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.

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.

Identification of alloys using quantitative chemical analysis is an essential step during a metallurgical failure analysis process. There are several methods available for quantitative analysis of metal alloys, and the analyst should carefully approach selection of the method used. The choice of appropriate analytical techniques is determined by the specific chemical information required, the condition of the sample, and any limitations imposed by interested parties. This article discusses some of the commonly used quantitative chemical analysis techniques for metals. The discussion covers the operating principles, applications, advantages, and disadvantages of optical emission spectroscopy (OES), inductively coupled plasma optical emission spectroscopy (ICP-OES), X-ray spectroscopy, and ion chromatography (IC). In addition, information on combustion analysis and inert gas fusion analysis is provided.

This article covers the three most popular techniques used to characterize the very outermost layers of solid surfaces: Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Some of the more important attributes are listed for preliminary insight into the strengths and limitations of these techniques for chemical characterization of surfaces. The article describes the basic theory behind each of the different techniques, the types of data produced from each, and some typical applications. Also discussed are the different types of samples that can be analyzed and the special sample-handling procedures that must be implemented when preparing to do failure analysis using these surface-sensitive techniques. Data obtained from different material defects are presented for each of the techniques. The examples presented highlight the typical data sets and strengths of each technique.

An axle shaft in an open-pit mining truck hauling overburden failed after operating for 27,000 h. Previous failures had resulted from longitudinal shear, but this had not, bringing material quality into question. Chemical analysis verified that the part was SAE4340 Ni-Cr-Mo alloy steel and thus met material specification. The failure was a result of torsional fatigue in the tensile plane, originating from one of several gouges around the splined radius of the shaft. The fatigue crack progressed for a large number of cycles before final fracture. The shaft met metallurgical requirements and should have withstood normal operating conditions. The spacing of the gouge marks coincided with the spacing of the splines, indicative of careless assembly with the mating wheel gear.

The upper frame from a large cone crusher failed in severe service after an unspecified service duration. The ductile iron casting was identified as grade 80-55-06, signifying minimum properties of 552 MPa (80 ksi) tensile strength, 379 MPa (55 ksi) yield strength, and 6% elongation. Investigation (visual inspection, chemical analysis, unetched 30x images, and 2% nital etched 30x images) was difficult because the fracture surface of the frame section was obliterated by postfracture corrosion. Repeated attempts at cleaning using progressively stronger chemicals revealed that no telltale fracture morphology remained. However, the investigation supported the conclusion that the crusher frame failed via brittle overload fracture, likely due to excessive service stresses and substandard mechanical properties. Recommendations included additional quality-control measures to provide better spheroidal graphite morphology at the frame surface.

After about two years in service, a 303 stainless steel valve in contact with a carbonated soft drink in a vending machine occasionally dispensed a discolored drink with a sulfide odor. According to the laboratory at the bottling plant, the soft drink in question was strongly acidic, containing citric and phosphoric acids and having a pH of 2.4 to 2.5. Investigation (visual inspection, chemical analysis, immersion testing in the soft drink, and 100x unetched micrographs) supported the conclusion that the failure was caused by the size and distribution of sulfide stringers in the alloy used in the valve. Manganese sulfide stringers in the valve were exposed at end-grain surfaces in contact with the beverage. The stringers, which were anodic to the surrounding metal, were subject to corrosion, producing a hydrogen sulfide concentration in the immediately adjacent liquid. Recommendations included changing the valve material to type 304 stainless steel.

Socket head cap screws used in a naval application were failing in service due to delayed fracture. The standard ASTM A 574 screws were zinc plated and dichromate coated. Investigation (visual inspection, 1187 SEM images, chemical analysis, and tension testing) of both the failed screws and two unused, exemplar fasteners from the same lot supported the conclusion that the cap screws appear to have failed due to hydrogen embrittlement, as revealed by delayed cracking and intergranular fracture morphology. Static brittle overload fracture occurred due to the tension preload, and prior hydrogen charging that occurred during manufacturing. The probable source of charging was the electroplating, although postplating baking was reportedly performed as well. Recommendations included examining the manufacturing process in detail.

