A flanged 100 mm (4 in.) diam low-carbon steel spool piece lined with Teflon was removed from a sulfuric acid denitrification system after cracks were observed in the painted coating. Visual and microstructural examination along with SEM fractography revealed scaled iron oxides on all opened crack surfaces. The surfaces had a faceted morphology, indicating intergranular fracture. Cracks originated at the interface between the tube and the Teflon liner Corrosion products were found caked into the intergranular region between the liner and the spool. The portion of the liner that had been exposed to the process stream was discolored. Failure of the spool was attributed to stress-corrosion cracking promoted by the presence of nitrates. Nitric acid contaminant in the sulfuric acid stream had diffused through the liner and accumulated in the annular space. Use of a liner that is more impermeable to the diffusion of ionic species was recommended.

A gray cast iron (ASTM 247 type A) gate valve in an oleum and sulfuric acid piping loop at a chemical process plant fractured catastrophically after approximately 10 years of service. The valve was a 150 mm (6 in.) bolted flange type rated to conform to ANSI B16.1 for service at 1034 kPa (150 psi) and 120 deg C (250 deg F) maximum in 93 to 99% sulfuric acid. The fracture originated at stress-corrosion cracks that occurred in a high-stress transition region at the valve body-to-flange juncture. The mechanical properties of the failed valve were below those of the manufacturer's cited specification, and the wall thickness through which the fracture occurred exceeded the minimum 9.5 mm (38 in.) thickness cited by the manufacturer The valve flange had been unbolted and rebolted to a maintenanced piping coil immediately prior to failure. It was recommended that the flange-to-valve body juncture be redesigned to reduce stress levels. A method of maintenance and inspection in concert with a criterion for life prediction for this and other valves and components in the system was also recommended.

A cold-formed Grade TP 304 stainless steel swaged region of a reheater tube in service for about 8000 hours cracked because of sulfur-induced stress-corrosion cracking (SCC). Cracking initiated from the external surface and a high sulfur content was detected in the outer diameter and crack deposits. Comparison of the microstructure and hardness of the swaged region and unswaged Grade TP 304 stainless steel tube metal indicated that the swaged section was not annealed to reduce the effects of cold working. The high hardness created during swaging increased the stainless steel's susceptibility to sulfur-induced SCC. Because SCC requires water to be present, cracking most likely occurred during downtime or startups. To prevent future failures, the boiler should be kept dry during downtime to avoid formation of sulfur acids, and the swaged sections of the tubes should be heat treated after swaging to reduce or eliminate strain hardening of the metal.

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.

Although field corrosion tests had indicated that type 316L stainless steel would be a suitable material for neutralization tanks, the vessels suffered severe corrosion when placed in service. Welded coupons of type 316L had been tested along with similar Alloy 20Cb® (UNS NO8020) specimens in a lead-lined tank equipped with copper coils that had served in this function prior to construction of the new tanks. Both materials exhibited virtually no corrosion and no preferential weld attack. Type 316L was selected for the project. The subsequent corrosion was the result of the borderline passivity of type 316L in hot dilute sulfuric acid (about 0.1%). Inaccuracy of the testing was attributed to the presence of cupric ions in the lead-lined vessel fluids, which had been released by corrosion of the copper coils. Careful control of both temperature and pH was recommended to reduce the corrosion to an acceptable limit.

The interior of a cylindrical tank used for the road transport of concentrated sulfuric acid revealed severe blistering of the plates, mainly over the crown and more particularly on the first ring. The tank, made in 1958, was of welded construction, the material being mild steel plate. Some of the blisters were pierced by drilling a hole in the center and at the same time applying a small flame. In several cases combustion of the escaping gas caused minor explosions, a result characteristic of hydrogen. Etching showed the material to be a low-carbon steel in the partly spheroidized condition. There was no evidence of cracking of the material in the region of the blisters and bend tests demonstrated it possessed satisfactory ductility. The primary cause of the blistering was ascribed to the presence of discontinuities within the plate. This provided cavities in which the hydrogen was able to accumulate and build up pressure. Had the material been free from discontinuities of appreciable size, the blistering would not have occurred.

