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TGA
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in Thermal Analyses of a Polymer Failure
> ASM Failure Analysis Case Histories: Automobiles and Trucks
Published: 01 June 2019
Fig. 2 TGA scans for the automotive part at three ages and for the two control samples.
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Published: 01 December 2019
Fig. 9 A comparative overlay of the thermogravimetric analysis (TGA) thermograms obtained on core and surface material of the bracket
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in Failure Analysis of Epoxy Resin Encapsulant During a Long-Term Storage
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 5 TGA curves of epoxy resin encapsulants
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in Failure Analysis of Fatigue Fracture on the Outer Ring of a Cylindrical Roller Bearing in an Air Blower Motor
> Handbook of Case Histories in Failure Analysis
Published: 01 December 2019
Fig. 9 TGA results of the greases: ( a ) fresh and ( b ) used
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Series: ASM Failure Analysis Case Histories
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001767
EISBN: 978-1-62708-241-9
... of the thermogravimetric analysis (TGA) thermograms obtained on core and surface material of the bracket Abstract Six transformer brackets failed in service, sending a group of three pole-mounted transformers to the ground below. The brackets were made from acrylonitrile-butadiene-styrene (ABS) resin and had been...
Abstract
Six transformer brackets failed in service, sending a group of three pole-mounted transformers to the ground below. The brackets were made from acrylonitrile-butadiene-styrene (ABS) resin and had been in service for more than 30 years. Remnants of the fractured brackets were analyzed using optical and scanning electron microscopy, Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The exterior surfaces of all six brackets were alike and shared similar features, including witness marks, discoloration, mechanical deformation, and secondary cracking, along with crack networks. Both FTIR and TGA analyses indicated that the surface material was in a highly degraded state, likely due to weathering and thermal and ultraviolet exposure. This, in turn, led to the formation of cracks that propagated under the cyclic forces of vibration and wind. As the cracks grew larger, the weight of the transformer eventually overloaded the brackets, resulting in failure.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c9001901
EISBN: 978-1-62708-218-1
... Abstract Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to analyze an automotive polyoxymethylene (POM) sensor housing that was depolymerizing during service. It was found that a combination of heat, oxygen, and sulfuric acid attacked and caused premature...
Abstract
Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to analyze an automotive polyoxymethylene (POM) sensor housing that was depolymerizing during service. It was found that a combination of heat, oxygen, and sulfuric acid attacked and caused premature failure of the part. POM should not be selected for automotive applications where elevated temperatures and acidic environments can exist. If exposure to acid is suspected, sodium bicarbonate should be applied to neutralize the surrounding environment, followed by copious quantities of water, and repeated until no effervescence is observed.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.chem.c0090454
EISBN: 978-1-62708-220-4
... solvent. Investigation (visual inspection, stereomicroscopic examination, 20x/100x SEM images, micro-FTIR in the ATR mode, and analysis using DSC and TGA) supported the conclusion that the chemical storage vessel failed via a creep mechanism associated with the exertion of relatively low stresses...
Abstract
A chemical storage vessel failed while in service. The failure occurred as cracking through the vessel wall, resulting in leakage of the fluid. The tank had been molded from a high-density polyethylene (HDPE) resin. The material held within the vessel was an aromatic hydrocarbon-based solvent. Investigation (visual inspection, stereomicroscopic examination, 20x/100x SEM images, micro-FTIR in the ATR mode, and analysis using DSC and TGA) supported the conclusion that the chemical storage vessel failed via a creep mechanism associated with the exertion of relatively low stresses. The source of the stress was thought to be molded-in residual stresses associated with uneven shrinkage. This was suggested by obvious distortion evident on cutting the vessel. Relatively high specific gravity and the elevated heat of fusion indicated that the material had a high level of crystallinity. In general, increased levels of crystallinity result in higher levels of molded-in stress and the corresponding warpage. The significant reduction in the modulus of the HDPE material, which accompanied the saturation of the resin with the aromatic hydrocarbon-based solvent, substantially decreased the creep resistance of the material and accelerated the failure.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0090445
EISBN: 978-1-62708-222-8
... the presence of contaminant material exclusively within the ABS resin used to mold the failed covers, and the thermograms suggested contamination with a PBT resin. Further TGA analysis showed the contamination was estimated to account for approximately 23% of the failed cover material. The conclusion...