During a routine inspection, cracks were discovered in several aluminum alloy (similar to either 2014 or 2017) coupling nuts on the fuel lines of a missile. The fuel lines had been exposed to a marine atmosphere for six months while the missile stood on an outdoor test stand near the seacoast. A complete check was then made, both visually and with the aid of a low-power magnifying glass, of all coupling nuts of this type on the missile. Investigation (visual inspection, spectrographic and chemical analysis, and metallographic examination) supported the conclusion that the cracking of the aluminum alloy coupling nuts was caused by stress corrosion. Contributing factors included use of a material that is susceptible to this type of failure, sustained tensile stressing in the presence of a marine (chloride-bearing) atmosphere, and an elongated grain structure transverse to the direction of stress. The elongated grain structure transverse to the direction of stress was a consequence of following the generally used procedure of machining this type of nut from bar stock. Recommendations included changing the materials specification for new coupling nuts for this application to permit use of only aluminum alloys 6061-T6 and T651 and 2024-T6, T62, and T851.

Plate perforation occurred in the cylindrical section and walls of the inlet foot (2.38 mm thick Incoloy 825 plate welded using INCO welding rod 135) of an inert gas fire prevention system in an oil tanker. Cross-sectional microprobe analysis showed the corrosion product to contain sulfur, mainly from the flue gas, and calcium and chlorine, mainly from the sea water. The gray corrosion product was interspersed with rust and a black carbonaceous deposit. Corrosion pitting and poor weld penetration, with carbide precipitation and heavy etching at grain boundaries, indicated sensitization and susceptibility to aqueous intergranular corrosion. Chemical analysis showed the predominant acid radical to be sulfate (6.20% in the carbonaceous deposit and 0.60% in the corrosion product), suggesting that oxidation of SO2 in the flue gas caused the corrosion. Moisture condensation, the carbon acting as a cathode, and alloy susceptibility to intergranular corrosion contributed to the corrosion.

Several glass wool insulation sections from a heat-treat furnace showed visible, but only cosmetic discoloration. EDS showed the presence of silicon, aluminum, and oxygen in the nondiscolored region, and these elements are consistent with glass wool. Relatively high levels of chromium and nickel were detected in the discolored area, along with lower amounts of iron, manganese, sodium, calcium, cobalt, and sulfur, in addition to the surrounding glass wool elements. Results of this limited evaluation showed the discoloration was caused by the presence of elevated levels of chromium, nickel, and aluminum. The visual appearance, along with the EDS findings, suggested these elements were present in the form of oxides. These oxides were likely deposited from adjacent structural components of the furnace, which had oxidized during operation.

One of 14 vertical radiant tubes (RA 333 alloy) in a heat-treating furnace failed when a hole about 5 x 12.5 cm (2 x 5 in.) corroded completely through the tube wall. The tube measured 183 cm (72 in.) in length and 8.9 cm (3 in.) in OD and had a wall thickness of about 3 mm (0.120 in.). Failure occurred where the tube passed through the refractory hearth (floor) of the furnace. Although the furnace atmosphere was neutral with respect to the work, it had a carburizing potential relative to the radiant tubes. Analysis (visual inspection, 250x spectroscopic examination of specimens etched with mixed acids, metallographic examination, and chemical analysis) supported the conclusions that the premature failure of the tube by perforation at the hearth level resulted from (1) corrosion caused by sulfur contamination from the refractory cement in contact with the tube and (2) severe local overheating at the same location. Recommendations included replacing all tubes using a low sulfur refractory cement in installation and controlling burner positioning and regulation more closely to avoid excessive heat input at the hearth level.

Over a period of about one year, three RA 330 alloy salt pots from a single heat-treating plant were submitted to failure analysis. All of the pots, which had 9.5 mm thick walls, were used primarily to contain neutral salts at temperatures from about 815 to 900 deg C (1500 to 1650 deg F). However, some cyaniding was also performed in these pots, which, when not in use, were idled at 760 deg C (1400 deg F). It was reported that sludge was removed from the bottom of the pots once a day. Normal pot life varied from about 6 to 20 months. The pots were removed from the furnace, visually inspected, and rotated 120 deg every three weeks to ensure that no single location was overheated for a prolonged period of time. Analysis (visual inspection, chemical analysis, metallographic examination, and x-ray analysis, 60x micrograph etched with 10% oxalic acid) supported the conclusion that the cause of failure of each of the three salt pots was severe intergranular corrosion accompanied by substantial chromium depletion. No recommendations were made.

A flat spring for the main landing gear of a light aircraft failed after safe execution of a hard landing. The spring material was identified by chemical analysis to be 6150 steel. The fracture was found to have occurred near the end of the spring that was inserted through a support member about 25 mm thick and attached to the fuselage by a single bolt. Brinelling (plastic flow and indentation due to excessive localized contact pressure) was observed on the upper surface of the spring where the forward and rear edges of the spring contacted the support member. It was indicated by chevron marks that brittle fracture had started beneath the brinelled area at the forward edge of the upper surface of the spring. The origin of the brittle fracture was found to be a small fatigue crack that had been present for a considerable period of time before final fracture occurred. Fracture of the landing-gear spring was concluded to have been caused by a fatigue crack that resulted from excessive brinelling at the support point. Regular visual examinations to detect evidence of brinelling and wear at the support in aircraft with this configuration of landing-gear spring were recommended.

