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.

Failure analysis of a mobile harbor crane wheel hub that included SEM and EDS analyses demonstrated that the mechanism of failure was fatigue. The wheel hub was a ductile cast iron component that had been subjected to cyclic loading during a ten-year service period. The fracture surface of the fatigue failure also contained corrosion deposit, suggesting that cracking occurred over a period of time sufficient to allow corrosion of the cracked surfaces. Replacement and alignment of the failed wheel hub was recommended along with inspection of the nonfailed wheel hubs that remained on the crane.

An Incoloy 800H (UNS N08810) transfer line on the outlet of an ethane-cracking furnace failed during decoking of the furnace tubes after nine years in service. A metallographic examination using optical and scanning electron microscopy as well as energy-dispersive x-ray spectroscopy revealed that the failure was due to sulfidation. The source of the sulfur in the furnace effluent was either dimethyl disulfide, injected into the furnace feed to prevent coke formation and carburization of the furnace tubes, or contamination of the feed with sulfur bearing oil.

A kiln, 7.6 m (25 ft) long with a 1 m (3 ft) internal diameter and a 6.3 mm (0.25 in.) wall thickness, is used to regenerate spent charcoal returned by water utilities. This charcoal contains up to 0.57% S and 2.04% Cl. The kiln is made of Inconel 601 (N06601) welded using Inconel 617 (N06617) as a filler alloy. Wet charcoal is fed in at one end of the kiln and travels while being tumbled within the inclined rotating vessel. Temperatures range from 480 deg C (900 deg F) (Zone 1) to 900 deg C (1650 deg F) (Zones 2 and 3). Steam is introduced at the discharge end at 95 g/s (750 lb/h), 34 to 69 kPa (5 to 10 psi), and 125 deg C (260 deg F). The kiln developed perforations within eight months of operation. Investigation (visual inspection, metallurgical analysis, energy-dispersive spectroscopy, and 44X micrographs) supported the conclusion that the sulfur and chlorine in the charcoal attacked the Inconel 601, forming various sulfides and chlorides. Recommendations included on-site testing, and installation of test coupons of various alloys before fabricating another kiln. The suggested alloys were RA85H, 800HT, HR-120, Haynes 556, and HR-160.

The US Army Research Laboratory performed a failure investigation on a broken main landing gear mount from an AH-64 Apache attack helicopter. A component had failed in flight, and initially prevented the helicopter from safely landing. In order to avoid a catastrophe, the pilot had to perform a low hover maneuver to the maintenance facility, where ground crews assembled concrete blocks at the appropriate height to allow the aircraft to safely touch down. The failed part was fabricated from maraging 300 grade steel (2,068 MPa [300 ksi] ultimate tensile strength), and was subjected to visual inspection/light optical microscopy, metallography, electron microscopy, energy dispersive spectroscopy, chemical analysis, and mechanical testing. It was observed that the vacuum cadmium coating adjacent to the fracture plane had worn off and corroded in service, thus allowing pitting corrosion to occur. The failure was hydrogen-assisted and was attributed to stress corrosion cracking (SCC) and/or corrosion fatigue (CF). Contributing to the failure was the fact that the material grain size was approximately double the required size, most likely caused from higher than nominal temperatures during thermal treatment. These large grains offered less resistance to fatigue and SCC. In addition, evidence of titanium-carbo-nitrides was detected at the grain boundaries of this material that was prohibited according to the governing specification. This phase is formed at higher thermal treatment temperatures (consistent with the large grains) and tends to embrittle the alloy. It is possible that this phase may have contributed to the intergranular attack. Recommendations were offered with respect to the use of a dry film lubricant over the cadmium coated region, and the possibility of choosing an alternative material with a lower notch sensitivity. In addition, the temperature at which this alloy is treated must be monitored to prevent coarse grain growth. As a result of this investigation and in an effort to eliminate future failures, ARL assisted in developing a cadmium brush plating procedure, and qualified two Army maintenance facilities for field repair of these components.

Suspension lugs fabricated from AISI 4340 steel used to facilitate loading of bombs onto the underside of military aircraft could not sustain required loads during routine proof load testing. Three failed lugs underwent visual examination, chemical analysis, metallography, hardness testing, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. It was determined that the failures were due to forging defects. Both forging laps and seams acted as stress concentrators when the lugs were loaded during proof testing.

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.

