Initially, two vertical double-acting two-stage compressors delivering chlorine gas at a pressure of 100 psi appeared to be running satisfactorily. About six months later the LP piston-rod of the No. 2 compressor failed due to burning, the compressor being worked double-acting at the time. About five months later, the HP piston rod of the No. 1 compressor failed in a similar manner. Specimens for microscopic examination were cut from the rod in the region of the failure and from the extreme end that had been situated above the piston and hence not subjected to an appreciable rise in temperature. The material was a steel in the normalized condition with a 0.35% C content. It appears probable that deficient lubrication of the gland resulted in overheating of the rod due to friction. The presence of a sprayed-metal coating was probably an additional factor in promoting failure, as it would present to the gas a surface area considerably greater than that of a homogeneous material.

The thin plates within a type 309 stainless steel chlorinated solvent combustion preheater/heat exchanger designed to process fumes from a solvent coating process showed severe corrosion within 6 months of service. Within a year corrosion had produced holes in the plates, allowing gases to shunt across the preheater/exchanger. Metallographic examination of the plates showed that accelerated internal oxidation had been the cause of failure. Corrosion racks of candidate alloys (types 304, 309, and 316 stainless steels, Inconel 600, Inconel 625, Incoloy 800, Incoloy 825, and Inco alloy C-276) were placed directly in the hot gas stream, containing HCl and Cl2, for in situ testing. Results of this investigation showed that nickel-chromium corrosion-resistant alloys, such as Inconel 600, Inconel 625, and Inco alloy C-276, performed well in this environment. Laboratory testing of the same alloys, along with Inconel alloys 601, 617, and 690 and stainless steel type 347 was also conducted in a simulated waste incinerator nitrogen atmosphere containing 10% Co2, 9% O2, 4% HCl, 130 ppm HBr and 100 ppm SO2 at 595, 705, 815, and 925 deg C (1100, 1300,1500, and 1700 deg F). The tests confirmed the suitability of the nickel-chromium alloys for such an environment. Inconel 625 was selected for fabrication of a new preheater/exchanger.

A tie rod, nut, and bellows from a failed 610 mm (24 in.) diam tied universal expansion joint that carried tail gases consisting of N 2 + O 2 with slight traces of nitrogen oxides and water were examined. The materials were SA 193-B7 (AISI 4140), SA 194–214, and Incoloy 800H, respectively. Visual examination of the bellows revealed cracks in heavily cold-worked areas (both inside and outside) and considerable corrosion. SEM analysis showed a classical intergranular failure pattern with microcracking. The threaded tie rod microstructure contained spheroidized carbide that was more pronounced at the tie rod end of the failure. Energy-dispersive X-ray analysis of fracture surfaces from the bellows showed the presence of chlorine and sulfur. Failure of the bellows was attributed to stress-corrosion cracking, with chlorine and sulfur being the corroding agents. The rod damage was the result of failure of the bellows, which allowed escaping hot gases to impinge on the tie rods and heat them to approximately 595 deg C (1100 deg F). It was recommended that the insulation be analyzed to determine the origin of the chlorine and sulfur and that it be replaced if necessary.

Catastrophic pitting corrosion occurred in type 304L stainless steel pipe flange assemblies in an industrial food processor. During regular service the pumped medium was pureed vegetables. In situ maintenance procedures included cleaning of the assemblies with a sodium hypochlorite solution. It was determined that the assemblies failed due to an austenite-martensite galvanic couple activated by a chlorine bearing electrolyte. The martensitic areas resulted from a transformation during cold-forming operations. Solution annealing after forming, revision of the design of the pipe flange assemblies to eliminate the forming operation, and removal of the source of chlorine were recommended.

