Eddy current inspection was performed on a vertical evaporator unit (that contained 180 tubes) used in a chemical processing plant. It was advised that the tube material was type 316 stainless steel. The shell-side fluid was condensate and gaseous methylene chloride, while the tube-side fluid was contaminated liquid methylene chloride. More than 100 tubes exhibiting severe outer surface pitting and cracklike indications near each tube sheet were revealed during eddy current inspection. It was observed that the indications correlated with rust-stained, pitted, and cracked areas on the outer surfaces. The cracking was revealed by metallographic examination to have initiated from the outer surface, frequently at pits, and penetrated the tube wall in a transgranular, branching fashion. The crack features were characteristic of chloride stress-corrosion cracking. A change in tube material was recommended to avoid future failures and loss of service.

A substantial number of copper alloy C27000 (yellow brass, 65Cu-35Zn) ferrules for electrical fuses cracked while in storage and while in service in paper mills and other chemical processing plants. The ferrules, made by three different manufacturers, were of several sizes. One commonly used ferrule was 3.5 cm long by 7.5 cm in diam and was drawn from 0.5 mm (0.020 in.) thick strip. Investigation (visual inspection, metallographic examination, and a mercurous nitrate test, which is an accelerated test used to detect residual stress in copper and copper alloys) of both ferrules from fuses in service and storage in different types of plants, and ferrules from newly manufactured fuses, supported the conclusion that the ferrules failed by SCC resulting from residual stresses induced during forming and the ambient atmospheres in the chemical plants. The atmosphere in the paper mills was the most detrimental, and the higher incidence of cracking of ferrules there was apparently related to a higher concentration of ammonia in conjunction with high humidity. Recommendations included specifying that the fuses meet the requirements of ASTM B 154.

One of five underground drain lines intended to carry a highly acidic effluent from a chemical-processing plant to distant holding tanks failed in just a few months. Each line was made of 304L stainless steel pipe 73 mm (2 in.) in diam with a 5 mm (0.203 in.) wall thickness. Lengths of pipe were joined by shielded metal arc welding. Soundness of the welded joints was determined by water back-pressure testing after several lengths of pipe had been installed and joined. Before completion of the pipeline, a pressure drop was observed during back-pressure testing. An extreme depression in the backfill revealed the site of failure. Analysis (visual inspection, electrical conductivity, and soil analysis) supported the conclusions that the failure had resulted from galvanic corrosion at a point where the corrosivity of the soil was substantially greater than the average, resulting in a voltage decrease near the point of failure of about 1.3 to 1.7 V. Recommendations included that the pipelines be asphalt coated and enclosed in a concrete trough with a concrete cover. Also, magnesium anodes, connected electrically to each line, should be installed at periodic intervals along their entire length to provide cathodic protection.

Weld-decay and stress-corrosion cracking developed in several similar all-welded vessels fabricated from austenitic stainless steel. During a periodic examination cracks were revealed at the external surface of one of the vessels. External patch welds had been applied at these and several other corresponding locations. Cracks visible on the external surface developed from the inside in a region close to the toe of the internal fillet weld to the deflector plate, and another deep crack associated with a weld cavity is visible slightly to the right of the main fissure. Microscopic examination revealed that precipitation of carbides at the grain boundaries had taken place in the vicinity of the cracks, but that the paths of the cracks were not wholly intergranular. Conditions present in the vicinity of the internal fillet weld must have been such as to favor both inter- and transgranular cracking. It is probable that the heating associated with the repair welds made from time to time also contributed to the trouble. The transgranular cracks, however, were indicative of stress-corrosion cracking.

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.

Several tubes in a 35 m 2 (115 ft 2 ) type 316 stainless steel shell-and-tube condenser leaked unexpectedly in an organic chemical plant that produces vinyl acetate monomer. Leaks were discovered after 5 years of operation and relocation of the condenser to another unit in the same plant. Examination of tubes and tube sheets revealed pitting damage on the OD surface. Some of the pits had penetrated fully, resulting in holes. Inside diameter surfaces were free of corrosion. Macro- and microexaminations indicated that the tubes had been properly manufactured. Pitting was attributed to stagnant water on the shell side. It was recommended that the surfaces not be kept in contacts with closed stagnant water for appreciable lengths of time.