Abstract
Numerous protective covers, used in conjunction with an electrical appliance, failed during assembly with the mating components. The failures were traced to a particular production lot of the covers and occurred during insertion of the screws into the corresponding bosses. The parts had been injection molded from an ABS resin to which regrind was routinely added. Inspection of both the failed covers and retained parts, which exhibited normal behavior during assembly, included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The FTIR results indicated the presence of contaminant material exclusively within the ABS resin used to mold the failed covers, and the thermograms suggested contamination with a PBT resin. Further TGA analysis showed the contamination was estimated to account for approximately 23% of the failed cover material. The conclusion was that the appliance covers failed via brittle fracture associated with stress overload. The failures, which occurred under normal assembly conditions, were attributed to embrittlement of the molded parts, due to contamination of the ABS resin with a high level of PBT. The source of the PBT resin was not positively identified, but a likely source appeared to be the use of improper regrind.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.homegoods.c0090457
EISBN: 978-1-62708-222-8
... images, micro-FTIR in the ATR mode, and DSC/TGA/MFR analysis) showed no evidence of contamination or degradation from the molding process. The conclusion was that the parts failed via brittle fracture associated with stress overload. The stress overload was accompanied by severe apparent embrittlement...
Abstract
Components of a latch assembly used in a consumer safety restraint exhibited a relatively high failure rate. The failures were occurring after installation but prior to actual field use when failure could result in severe injury. Cracking occurred within retaining tabs used to secure a metal slide on an older design, whereas newer components showed no signs of failure. The latch assembly components were injection molded from an unfilled commercial grade of a polyacetal copolymer. Investigation of failed parts (including visual inspection, a specially designed proof load test, 59x SEM images, micro-FTIR in the ATR mode, and DSC/TGA/MFR analysis) showed no evidence of contamination or degradation from the molding process. The conclusion was that the parts failed via brittle fracture associated with stress overload. The stress overload was accompanied by severe apparent embrittlement resulting from a relatively high strain rate event and/or significant stress concentration. A relatively sharp corner formed by a retaining tab on the older design was shown to be a primary cause of the failures.
Book Chapter
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090451
EISBN: 978-1-62708-218-1
..., and analysis using DSC and TGA) with non-failed parts supported the conclusion that that the failure was via brittle fracture associated with the exertion of stresses that exceeded the strength of the resin as-molded caused by the disparity in the CTEs of the PET jacket and the mating steel sleeve. The drying...
Abstract
Cracking occurred within the plastic jacket (injection molded from an impact-modified, 15% glass-fiber-reinforced PET resin.) of several assemblies used in a transportation application during an engineering testing regimen which involved cyclic thermal shock (exposing the parts to alternating temperatures of -40 and 180 deg C (-40 and 360 deg F)). Prior to molding, the resin had reportedly been dried at 135 deg C (275 deg F). The drying process usually lasted 6 h, but occasionally, the material was dried overnight. Comparison investigation (visual inspection, 20x SEM views, micro-FTIR, and analysis using DSC and TGA) with non-failed parts supported the conclusion that that the failure was via brittle fracture associated with the exertion of stresses that exceeded the strength of the resin as-molded caused by the disparity in the CTEs of the PET jacket and the mating steel sleeve. The drying process had exposed the resin to relatively high temperatures, which caused substantial molecular degradation, thus limiting the part's ability to withstand the stresses. The drying temperature was found to be significantly higher than the recommendation for the PET resin, and the testing itself exposed the parts to temperatures above the recognized limits for PET.
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
..., 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...
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.
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
... 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...
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
Volume: 3
Publisher: ASM International
Published: 01 December 2019
DOI: 10.31399/asm.fach.v03.c9001798
EISBN: 978-1-62708-241-9
... Carbon and oxygen contents of epoxy resin encapsulants Table 2 Carbon and oxygen contents of epoxy resin encapsulants Specimen C (wt.%) O (wt.%) C/O Normal 71.97 28.03 2.57 Softened 70.52 29.48 2.39 Fluid 70.27 29.73 2.36 Typical parameters in three TGA curves...
