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.

A batch of bimetal foil/epoxy laminates was rejected because of poor peel strength. The laminates were manufactured by sintering a nickel/phosphorus powder layer to a copper foil, cleaning, then chromate conversion coating the nickel-phosphorus surface, and laminating the nickel-phosphorus side of the clad bimetal onto an epoxy film, so that the end product contained nickel-phosphorus sandwiched between copper and epoxy, with a chromate conversion layer on the epoxy side of the nickel-phosphorus. Peel testing showed abnormally low adhesion strength for the bad batch of peel test samples. Comparison with normal-strength samples using XPS indicated an 8.8% Na concentration on the surface of the bad sample; the good example contained less than 1% Na on the surface. After 15 min of argon ion etching, depth profiling showed high concentrations of sodium were still evident, indicating that the sodium was present before the chromate conversion treatment was performed. A review of the manufacturing procedures showed that sodium hydroxide was used as a cleaning agent before the chromate conversion coating. Failure cause was that apparently the sodium hydroxide had not been properly removed during water rinsing. Thus, recommendation was to modify that stage in the processing.

A Ti-6Al-4V alloy pressure vessel failed during a proof-pressure test, fracturing along the center girth weld. The girth joints were welded with the automatic gas tungsten arc process utilizing an auxiliary trailing shield attached to the welding torch to provide inert-gas shielding for the exterior surface of the weld. A segmented backup ring with a gas channel was used inside the vessel to shield the weld root. The pressure vessel failed due to contamination of the fusion zone by oxygen, which resulted when the gas shielding the root face of the weld was diluted by air that leaked into the gas channel. Thermal stresses cracked the embrittled weld, exposing the crack surfaces to oxidation before cooling. One of these cracks caused a stress concentration so severe that failure of the vessel wall during the proof test was inevitable. A sealing system at the split-line region of the segmented backup ring was provided, and a fine-mesh stainless steel screen diffuser was incorporated in the channel section of the backup ring to prevent air from leaking in. A titanium alloy color chart was furnished to permit correlation of weld-zone discoloration with the degree of atmospheric contamination.

One inch diam Type 304 stainless steel piping was designed to carry containment atmosphere samples to an analyzer to monitor hydrogen and oxygen levels during operational and the design basis accident conditions that are postulated to occur in a boiling water reactor. Only one of six lines in the system had thru-wall cracks. Shallow incipient cracks were detected at the lowest elevations of one other line. The balance of the system had no signs of SCC attack. Chlorides and corrosion deposits in varying amounts were found throughout the system. The failure mechanism was transgranular, chloride, stress-corrosion cracking. Replacement decisions were based on the presence of SCC attack or heavy corrosion deposits indicative of extended exposure time to chloride-contaminated water. The existing uncracked pipe, about 75 percent of the piping in the system, was retained despite the presence of low level surface chlorides. Controls were implemented to insure that temperatures are kept below 150 deg F, or, walls of the pipe are moisture-free or the cumulative wetted period will never exceed 30 h.

An outer fan-duct assembly of titanium alloy Ti-5Al-2.5Sn (AMS 4910) for a gas-turbine fan section cracked 75 mm (3 in.) circumferentially through a repair weld in an arc weld in the front flange-duct segment. Examination of the crack with a binocular microscope revealed no evidence of fatigue. A blue etch-anodize inspection showed the presence of an alpha case along the edges of the repair weld. The alpha case, a brittle oxide-enriched layer, forms when welds are inadequately shielded from the atmosphere during deposition. The brittleness of this layer caused transgranular cracks to form and propagate in tension under the thermal stresses created by the repair-weld heat input. The crack resulted from contamination and embrittlement of a repair weld that had received inadequate gas shielding. Thermal stresses cracked the oxide-rich layer that formed. The gas-shielding accessories of the welding torch were overhauled to ensure that leak-in or entrainment of air was eliminated. Also, the purity of the shielding-gas supplies was rechecked to make certain that these had not become contaminated.