A hollow, splined alloy steel aircraft shaft (machined from an AMS 6415 steel forging – approximately the same composition as 4340 steel – then quenched and tempered to a hardness of 44.5 to 49 HRC) cracked in service after more than 10,000 h of flight time. The inner surface of the hollow shaft was exposed to hydraulic oil at temperatures of 0 to 80 deg C (30 to 180 deg F). Analysis (visual inspection, 15-30x low magnification examination, 4x light fractograph, chemical analysis, hardness testing) supported the conclusions that the shaft cracked in a region subjected to severe static radial, cyclic torsional, and cyclic bending loads. Cracking originated at corrosion pits on the smoothly finished surface and propagated as multiple small corrosion-fatigue cracks from separate nuclei. The originally noncorrosive environment (hydraulic oil) became corrosive in service because of the introduction of water into the oil. Recommendations included taking additional precautions in operation and maintenance to prevent the use of oil containing any water through filling spouts or air vents. Also, polishing to remove pitting corrosion (but staying within specified dimensional tolerances) was recommended as a standard maintenance procedure for shafts with long service lives.

During a routine inspection on an aircraft assembly line, an airframe attachment bolt was found to be broken. The bolt was one of 12 that attach the lower outboard longeron to the wing carry-through structure. Failure occurred on the right-hand forward bolt in this longeron splice attachment. The bolt was fabricated from PH13-8Mo stainless steel heat treated to have an ultimate tensile strength of 1517 to 1655 MPa (220 to 240 ksi). A water-soluble coolant was used in drilling the bolt hole where this fastener was inserted. Investigation (visual inspection, 265 SEM images, hardness testing, auger emission spectroscopy and secondary imaging spectroscopy, tensile testing, and chemical analysis) supported the conclusion that failure of the attachment bolt was caused by stress corrosion. The source of the corrosive media was the water-soluble coolant used in boring the bolt holes. Recommendations included inspecting for corrosion all the bolts that were installed using the water-soluble coolant at the spliced joint areas, rinsing all machined bolt holes with a noncorrosive agent, and installing new PH13-8Mo stainless steel bolts with a polysulfide wet sealant.

Military aircraft use a cartridge ignition system for emergency engine starts. Analysis of premature failures of steel (AISI 4340) breech chambers in which the solid propellant cartridges were burned identified corrosion as one problem with an indication that stress-corrosion cracking may have occurred. A study was made for stress-corrosion cracking susceptibility of 4340 steel in a paste made of the residues collected from used breech chambers. The constant extension rate test (CERT) technique was employed and SCC susceptibility was demonstrated. The residues, which contained both combustion products from the cartridges and corrosion products from the chamber, were analyzed using elemental analysis and x-ray diffraction techniques. Electrochemical polarization techniques were also utilized to estimate corrosion rates.

The purpose of this investigation was to determine the cause of the ultrasonic signal attenuation noted during an inspection of a composite aircraft component. Although ultrasonics was able to identify the location of the defective areas, destructive analysis had to be utilized to determine the exact nature of the defect. The investigation describes how cross-sectioning, fractography, and chemical analysis were utilized to determine the type of defect responsible for the signal attenuation.

Helicopter rotor blade components that included the horizontal hinge pin, the associated nut, and the locking washer were examined. Visual examination of the submitted parts revealed that the hinge pin, fabricated from 4340 steel, was broken and that the fracture face showed a flat beach mark pattern indicative of a preexisting crack. The threaded area of the pin had an embedded thread that did not appear to come from the pin. A chemical analysis was conducted on the embedded thread and on an associated attachment to determine the origin of the thread. Analysis showed that the thread and nut were 4140 steel. Scanning electron fractographic examination of the fracture initiation site strongly suggested that the fracture progressed by fatigue. It was concluded that the failure of the horizontal hinge pin initiated at areas of localized corrosion pits. The pits in turn initiated fatigue cracks, resulting in a failure mode of corrosion fatigue. It was recommended that all of the horizontal hinge pins be inspected. Those pins determined to be satisfactory for further use should be stripped of cadmium, shot peened, and coated with cadmium to a minimum thickness of 0.0127 mm (0.0005 in.).