A heat exchanger failed five years after going into service in an ammonia synthesis plant. Its container, made of Cr-Mo alloy steel (Material No. 1.7362), operated in an environment that did not exceed 400 deg C or 600 atm of hydrogen partial pressure. X-ray examination revealed a fissure in one of the welded seams, which according to microscopic examination, originated in the base material of the container. Higher magnification revealed a narrow zone adjacent to the weld seam permeated with intergranular cracks, the result of hydrogen attack. It also showed the structure to be completely martensitic. Thus, the failure was due to hardening of the base material during welding, and recommendation was made to temper or anneal the welded regions to reduce the effects of hydrogen under pressure.

Unalloyed steels and the pure nickel steels frequently used in the past can sustain significant damage from hydrogen attack in ammoniacal environments. The attack causes decarburization that leads to a loosening of the structure due to the precipitation of methane along grain boundaries. It occurs between 200 and 300 deg C, depending on hydrogen pressure. Parts of an apparatus that operate in these types of environments must be checked constantly if they are not made from hydrogen-resistant steel. The results of two such examinations serve to illustrate the challenges.

After about four years of service, cracks appeared on the internal or process-side surfaces of four evaporator pans in a sugar concentrator. The pans consisted of a Mo stabilized austenitic stainless steel inner vessel surrounded by a mild steel steam jacket. Corrosion of the external surface had taken place in the form of confluent pitting over a band adjacent to the fillet weld which attached the pan to the blocking ring. Numerous cracks were present in this corroded zone. Microscopical examination of several specimens cut from the sample revealed that the internal cracks in the pan itself originated from the external side of the plate, i.e. from the region covered by the shrouding ring. They were predominantly of the transgranular type. Because the cracks were not of the intergranular type as usually found with weld decay, they were considered to be indicative of stress-corrosion cracking. Stresses responsible for the cracking resulted from weld contraction. The pans had been hosed down periodically with water from local boreholes to remove sugar from the external surfaces, which introduced the corrosive medium.

A 680,000 kg (750 ton) per day ammonia unit was shut down following a fire near the outlet of the waste heat exchanger. The fire had resulted from leakage of ammonia from the type 316 stainless steel outlet piping. The outlet piping immediately downstream from the waste heat exchanger consisted of a flange made from a casting, and a reducing cone, a short length of pipe, and a 90 deg elbow, all made of 13 mm thick plate. A liner wrapped with insulation was welded to the smaller end of the reducing cone. All of the piping up to the flange was wrapped with insulation. Investigation (visual inspection, 10x unetched images, liquid-penetrant inspection, and chemical analysis of the insulation) supported the conclusion that the failure occurred in the area of the flange-to-cone weld by SCC as the result of aqueous chlorides leached from the insulation around the liner by condensate. Recommendations included eliminating the chlorides from the system, maintaining the temperature of the outlet stream above the dewpoint at all times, or that replacing the type 316 stainless steel with an alloy such as Incoloy 800 that is more resistant to chloride attack.

A cooler of an ammonia synthesis plant was destroyed after three years of service due to the rupture of a distribution manifold. Synthesis gas under high pressure and at about 300 deg C, consisting of 10% NH3 and unconverted gas of 25% N2 and 75% H2 content, was water-cooled externally to room temperature in this unit. The fracture had the typical flat-gray fibrous structure of a material destroyed by hydrogen. Specimens for the metallographic investigation showed that the structure appeared to have been loosened by intergranular separations. DVM notched impact specimens from the affected area yielded low specific impact energy values. These are the significant characteristics of hydrogen attack. The attack penetrated to a depth of 13 to 16 mm. It was recommended that the manifolds be made of hydrogen-resistant steel instead of the unalloyed steel used.

Handles welded to the top cover plate of a chemical-plant downcomer broke at the welds when the handles were used to lift the cover. The handles were fabricated of low-carbon steel rod; the cover was of type 502 stainless steel plate. The attachment welds were made with type 347 stainless steel filler metal to form a fillet between the handle and the cover. The structure was found to contain a zone of brittle martensite in the portion of the weld adjacent to the low-carbon steel handle; fracture had occurred in this zone. The brittle martensite layer in the weld was the result of using too large a welding rod and too much heat input, melting of the low-carbon steel handle, which diluted the austenitic stainless steel filler metal and formed martensitic steel in the weld zone. Because it was impractical to preheat and postheat the type 502 stainless steel cover plate, the low-carbon steel handle was welded to low-carbon steel plate, using low-carbon steel electrodes. This plate was then welded to the type 502 stainless steel plate with type 310 stainless steel electrodes. This design produced a large weld section over which the load was distributed.

