Designation: ASTM G 161 00 Guide for Corrosion-Related Failure Analysis & Evaluation of Corrosion Pitting

1. Scope 1.1 This guide covers key issues to be considered when examining metallic failures when corrosion is suspected as either a major or minor causative factor. 1.2 Corrosion-related failures could include one or more of the following: change in surface appearance (for example, tarnish, rust, color change), pin hole leak, catastrophic structural failure (for example, collapse, explosive rupture, implosive rupture, cracking), weld failure, loss of electrical continuity, and loss of functionality (for example, seizure, galling, spalling, swelling). 1.3 Issues covered include overall failure site conditions, operating conditions at the time of failure, history of equipment and its operation, corrosion product sampling, environmental sampling, metallurgical and electrochemical factors, morphology (mode) or failure, and by considering the preceding, deducing the cause(s) of corrosion failure. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2. Referenced Documents 2.1 ASTM Standards: E 3 Methods of Preparation of Metallographic Specimens2 E 1459 Guide for Physical Evidence Labeling and Related Documentation3 E 1492 Practice for Receiving, Documenting, Storing, and Retrieving Evidence in a Forensic Science Laboratory3 G 1 Practice for Preparing, Cleaning, and Evaluating Corrosion Test Specimens4 G 46 Guide for Examination and Evaluation of Pitting Corrosion4 3. Significance and Use 3.1 This guide is intended to assist those encountering corrosion or possible corrosion as a causative factor in a failure analysis. 3.2 This guide is not an absolute plan that will identify the cause of corrosion in all failure analyses. 3.3 This guide is intended to help an investigator identify significant sources and types of corrosion information that may be available for failure analysis. 3.4 Appendix X1 contains a checklist that is intended to assist in corrosion-related failure evaluations. 4. Organizing the Analysis 4.1 Early recognition of corrosion as a factor in a failure analysis is critical to any such investigation. Therefore, it is generally desirable to conduct the analysis as soon as possible after the apparent failure. It is always desirable to protect the physical evidence until the analysis can begin. Much important corrosion information can be lost if a failure scene is altered or changed before appropriate observations can be made. 4.2 A written plan for the detailed analysis should be prepared. The plan may include methods of documentation (photographs before and during analysis, sketches, statements), responsibilities of parties, reporting needs, and scheduling.

4.3 If the capability (corrosion knowledge and experience) of in-house personnel and availability of resources are inadequate to make the analysis in a timely manner, it may be expedient to seek third party services. 5. Failure Site Conditions 5.1 When possible, an overall examination of the conditions at a failure site prior to cleaning, moving, or sampling debris should be conducted. Impressions as to physical arrangements, odors, colors, textures, and conditions of adjacent structures can provide important clues as to active corrosion processes. 5.2 Photographs or videotapes serve as documentation of the observations. Color photographs are preferable. It is helpful to include labels and indications of size, location, and orientation in the photographs. Photographs before, during, and after sampling are recommended. 5.3 Sketches and drawings with notes as to detailed observations can be beneficial for later evaluations. Locations of samples and photographs may be shown. 5.4 Interviews with those who were present or nearby when the failure occurred would be appropriate. Information on time,
This guide is under the jurisdiction of ASTM Committee G01 on Corrosion of Metals and is the direct responsibility of Subcommittee G01.05 on Laboratory Corrosion Tests. Current edition approved May 10, 2000. Published June 2000. Originally published as G 161- 99. Last previous edition G 161 - 99a. 2 Annual Book of ASTM Standards, Vol 03.01. 3 Annual Book of ASTM Standards, Vol 14.02. 4 Annual Book of ASTM Standards, Vol 03.02.
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sights, sounds, and conditions can be gained during such interviews. 6. Operating Conditions At Time of Failure 6.1 Ascertain the operating conditions from operators logs, recorders, and data loggers (verify the accuracy of time records). Special attention should be given to the stability of the operating conditions, for example, were they stable or variable. Conditions of corrosion concern could be temperature, pressure, flow rate, velocity, process stream pH and chemical composition, time, and weather. 6.2 Special attention should be given to out-of-specification or other abnormal or unusual upset conditions. 6.3 It may be necessary to plot or track operating conditions for an indefinite period of time prior to the detection of failure to more clearly identify any unusual, contributory operating conditions. 6.4 If similar, parallel equipment at the same or other location was operating at the time of the corrosion-related failure, note the operating conditions as a reference point. Such information could be useful in judging the normalcy of the operating conditions associated with the failure. 6.5 Corrosion monitoring instruments and coupons, if present, should be examined to help document operating conditions at the time of failure. 7. Historical Information 7.1 Historical information, when available, is extremely useful in understanding some situations. All of the types of information noted may not be useful. Often in cases of older equipment, historical information may be nearly impossible to find because of lost files or retired personnel. Based on cost,