Problems with materials compatibility were encountered in pyrotechnically driven devices used in a number of ordnance applications requiring rapid mechanical actuation. A fine bridgewire is located in contact with the chemical pyrotechnic, and the charge is ignited by electrical heating of the bridgewire. Evidence of severe corrosion was revealed on examination of the nickel-chromium-iron alloy bridgewire and the nickel-iron alloy pins. Metallic elements in the pin or bridgewire and substantial amounts of chlorine were detected from the x-ray spectra. Morphological changes indicative of decomposition and dissolution were revealed to have occurred in regions of the pyrotechnic that had been in contact with the bridgewire and pin surfaces by examination of the titanium-potassium perchlorate (Ti-K-Cl-O4) pyrotechnic. Substantial amounts of water were revealed to be associated with the surfaces of the titanium particles in the pyrotechnic by nuclear magnetic resonance. It was proposed that the chlorine-containing residue combined with the water from the pyrotechnic to form a thin aqueous film corroding the bridgewire and pins. A new cleaning procedure was implemented for the glass headers to eliminate the chloride contamination and a vacuum drying procedure was instituted for the pyrotechnic.

One of three valves in a dry automatic sprinkler system tripped accidentally, thus activating the sprinklers. Maintenance records showed that the three valves had been in service less than two years. The valve consisted of a cast copper alloy clapper plate that was held closed by a pivoted malleable iron latch. The latch and top surface of the clapper plate were usually in a sanitary-water environment (stabilized, chlorinated well water with a pH of 7.3) under stagnant conditions. Process make-up water that had been clarified, filtered, softened, and chlorinated and had a pH of 9.8 was occasionally used in the system. Analysis (visual inspection and 250x micrograph) supported the conclusions that failure of the latch was caused by plastic deformation from extensive loss of metal by galvanic corrosion and the sudden loading related to the tripping of the valve. Failure in some regions of the contact area was by ductile (transgranular) fracture. Recommendations included changing the latch material from malleable iron to silicon bronze (C87300). The use of silicon bronze prevents corrosion or galvanic attack and proper adjustment of the latch maintains an adequate contact area.

A cast silicon bronze (UNS C86700) impeller that had been severely corroded was submitted for failure analysis. The failed part was used to pump potable water, but service life and chlorine content of the water were unknown. The impeller displayed a Cu-rich red phase on its surfaces and showed a pattern very similar to dezincification. Further investigation to determine the cause of damage using light microscopy and SEM-EDS techniques revealed that the microstructure consisted of multiple phases and that a Si-rich phase was being preferentially attacked, leading to increased porosity. After a thorough examination, it was concluded that the part had failed due to dealloying via desiliconification.

A bent Ni-Cu Monel 400 alloy tube, which operated as part of a pipeline in a petrochemical distillery, failed by through-thickness cracking. The pipeline was used to carry a stream of gaseous hydrocarbons containing hydrochloric acid (HCl) into a reaction tower. The tower provided a caustic solution (NaOH) to remove HCl from the stream, before the latter was directed to a burner. Metallographic examination showed that the cracks were intergranular and were frequently branched. Although nominal chemical composition of the component was found within the specified range, energy dispersive x-ray analysis (EDXA) indicated significant segregation of sulfur and chlorine along the grain boundaries. Failure was attributed to hypochlorous-acid (HClO)-induced stress-corrosion cracking (SCC). The HClO was formed by the reaction of HCl with atmospheric O 2 that entered the tube during shutdowns and startups. Residual stresses, originating from in situ bend forming of the tube during assembly of the line, provided a driving force for crack growth, and the segregation of sulfur on grain boundaries made the material more susceptible to cracking.

Radial cracking occurred adjacent to 11 vanes in a 19-vane impeller operating in a chemical plant environment. The impeller vanes were fillet welded to both the disk and the cover Cracks were next to the fillet welds and near the cover outer diameter They generally did not extend to the outer diameter. The entire impeller surface was tested by the dry magnetic particle method. Visual and microstructural examinations revealed intergranular cracking. Energy-dispersive spectroscopy of corrosion products contained in the cracks disclosed the presence of chlorine and sulfur The failure was attributed to stress-corrosion cracking caused by a corrosive atmosphere.

