rate determination. It was the conclusion of the investigation that the part failed via brittle fracture, with evidence also indicating low cycle fatigue associated with cyclic temperature changes from normal service. The design of the part and the material selection were significant contributing factors because of stresses induced during molding, physical aging of the amorphous polysulfone resin, and the substantial differential in coefficients of thermal expansion between the polysulfone and the mating steel insert.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c9001622
EISBN: 978-1-62708-222-8
Abstract
A stamped coin exhibited visible discolored areas, seen as a tan haze on the surface. The discoloration was considered merely cosmetic. The nonstained and stained regions were studied using SEM/EDS. Greater amounts of aluminum and magnesium were found in the stained area as compared with the nonstained region. Some carbon and oxygen were detected in both areas, which may be suggestive of organic substances. Fourier transform infrared spectroscopy (FTIR) revealed traces of hydrocarbons and ether/alcohol materials in the stained area, suggesting that the stain was associated with a cellulose or carbohydrates (sugars). These findings, along with the appearance, suggest that a sugar-containing substance, such as coffee or a soft drink, dried onto the surface of this coin and caused the observed discoloration.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003525
EISBN: 978-1-62708-180-1
Abstract
This article reviews the analytical techniques most commonly used in plastic component failure analysis. These include the Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The descriptions of the analytical techniques are supplemented by a series of case studies that include pertinent visual examination results and the corresponding images that aid in the characterization of the failures. The article describes the methods used for determining the molecular weight of a plastic resin. It explains the use of mechanical testing in failure analysis and also describes the considerations in the selection and use of test methods.