An aluminum brass seawater surface condenser failed due to pitting after less than one year of service. Large pits filled with a green deposit were evidenced under the nonuniform black scale present over the entire inside surface of the tube. The black deposit was identified as primarily copper sulfide, with zinc and aluminum sulfides while the green deposit was revealed to be copper chloride. The combination of sulfide and chloride attack on the tubes was concluded to have resulted in the failure. Injection of ferrous sulfate upstream of the condenser which could aid the formation of protective oxide films was recommended.

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.

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.

Failure of three C22000 commercial bronze rupture discs was caused by mercury embrittlement. The discs were part of flammable gas cylinder safety devices designed to fail in a ductile mode when cylinders experience higher than design pressures. The subject discs failed prematurely below design pressure in a brittle manner. Fractographic examination using SEM indicated that failure occurred intergranularly from the cylinder side. EDS analysis indicated the presence of mercury on the fracture surface and mercury was also detected using scanning auger microprobe (SAM) analysis. The mercury was accidentally introduced into the cylinders during a gas-blending operation through a contaminated blending manifold. Replacement of the contaminated manifold was recommended along with discontinued use of mercury manometers, the original source of mercury contamination.

Following a freight train derailment, part of a fractured side frame was retained for study because a portion of its fracture surface exhibited a rock candy appearance and black scale. It was suspected of having failed, thereby precipitating the derailment. Metallography, scanning electron microscopy, EDXA, and x-ray mapping were used to study the steel in the vicinity of this part of the fracture surface. It was found to be contaminated with copper. Debye-Scherrer x-ray diffraction patterns obtained from the scale showed that it consisted of magnetite and hematite. It was concluded that some copper was accidentally left in the mold when the casting was poured. Liquid copper, carrying with it oxygen in solution, penetrated the austenite grain boundaries as the steel cooled. The oxygen reacted with the steel producing a network of scale outlining the austenite grain structure. When the casting fractured as a result of the derailment, the fracture followed the scale in the contaminated region thus creating the “rock candy” fracture.

Several type 304L stainless steel dished ends used in the fabrication of cylindrical vessels developed extensive cracking during storage. All of the dished ends had been procured from a single manufacturer and belonged to the same batch. When examined visually, several rust marks were observed, indicating contamination by rusted carbon steel particles. Liquid penetrant testing was used to determine the extent of the cracks, and in situ metallographic analysis was performed over the cracked region. The morphology of the cracks was indicative of transgranular stress-corrosion cracking (TGSCC). Conditions promoting the occurrence of the TGSCC included significant tensile stresses on the inside of the dished ends, the presence of surface contamination by iron due to poor handling practice using carbon steel implements, and storage in a coastal environment with an average temperature of 25 to 32 deg C (77 to 90 deg F), an average humidity ranging from 70 to 80%, and an atmospheric NaCl content ranging from 8 to 45 mg/m2 /day. Recommendations preventing further occurrence of the situation were strict avoidance of the use of carbon steel handling implements, strict avoidance of cleaning practices that cause long-term exposure to chlorine-containing cleaning fluid, and solution annealing of the dished ends at 1050 deg C (1920 deg F) for 1 h followed by water quenching to relieve residual stresses.

An SB407 alloy 800H tube failed at a 100 deg bend shortly after startup of a new steam superheater. Three bends failed and one bend remote from the failure area was examined. Visual examination showed that the fracture started on the outside surface along the inside radius of the bend and propagated in a brittle, intergranular fashion. Chemical analysis revealed that lead contamination was a significant factor in the failure and phosphorus may have contributed. The localized nature of the cracks and minimum secondary cracking suggested a distinct, synergistic effect of applied tensile stress with the contamination. Stress analysis found that stress alone was not enough to cause failure; however the operating stresses in the 100 deg bends were higher than at most other locations in the superheater Reduced creep ductility may be another possible cause of failure. Remedial actions included reducing the tube temperature, replacing the Schedule 40 100 deg bends with Schedule 80 pipe, and solution annealing the pipe after bending.