Abstract
The crosslinked epoxy resin encapsulant protecting an electromagnetic valve coil failed during long-term storage and was examined to determine the cause. The investigation included fault-tree analysis, FTIR and EDX spectroscopy, and differential scanning calorimetry with thermogravimetric analysis. Based on test data, the epoxy resin had not been properly cured and was hydrolyzed in its compromised state because of humidity. Hence, the depolymerized material gradually softened to the point where the effect of creep caused it to flow, ultimately causing the failure.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006931
EISBN: 978-1-62708-395-9
..., T m Phase changes, T g and T m Differential scanning calorimetry (DSC) Heat of polymerization, fusion, T g , T m Phase changes, reaction kinetics degree of cross linking, degradation inhibitor content and effectiveness Thermogravimetric analysis (TGA) Composition, weight loss...
Abstract
This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.
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
... their relative thermal stability, the two tubing materials were analyzed via thermogravimetric analysis (TGA). Both sets of results were consistent with those expected for plasticized PVC resins. The thermograms representing the reference and failed sample materials showed comparable plasticizer contents of 28...
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.
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
... identification, contamination, degradation, chemical contact Differential scanning calorimetry (DSC) Heat of fusion, melting point, glass transition temperature, heat capacity Material identification, level of crystallinity, aging/degradation, thermal history Thermogravimetric analysis (TGA) Weight loss...
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.
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
... or to determine whether a plastic resin has undergone partial oxidation. Thermogravimetric Analysis Thermogravimetric analysis (TGA) is a thermal analysis technique that measures the amount and rate of change in the weight of a material as a function of temperature or time in a controlled atmosphere...
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.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006924
EISBN: 978-1-62708-395-9
...: Ref 44 Fig. 21 Percent mass loss as a function of temperature for phenolic resin samples as noted in the figure. TGA, thermogravimetric analysis; DTG, derivative thermogravimetry. Source: Ref 45 Fig. 22 Thermogravimetric analysis of thermoplastic-thermoset adhesive, 15 °C/min...
Abstract
This article discusses the most common thermal analysis methods for thermosetting resins. These include differential scanning calorimetry, thermomechanical analysis, thermogravimetric analysis, and dynamic mechanical analysis. The article also discusses the characterization of uncured thermosetting resins as well as the curing process. Then, the techniques to characterize the physical properties of cured thermosets and composites are presented. Several examples of stress-strain curves are shown for thermosets and thermoplastic polymers.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006923
EISBN: 978-1-62708-395-9
... (d) ASTM D256 Izod impact TGA (e) DSC (b) TMA (c) Extrapolated onset temperature wt% at 600 °C (1110 °F) °C °F °C °F J/m ft · lbf/in. °C °F PVC, flexible 29 65 150 41 105 T g 270 5.0 274 525 5.7 PVC, rigid 30 120 250 102 215 T g 20 0.4 278 530...
Abstract
This article discusses the thermal properties of engineering plastics and elastomers with respect to chemical composition, chain configuration, and base polymer conformation as determined by thermal analysis. It describes the processing of base polymers with or without additives and their response to chemical, physical, and mechanical stresses whether as an unfilled, shaped article or as a component of a composite structure. It summarizes the basic thermal properties of thermoplastics and thermosets, including thermal conductivity, temperature resistance, thermal expansion, specific heat, and glass transition temperature. It also provides information on polyimide and bismaleimide resin systems. Representative examples of different types of engineering thermoplastics are discussed primarily in terms of structure and thermal properties.
Series: ASM Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090442
EISBN: 978-1-62708-218-1
... A comparison of the second heating run results, further suggesting degradation of the failed sleeve material The sleeve materials were further analyzed using TGA. The thermograms obtained on the reference and failed samples were generally consistent, including equivalent glass contents. Additionally...
Abstract
A number of plastic sleeves used in an automotive application cracked after assembly but prior to installation into the mating components. The sleeves were specified to be injection molded from a 20% glass-fiber-reinforced polybutylene terephthalate (PBT) resin. After molding, electronic components are inserted into the sleeves, and the assembly is filled with a potting compound. Investigation of the cracked parts and some reference parts available for testing included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. Subtle spectrum differences suggested degradation of the failed part material, and the thermograms supported this. The conclusion was that the failed sleeves had cracked due to embrittlement associated with severe degradation and the corresponding molecular weight reduction. The reduction in molecular weight significantly reduced the mechanical properties of the sleeves. The cause of the degradation was not evident, but the likely source appears to be the molding operation and exposure to elevated temperature for an extended period of time.
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