Six ASTM A-574 steel cap screws from a hydraulic coupling failed after 3 months in service. The screws were replacements for smaller-diameter cap screws that had been installed during an outage. Six new cap screws were examined along with the failed screws. Eight fracture locations were identified—three at the head-to-shank fillet, four at the eighth thread root from the cap, and one at the sixth thread root from the cap. Fracture surfaces were examined using a stereomicroscope and SEM, and the fracture mode was shown to be transgranular. EDS on the fracture surfaces showed sulfur and chlorine in the surface deposits. The observations indicated that the screws had failed by fatigue. Insufficient preloading was considered to be the most likely cause of the fatigue cracking. It was recommended that the proper preload on the screws be verified and maintained.

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.

Severe pitting was found on the internal surfaces of SA-210 Grade C waterwall tubing of a coal-fired boiler at a cogeneration facility. Metallographic examination showed the pits to be elliptical, having an undercut morphology with supersurface extensions,. a type of pitting characteristic of acidic attack. Energy-dispersive X-ray spectroscope revealed the presence of chlorine in the pit deposits, indicating that the pitting was promoted by underdeposit chloride attack. The presence of copper in deposits on the internal surface of the tubing may have acted as a secondary factor. Acidic conditions may have formed during a low-pH excursion that reportedly occurred several years prior. To prevent future failures, severely damaged tubing must be replaced. Internal deposit buildup must be removed by chemical cleaning to prevent further pitting. Water quality needs continued monitoring and maintenance to ensure that another low-pH excursion does not occur.

A type 321 stainless steel downcomer expansion joint that handled process gases was found to be leaking approximately 2 to 3 weeks after installation. The expansion joint was the second such coupling placed in the plant after failure of the original bellows. The failed joint was disassembled and examined to determine the cause of failure. Energy-dispersive x-ray analysis revealed significant peaks for chlorine and phosphorus, indicating failure by chloride stress-corrosion cracking (SCC). Cracks in the liner and bellows exhibited a branched pattern also typical of SCC. Cracks through the inner liner initiated on the outer surface of the liner and propagated inward, whereas cracks in the bellows originated on the inner surface and propagated outward. Stress-corrosion cracking of the assembly was caused by chloride contaminants trapped inside the bellows following hydrostatic testing. Checking the test fluid for chloride and removing all fluids after hydrostatic testing were recommended to prevent further failure.

An investigation of the impeller and deposit samples from a centrifugal compressor revealed that an aluminum IR-12 refrigerant reaction had occurred, causing extensive damage to the second-stage impeller and contaminating the internal compressor components. The spherical surface morphology of the impeller fragments suggested that the aluminum had melted and resolidified. The deposits were similar in composition and were identified by XRD as consisting primarily of aluminum trifluoride. In addition, EDS analysis detected major amounts of chlorine and iron. Results of a combustion test indicated that the compressor deposit was comprised of a 9. 8 wt% carbon and that the condenser deposit contained 8.7 wt% carbon. It was concluded that the primary cause of failure was the rubbing of the impeller against the casting and that a self-sustaining Freon fire had occurred in the failed compressor

Leakage was identified around a coupling welded into a stainless steel holding tank that stored condensate water with low impurity content. The tank and fitting were manufactured from type 304 stainless steel. The coupling joint consisted of an internal groove weld and an external fillet weld. Cracking was found to be apparent on the tank surface, adjacent to the coupling weld. Chlorine, carbon, and oxygen in addition to the base metal elements were revealed by energy-dispersive x-ray spectrometric analysis. A great number of secondary, branching cracks were evident in the weld, heat-affected zone, and base metal. The branching and transgranular cracking was found to emanate primarily from the exterior of the tank. It was concluded that the tank failed as a result of stress-corrosion cracking that initiated at the exterior surface as aqueous chlorides, especially within an acidic environment, have been shown to cause SCC in austenitic stainless steels under tensile stress.