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differential scanning calorimetry
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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
... 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...
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 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.
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.
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...
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.a0006849
EISBN: 978-1-62708-395-9
...), dimethyl phthalate (194.2), and benzene (78.12). MW, molecular weight. Source: Ref 32 Fig. 25 Differential scanning calorimetry thermogram Fig. 26 Melting point and percent crystallinity of high-density polyethylene 10 mcal/s range; 10 °C/min (18 °F/min), 7.1 mg (1.5 gr). Source: Ref...
Abstract
This article addresses some established protocols for characterizing thermoplastics and whether they are homogeneous resins, alloyed, or blended compositions or highly modified thermoplastic composites. It begins with a discussion on characterizing mechanical, rheological, and thermal properties of polymer. This is followed by a section describing molecular weight determination using viscosity measurements. Next, the article discusses the use of cone and plate and parallel plate geometries in melt rheology. It then reviews the processes involved in the analysis of thermoplastic resins by chromatography. Finally, the article covers three operations of thermoanalysis, namely differential scanning calorimetry, thermogravimetric analysis, and thermomechanical testing.
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
... , heat of reaction. Source: Ref 26 Fig. 11 Isothermal differential scanning calorimetry of epoxy resin at three temperatures. DGEBA, diglycidylether of bisphenol A; EDA, ethylene diamine. Source: Ref 25 Fig. 13 Conversion-versus-time data for the same epoxy-amine system shown...
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.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 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
... 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...
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 Failure Analysis Case Histories
Publisher: ASM International
Published: 01 June 2019
DOI: 10.31399/asm.fach.auto.c0090442
EISBN: 978-1-62708-218-1
... nature of their structures. However, subtle but distinct differences were apparent in the results, suggestive of degradation of the failed part material. Differential scanning calorimetry was performed on the sleeve materials using a heat/cool/heat methodology. Testing of the reference material...
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.
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
... to distinguish between these materials. Differential scanning calorimetry was used to analyze the latch material. The obtained results showed that the material underwent a single endothermic transition at approximately 165 °C (330 °F), characteristic of the melting point of a polyacetal copolymer...
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.
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
... °C/min (70 °F/min) −0.52 at 10 °C/min (18 °F/min) Differential scanning calorimetry comparison of glass transition temperature (<italic>T</italic><sub>g</sub>) results from sealed and unsealed pans Table 4 Differential scanning calorimetry comparison of glass transition temperature ( T g...
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 Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006945
EISBN: 978-1-62708-395-9
... for assembly design for manufacturing and assembly diglycidyl ether of bisphenol A digital image correlation dynamic key curve dynamic mechanical analysis degree of freedom dioctyl phthalate differential scanning calorimetry differential thermal analysis de ection temperature under load drop weight index poly...
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.9781627081801
EISBN: 978-1-62708-180-1
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0006548
EISBN: 978-1-62708-180-1
... growth rate DBTT ductile-to-ductile transition tempera- ture diam diameter DIN Deutsche Industrie-Normen DMA dynamic mechanical analysis DoD Department of Defense DPFAD deformation plasticity failure assess- ment diagram DSC differential scanning calorimetry DTA differential thermal analysis E Young s...
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006942
EISBN: 978-1-62708-395-9
... (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Detailed definitions and descriptions of these methods can be found in the articles “ Analysis of Polymer Structure ,” “ Thermal Analysis and Thermal Properties ,” and “ Physical, Chemical, and Thermal...
Abstract
Failure analysis is the process used to determine the cause of a failure. There is no definitive method for performing a failure analysis, and the method chosen is dependent upon the type of failure, the availability of background information, the tools available to perform the analysis, and the skills of the analyst. The information outlined in this article focuses on the general methodology while allowing for case-specific techniques to be utilized along the way. It covers the causes of failure, why a failure analysis is performed, the failure analysis process, the planning of failure analysis investigation, recommendations to prevent the need for a failure analysis, the implementation of product reviews, and forensic standards.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006929
EISBN: 978-1-62708-395-9
... at 40 °C/min (70 °F/min) −0.52 at 10 °C/min (18 °F/min) (a) Trade name of Shell Chemical Company Differential scanning calorimetry (DSC) comparison of glass transition temperature (<italic>T</italic><sub>g</sub>) results from sealed and unsealed pans Table 3 Differential scanning...
Abstract
This article provides an overview of the physics and math associated with moisture-related failures in plastic components. It develops key equations, showing how they are used to analyze the causes and effects of water uptake, diffusion, and moisture concentration in polymeric materials and resins. It explains how absorbed moisture affects a wide range of properties, including glass transition temperature, flexural and shear modulus,creep, stress relaxation, swelling, tensile and yield strength, and fatigue cracking. It provides relevant data on common polymers, resins, and fiber-resin composites.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006759
EISBN: 978-1-62708-295-2
.... Howard, NASA Thermal Analysis as a Tool in Chemical Analysis Thermal analysis of polymeric materials can be used in conjunction with FTIR or Raman spectroscopy to confirm the chemistry of a polymeric material. Although methods such as differential scanning calorimetry and thermogravimetric...
Abstract
Chemical analysis is a critical part of any failure investigation. With the right planning and proper analytical equipment, a myriad of information can be obtained from a sample. This article presents a high-level introduction to techniques often used for chemical analysis during failure analysis. It describes the general considerations for bulk and microscale chemical analysis in failure analysis, the most effective techniques to use for organic or inorganic materials, and examples of using these techniques. The article discusses the processes involved in the chemical analysis of nonmetallics. Advances in chemical analysis methods for failure analysis are also covered.
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.9781627083959
EISBN: 978-1-62708-395-9
Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006909
EISBN: 978-1-62708-395-9
Abstract
Accelerated life testing and aging methodologies are increasingly being used to generate engineering data for determining material property degradation and service life (or fitness for purpose) of plastic materials for hostile service conditions. This article presents an overview of accelerated life testing and aging of unreinforced and fiber-reinforced plastic materials for assessing long-term material properties and life expectancy in hostile service environments. It considers various environmental factors, such as temperature, humidity, pressure, weathering, liquid chemicals (i.e., alkalis and acids), ionizing radiation, and biological degradation, along with the combined effects of mechanical stress, temperature, and moisture (including environmental stress corrosion). The article also includes information on the use of accelerated testing for predicting material property degradation and long-term performance.
Book Chapter
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006757
EISBN: 978-1-62708-295-2
... Molecular weight (MW) and molecular weight distribution (MWD) using light scattering as well as other secondary methods Methods of thermal analysis Differential scanning calorimetry (DSC) and differential thermal analysis Thermomechanical analysis Dynamic mechanical analysis Thermogravimetric...
Abstract
Examination of a damaged component involves a chain of activities that, first and foremost, requires good observation and documentation. Following receipt and documentation, the features of damage can be recorded and their cause(s) investigated, as this article briefly describes, for typical types of damage experienced for metallic components. This article discusses the processes involved in visual or macroscopic examination of damaged material; the interpretation of fracture features, corrosion, and wear damage features; and the analysis of base material composition. It covers the processes involved in the selection of metallurgical samples, the preparation and examination of metallographic specimens in failure analysis, and the analysis and interpretation of microstructures. Examination and evaluation of polymers and ceramic materials in failure analysis are also briefly discussed.
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