Molded plastic couplings used in an industrial application exhibited abnormally brittle properties, as compared to previously produced components. The couplings were specified to be molded from a custom-compounded glass-filled nylon 6/12 resin. An inspection of the molding resin used to produce the discrepant parts revealed that the pellets were of two general types, neither of which matched the pellets from a retained resin lot. Investigation included visual inspection, micro-FTIR in the ATR mode, and analysis using DSC. The thermograms supported the conclusion that the brittle couplings contained a significant level of contamination, polypropylene and nylon 6/6. The source of the polypropylene was likely the purging compound used to clean the compounding extruder. The origin of the nylon 6/6 resin was unknown but may represent a previously compounded resin.

A nozzle in a wastewater vaporizer began leaking after approximately three years of service with acetic and formic acid wastewaters at 105 deg C (225 deg F) and 414 kPa (60 psig). The shell of the vessel was weld fabricated from 6.4 mm (0.25 in.) E-Brite stainless steel plate and measured 1.5 m (58 in.) in diameter and 8.5 m (28 ft) in length. Investigation (visual inspection, chemical analysis, radiography, dye-penetrant inspection, and hydrostatic testing of all E-Brite welds, 4x images, 100x/200x images electrolytically etched with 10% oxalic acid, and V-notch Charpy testing) supported the conclusion that failure of the nozzle weld was the result of intergranular corrosion caused by the pickup of interstitial elements and subsequent precipitation of chromium carbides and nitrides. Carbon pickup was believed to have been caused by inadequate joint cleaning prior to welding. The increase in the weld nitrogen level was a direct result of inadequate argon gas shielding of the molten weld puddle. Two areas of inadequate shielding were identified: improper gas flow rate for a 19 mm (0.75 in.) diam gas lens nozzle, and contamination of the manifold gas system. Recommendations included changes in the cleaning and welding process.

The contamination of lubrication with powdered stone resulted in progressive wear of the internal surfaces of a bearing. Because of the motion of rollers, the inner race exhibited an unusual cyclic washboard wear pattern. Because of a lack of bearing conformity, wear progressed into severe coarse-grain spalling.

Housings (being tested as part of a material conversion) from an electrical appliance failed during an engineering evaluation. They had been injection molded from a commercial polycarbonate/PET blend. Parts produced from the previous material, a nylon 6/6 resin, had consistently passed the testing regimen. Grease was applied liberally within the housing assembly during production. Investigation included visual inspection, 24x SEM images, micro-FTIR in the ATR mode, and analysis using DSC. No signs of material contamination were found, but the thermograms showed a crystallization of the PET resin. The grease present within the housing assembly, analyzed using micro-FTIR, was composed of a hydrocarbon-based oil, a phthalate-based oil, lithium stearate, and an amide-based additive. The conclusion was that the appliance housings failed through environmental stress cracking caused by a phthalate-based oil that was not compatible with the PC portion of the resin blend. Thus, the resin conversion was the root cause of the failures. Additionally, during the injection molding process the molded parts had been undercrystallized, reducing their mechanical strength. More importantly, the resin had been degraded, producing a reduction in the molecular weight and reducing both the mechanical integrity and chemical-resistance properties of the parts.

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.

TiN coated back surgery wires were made of Ti-6Al-4V. The reported failure was the presence of pits located in the uncoated area of the wires. The uncoated area of the wire is where the wire is fixtured in the coating chamber during coating. Examination and analysis of the pits using SEM/EDX detection unit revealed significant peaks of B, O, Zr and Fe. Moreover, the shape of the pits was similar to an arc crater. The formation of pits in the wire was caused during coating due to microarcing. A contaminated fixture used during the coating most likely caused the microarcing.

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.