Tube sheets (found to be copper alloy C46400, or naval brass, and 5 cm (2 in.) thick) of an air compressor aftercooler were found to be cracked and leaking approximately 12 to 14 months after they had been retubed. Most of the tube sheets had been retubed several times previously because of unrelated tube failures. Sanitary (chlorinated) well water was generally used in the system, although filtered process make-up water (river water) containing ammonia was occasionally used. Investigation (visual inspection, chemical analysis, mercurous nitrate testing, unetched 5X micrographs, and 250X micrographs etched in 10% ammonium persulfate solution) supported the conclusion that the tube sheets failed by SCC as a result of the combined action of internal stresses and a corrosive environment. The internal stresses had been induced by retubing operations, and the environment had become corrosive when ammonia was introduced into the system by the occasional use of process make-up water. Recommendations included making a standard procedure to stress relieve tube sheets before each retubing operation. The stress relieving should be done by heating at 275 deg C (525 deg F) for 30 min and slowly cooling for 3 h to room temperature.

Several cadmium-plated carbon steel socket head cap screws that were part of a slide valve assembly on a regenerator line in a petrochemical plant failed during initial loading. Metallographic and XDS chemical analysis in conjunction with SEM examination of one failed and one unfailed cap screw indicated that the screws had failed by hydrogen embrittlement. The plating process was the likely source of the hydrogen. It was recommended that the remainder of the cap screws from the same lot as the failed screws be baked at approximately 190 deg C (375 deg F) for 24 h.

A process vessel heating coil, consisting of several 3 ft diam turns, was supplied with steam at 400 psi and a temperature of 343 deg C (650 deg F). At bi-weekly intervals well water was introduced to effect rapid cooling of the contents. After about eight months, leakage developed from a circumferential crack on the underside of the uppermost turn. Shorter cracks were found at a similar location on the bottom turn, and further leakage occurred at pinhole perforations adjacent to the crack in the top turn and near to a butt-weld in the coil. Microscopic examination revealed that the cracks were predominantly of the intergranular variety. In addition, transgranular cracks were present. Material was an austenitic stainless steel of the type specified but the absence of columbium and titanium in significant amounts showed that it was not stabilized against intergranular carbide precipitation. The transgranular cracks indicated that failure was due partly to stress-corrosion. It was concluded that the chlorides provided the main corrodent for both the stress and intercrystalline-corrosion cracking.

A portion of the wall of a reactor vessel used in burning impurities from carbon particles failed by localized melting. The vessel was made of Hastelloy X (Ni-22Cr-9Mo-18Fe). Considering the service environment, melting could have been caused either by excessive carburization (which would have lowered the melting point of the alloy markedly) or by overheating. A small specimen containing melted and unmelted metal was removed from the vessel wall and examined metallographically. It was observed that the interface between the melted zone and the unaffected base metal was composed of large grains and enlarged grain boundaries. An area a short distance away from the melted zone was fine grained and relatively free of massive carbides. This evidence supported the conclusion that the vessel failed by melting that resulted from heating to about 1230 to 1260 deg C (2250 to 2300 deg F), which exceeded normal operating temperatures, and carburization was not the principal cause of failure. No recommendations were made.

Beveled weld-joint V-sections were fabricated to connect inlet and outlet sections of tubes in a type 347 stainless steel heat exchanger for a nitric acid concentrator. Each V-section was permanently marked with the tube numbers by a small electric-arc pencil. After one to two years of service, multiple leaks were observed in the heat-exchanger tubes. Investigation supported the conclusion that the corrosion occurred at two general locations: the stop point of the welds used to connect the inlet and outlet legs of the heat exchanger, and the stop points on the identifying numerals. Recommendations included replaced the material with type 304L stainless steel.

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.

AISI type 410 stainless steel tube bundles in a heat exchanger experienced leakage during hydrostatic testing even before being in service. The inside surfaces of the tubes was observed to have been pitted. Chloride-ion pitting was revealed by the undercutting in the cross section of a pit and further confirmed by x-ray spectrometry. It was concluded that the failure was caused by pitting due to chlorides in the water used to flush the tubes before service. The use of brackish water to flush or test stainless steel equipment was recommended to avoid pitting.