A nuclear steam-generator vessel constructed of 100-mm thick SA302, grade B, steel was found to have a small leak. The leak originated in the circumferential closure weld joining the transition cone to the upper shell. The welds had been fabricated from the outside by the submerged arc process with a backing strip. The backing was back gouged off, and the weld was completed from the inside with E8018-C3 electrodes by the shielded metal arc process. Striations of the type normally associated with progressive or fatigue-type failures including beach marks that allowed tracing the origin of the fracture to the pits on the inner surface of the vessel were revealed. Copper deposits with zinc were revealed by EDS examination of discolorations. Pitting was revealed to have been caused by poor oxygen control in the steam generators and release of chloride into the steam generators. It was concluded by series of controlled crack-propagation-rate stress-corrosion tests that A302, grade B, steel was susceptible to transgranular stress-corrosion attack in constant extension rate testing with as low as 1 ppm chloride present. It was recommended to maintain the coolant environment low in oxygen and chloride. Copper ions in solution should be eliminated or minimized.

Pendant-style reheater, constructed of ASME SA-213, grade T-11, steel ruptured. A set of four tubes, specified to be 64 mm OD x 3.4 mm minimum wall thickness was examined. A small quantity of loose debris was removed from the inside of one of the tubes. The major constituent was revealed by EDS analysis of the debris to be iron with traces of phosphorus, manganese, sodium, calcium, copper, zinc, potassium, silicon, chromium, and molybdenum. Thus the debris was interpreted to be the scale from ID of the tube with boiler feedwater chemicals from the attemperation spray. The likely cause of failure was concluded to be exfoliation of the scale from the ID surface of the tube. Creep failures were interpreted to be caused by localized temperatures higher than the maximum service temperature. Replacement of the affected tubes was recommended. Inspection of the tubes by radiography to find the circuits with the greatest accumulation of debris and replacing them as necessary was recommended on an annual basis.

An arsenical admiralty brass (UNS C44300) finned tube in a generator air cooler unit at a hydroelectric power station failed. The unit had been in operation for approximately 49,000 h. The cooling medium for the tubes was water from a river. Air flowed over the finned exterior of the tubes, while water circulated through the tubes. Investigation (visual inspection, leak testing, history review, 100X micrographs etched in potassium dichromate, chemical analysis, and EDS and XRD analysis of internal tube deposits) supported the conclusion that the cause of the tube leaks was ammonia-induced SCC. Because the cracks initiated on the inside surfaces of the tubes and because the river water was not treated before it entered the coolers, the ammonia was likely present in the river water and probably concentrated under the internal deposits. Recommendations included either eliminating the ammonia (prohibitively expensive in cost and time) or using an alternate material (such as a 70Cu-30Ni alloy or a more expensive titanium alloy) that is resistant to ammonia corrosion as well as to chlorides and sulfur species.

Cracks, with no other damage, were observed in a niobium alloy (Nb-106) part when it was pulled from several months of protective storage for assembly into a rocket nozzle. SEM views showed the cracks to be intergranular, with contaminant particles on a large number of the grain facets. EDX analysis showed they consisted of niobium and fluorine. Plastic replicas, prepared by standard TEM techniques, were analyzed with selected-area electron diffraction, showing a pattern match for niobium tetrafluoride. Auger analyses showed electron spectra containing peaks representing carbon, oxygen, nitrogen, fluorine, and chlorine. Investigation into the processing history of the part showed the tenacious oxide film formed by the affinity of niobium for oxygen - even when heat treated in a vacuum – was removed with a combination of strong acids: nitric, hydrochloric, hydrofluoric, and lactic, resulting in the contaminants found on the surface. Thus, residues of the cleaning acid on the part had caused SCC during storage, with the tensile stresses necessary to generate SCC assumed to have been residual stresses from the heat treatment. Recommendation was made that more stringent cleaning procedures to remove any trace of the cleaning acids be used.

Alloy steel forgings used as structural members of a ski chair lift grip mechanism were identified to have contained forging laps (i.e., sharp-notched discontinuities) during an annual magnetic particle inspection of all chair lift grip structural members at a mountain resort. The material was confirmed to be 34Cr-Ni-Mo6. A heavy oxide on the dark area of one of the broken-open laps was revealed by scanning electron microscopy in conjunction with EDS. A bright area that contained ductile dimple rupture was observed adjacent to the dark area. The oxidized portion of the fracture was established to be the preexisting forging lap while the bright area was created during the breaking-open process. As a corrective action all forgings showing laps were recommended to be removed from service. Critical review and revision of the forging process and revisions to the nondestructive evaluation procedures at the forging supplier was recommended.

The presence of subsurface cracks in a longitudinal weld seam of an AISI type 316 stainless steel heat-exchanger shell was revealed by radiographic testing. Numerous intergranular cracks associated with the root pass of the weld, which had propagated both parallel and normal to the weld seam, were revealed by metallographic examination (hot shortness). It was indicated by energy-dispersive spectroscopy that type 316 electrode was not used for the root pass and instead a nickel-copper alloy electrode was employed. It was thus concluded that cracking was caused due to the use of an incorrect electrode for the root pass as these electrodes are crack sensitive if overheated. The weld seam was completely ground out and replaced with the correct electrode material as a corrective measure.