Alloy 430 stainless steel tube-to-header welds failed in a heat recovery steam generator (HRSG) within one year of commissioning. The HRSG was in a combined cycle, gas-fired, combustion turbine electric power plant. Alloy 430, a 17% Cr ferritic stainless steel, was selected because of its resistance to chloride and sulfuric acid dewpoint corrosion under conditions potentially present in the HRSG low-pressure feedwater economizer. Intergranular corrosion and cracking were found in the weld metal and heat-affected zones. The hardness in these regions was up to 35 HRC, and the weld had received a postweld heat treatment (PWHT). Metallographic examination revealed that the corroded areas contained undertempered martensite. Fully tempered weld areas with a hardness of 93 HRB were not attacked. No evidence of corrosion fatigue was found. Uneven temperature control during PWHT was the most likely cause of failure.

A steam heated exchanger was designed for concentrating sulfuric acid. Tantalum was selected for the tubing and the tube sheet liner because of its outstanding corrosion resistance. However, although the exchanger passed a searching shop inspection, it leaked during site testing. Considerable argument ensued about whether the cracking observed was due to poor welding during fabrication, or through abuse during handling on site. An SEM examination of the fractures revealed high cycle, low amplitude fatigue, and the problem was traced to vibration during road transport. Further failures were avoided by improved design and packing. This paper illustrated the value of SEM fractography when a rapid investigation is needed under the pressures of a fast moving project.

A 1-in. diam pump spindle fractured within the length covered by the boss of the impeller which was attached to the spindle by means of an axial screw. The pump had been in use in a chemical plant handling mixtures of organic liquids and dilute sulfuric acid having a pH value of 2 to 4 at temperatures of 80 to 90 deg C (176 to 194 deg F). The fracture was unusual in that it was of a fibrous nature, the fibers-which were orientated radially-were readily detachable. The surface of the spindle adjacent to the fracture had an etched appearance and the mode of cracking in this region suggested that failure resulted from an intergranular attack. Subsequent microscope examination confirmed the generally intergranular mode of failure. A macro-etched section near the fracture revealed a radial arrangement of columnar crystals, indicating that the spindle was a cast and not a wrought product as had been presumed. Spectroscope examination showed this particular composition (Fe-23Cr-18Ni-1.8Mo-1.2Si) did not conform to a standard specification and is apparently a proprietary alloy. It was evident that the particular mode of failure was related to the inherent structure of the material.

Forged aluminum alloy 2014-T6 hinge brackets in naval aircraft rudder and aileron linkages were found cracked in service. The cracks were in the hinge lugs, adjacent to a bushing made of cadmium-plated 4130 steel. Investigation (visual inspection and 250X micrographs) supported the conclusion that the failure of the hinge brackets occurred by SCC. The corrosion was caused by exposure to a marine environment in the absence of paint in stressed areas due to chipping. The stress resulted from the interference fit of the bushing in the lug hole. Recommendations included inspecting all hinge brackets in service for cracks and for proper maintenance of paint. Also suggested was replacing the aluminum alloy 2015-T6 with alloy 7075-T6, and surface treatment for the 7075-T6 brackets was recommended using sulfuric acid anodizing and dichromate sealing. Finally, it was also recommended that the interference fit of the bushing in the lug hole be discontinued.

During a routine shear-pin check, the end lug on the barrel of the forward canopy actuator on a naval aircraft was found to have fractured. The lug was forged from aluminum alloy 2014-T6. Investigation (visual inspection, 2x views, and 140X micrographs etched with Keller's reagent) supported the conclusion that the cause of failure was SCC resulting from exposure to a marine environment. The fracture occurred in normal operation at a point where damage from pitting and intergranular corrosion acted as a stress raiser, not because of overload. The pitting and intergranular attack on the lug were evidence that the surface protection of the part had been inadequate as manufactured or had been damaged in service and not properly repaired in routine maintenance. Recommendations included anodizing the lug and barrel in sulfuric acid and giving them a dichromate sealing treatment, followed by application of a coat of paint primer. During routine maintenance checks, a careful examination was suggested to look for damage to the protective coating, and any necessary repairs should be made by cleaning, priming, and painting. Severely corroded parts should be removed from service.

Examination of a connecting-rod shell bearing from a six-cylinder gasoline engine was done after it was returned to the factory. Copper-lead alloy SAE 485 bonded to a low-carbon steel backing was used to make the bearing and the oil used in the engine was the recommended one. Measurable material loss was visible over most of the bearing halves particularly in a wide region at the centerline. A brittle waxlike substance identified to be a mixture of copper and lead sulfides covered the visible shallow pits and the darkened region. Change of oil with greater frequency to prevent the buildup of sulfur compounds or bearing halves that have corrosion-resistant overlay materials were recommended as best solutions.