Within the first few months of operation of an 8 km (5 mile) long 455 mm (18 in.) diam high-pressure steam line between a coal-fired electricity-generating plant and a paper mill, several of the Inconel 600 bellows failed. The steam line operated at 6030 kPa (875 psi) and 420 deg C (790 deg F). Metallographic sections, energy-dispersive x-ray spectra, chemical analyses, tensile tests, and Auger microscope analyses showed the failed bellows met the specifications for the material. However, investigation also showed entire oxide thickness was contaminated with relatively large amounts of sodium, calcium, potassium, aluminum, and sulfur, alkali, alkali earth, and other contaminants that completely permeated even the thin oxides on the fracture surfaces. Additional investigation of the purity of the steam itself as reported by the power plant showed that corrosion and cracks were ultimately caused by the steam. While under normal operation, the steam's purity posed no problem to the material, during boiler cleaning operations, the generating plant had allowed contamination to get into the steam line.

A failure analysis case study on railroad rails is presented. The work, performed under the sponsorship of the Department of Transportation, addresses the problem of shell and detail fracture formation in standard rails. Fractographic and metallographic results coupled with hardness and residual stress measurements are presented. These results suggest that the shell fractures form on the plane of maximum residual tensile stresses. The formation of the shells is aided by the presence of defects in the material in these planes of maximum residual stress. The detail fracture forms as a perturbation from the shell crack under cyclic loading and is constrained to develop as an embedded flaw in the early stages of growth because the crack is impeded at the gage side and surface of the rail head by compressive longitudinal stresses.

A cadmium-plated 4340 Ni-Cr-Mo steel ballast elbow assembly was submitted for failure analysis to determine the element or radical present in an oxidation product found inside the elbow assembly. Energy-dispersive x-ray analysis in the SEM showed that iron was the predominant species, presumably in an oxide form. The inside surface had the appearance of typical corrosion products. Hardness measurements indicated that the 4340 steel was heat treated to a strength of approximately 862 MPa (125 ksi). It was concluded that the oxide detected on the ballast elbow was iron oxide. The possibility that the corrosion products would eventually create a blockage of the affected hole was great considering the small hole diameter (4.2 mm, or 0.165 in.). It was recommended that a quick fix to stop the corrosion would be to apply a corrosion inhibitor inside the hole. This, however, would cause the possibility of inhibitor buildup and the eventual clogging of the hole. A change in the manufacturing process to include a cadmium plating on the hole inside surface was recommended. This was to be accomplished in accordance with MIL specification QQ-P-416, Type II, Class 1. A material change to 300-series stainless steel was also recommended.

A nickel alloy cylinder plated with chromium along its inner liner, installed in a commercial ice cream freezer, showed gray discoloration along its OD surface. The discolored parts exhibited significantly reduced cooling efficiency as compared with new cylinders. During operation, the OD of the cylinder was exposed to liquid ammonia refrigerant containing lubricant from the compressor. The lubricant (mineral oil) was intended to separate from the ammonia and be recirculated through the compressor. Nondestructive portable optical microscopy, XRF, EDS, and XPS analyses showed that the discoloration on the cylinder was associated with metal oxidation products coated with a thin oil film. One of the recommendations was to plate the OD of the cylinder with hard chromium to increase its resistance to erosion. Another recommendation was to reduce the amounts of water contamination in the refrigerant.

A type 304 austenitic stainless steel tube (0.008 max C, 18.00 to 20.00 Cr, 2.00 max Mn, 8.00 to 10.50 Ni) was found to be corroded. The tube was part of a piping system, not yet placed in service, that was exposed to an outdoor marine environment containing chlorides. As part of the assembly, a fabric bag containing palladium oxide was taped to the tube. The palladium served as a “getter.” Investigation (visual inspection and EDS analysis of corrosion debris) supported the conclusion that chlorides and palladium both contributed to corrosion in the crevice created by the tape on the tube, which was periodically exposed to water. Recommendations included taking steps to prevent water from entering and being trapped in this area of the assembly.

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.

Accelerated aging tests on detonator assemblies, to verify the compatibility of gold bridgewire and Pd-In-Sn solder with the intended explosives, revealed an unusual form of corrosion. The tests, conducted at 74 deg C (165 deg F) and 54 deg C (130 deg F), indicated a preferential attack of the gold. To investigate the problem, a matrix of test units was produced and analyzed. Scanning electron microscopy, EDX analysis, and x-ray diffraction techniques were used to determine the extent of the corrosion and identify the corrosion products. The results indicated that the preferential attack of the gold was due to HCN formed by decomposition of the explosive powder at high temperatures. Other associated reactions were also observed including the subsequent attack of the solder by the gold corrosion product and degradation of the plastic header.