time, and anticipated benefit, a judgement must be made as to the effort one should expend in retrieving historical information. 7.2 Useful details regarding original constructions may include, but are not limited to, design drawings and specifications, material specifications (composition, thermal treatments, surface treatments), joining (bolts, rivets, welds, adhesives), and surface treatments (coatings, pickling, etching, anodizing, plating, peening, grinding, insulation, or refractories). 7.3 Details regarding modifications made subsequent to original fabrication and prior to the corrosion-related failure may be extremely important because they often reveal lessthanoptimum field work. Modifications may have been made for one or more reasons, including, but not limited to, problems with original design, changed service requirements, corrected earlier failures, and correction of safety and environmental concerns. The same types of details suggested in 7.2 should be considered regarding modifications. 7.4 Details regarding operating history may be important. Three types of operating information that may require documentation are original design parameters, chronology of nominal operating parameters, and anomalous operating parameters, including out-of-specification periods and significant downtime periods. 7.5 Maintenance, cleaning, and repair histories may be important and should be documented. 7.6 Changes in specification for, and sources of, process raw materials and supplies may be significant and should be evaluated. 8. Sampling 8.1 Careful sampling is critical to the successful investigation of corrosion-related failures. Sampling in corrosion investigations is similar to that used in forensic investigations by criminologists. Guide E 1459 and Practice E 1492 address issues of labeling and documenting field evidence. These standards may provide useful guidance during sampling for corrosion investigations. 8.2 The written plan suggested in 4.2 should be supplemented with a written sampling plan. The plan should specify a sample location, identification system, and method of collection. 8.3 Avoid contamination during sampling by using clean tools. Personnel should wear gloves to avoid fingerprints and personal contact. 8.4 Sample containers should be clean and sealable to protect samples from contamination and damage. The material of sample containers should be selected carefully to avoid undesirable interaction with samples. Each container should be dated and identified according to the sampling plan. 8.5 Samples of corroded and uncorroded materials may be useful in the identification of causative factors. Samples should be as large as practical to give analysts sufficient material to work with and to protect critical corroded areas from damage during cutting and transporting. If failure initiation location is apparent, it should be sampled. When cutting samples, consideration should be given to temperature control and to the introduction of cutting and cooling fluids that could alter the surface and metallurgical conditions. Because of the solubility in water of many corrosion products, samples must be protected from extraneous moisture. 8.6 Corrosion products and deposits should be given special sampling treatment because they are often key elements in

understanding the failure. Care should be used in the selection of tools for collecting these samples. Nonmetallic tools are often preferred because they present less chance for contamination of the sample or for damaging critical corroded surfaces. When there is insufficient corrosion product or deposit for easy field sampling, care should be used when handling material so that subsequent laboratory sampling may be conducted. Because of the solubility in water of many corrosion products, samples must be protected from extraneous moisture. 8.7 Process stream samples may be desirable. The most useful process stream samples are those taken from the failure location as soon after the event as possible. Delayed or typical process stream samples are less useful because there is no assurance that they represent the conditions at failure. 8.8 Special sampling procedures may be required when microbiological factors are suspected of being involved. Before taking such samples, consult ASTM STP 1232 for guidance (1).5 8.9 Care should be taken during sampling to protect any
The boldface numbers in parentheses refer to the list of references at the end of this guide.
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fracture surfaces from becoming damaged. If partial reassembly is necessary, maintain an air gap between mating fracture surfaces. Bringing fracture surfaces together could eliminate very valuable information. 9. Evaluation of Samples 9.1 Compositions of samples of materials (including fasteners and weld beads), process streams, deposits, and corrosion products should be determined using appropriate analytical tools and techniques. 9.2 Metallic samples (including fasteners and weld beads) should be evaluated for metallurgical condition and structure. This evaluation may involve mechanical and physical property tests, metallographic examination of cross sections, and corrosion tests. 9.2.1 Selection of mechanical and physical property tests should consider the influence of service temperature and time on the properties being evaluated. 9.2.2 Selection of metallographic examination techniques should consider the influence of service temperature and time on the metallurgical structures being examined. 9.2.3 Corrosion testing of affected material may be necessary to identify metallurgical and environmental factors associated with the failure. Selection of corrosion tests should consider the suspected type of failure, the materials involved, and the suspected environment. 9.2.4 In some cases it may be necessary to remove corrosion products to permit evaluation. The guidance of Practice G 1 can be used to remove corrosion products with minimal damage to the metal sample. 9.3 Metallic samples are often subdivided into specimens suitable for laboratory evaluation. The location and orientation of each specimen must be documented by one or more of the following: photographs, drawings, or written descriptions. Each specimen should be labelled to aid in identifying its original location within the sample.

9.4 Failure locations, such as pits, fracture surfaces, crevices, and generally attacked surfaces, should be examined, and measurements should be made to document surface chemistry, pit depths, crack dimensions, and metal losses and other modes of attack. These examinations often require the use of light microscopes, scanning electron microscopes (including energy dispersive x-ray spectrometers (EDS)), and other instruments. In some cases, cross sections from corroded areas may require examination (see Methods E 3) to relate corrosion extent and morphology (for example, intergranular or transgranular) to metallurgical structure . In cases involving fracture, fractographic examination is recommended. 10. Assessment of Corrosion-Related Failure 10.1 Assessment involves the evaluation of observations from the failure location, operational information, materials evaluations, examinations of failure samples, and expert opinions. 10.2 Incorrect or out-of-specification materials, process streams, and operating conditions should be noted and described. 10.3 Unusual or unexpected species in corrosion products or deposits should be noted and described. 10.4 The type and extent of corrosion should be noted. The extent of corrosion may be determined by measurements and calculations of general corrosion rate, pitting penetration (see Guide G 46), or crack growth rate. It may also be useful to compare these rates with expected rates from the literature or experience. Rate discrepancies should be investigated (for example, by laboratory simulations). This information will be useful in judging the suitability of particular materials. 10.5 From these observations and findings, the investigator should be able to identify the one or more causative factor(s) involved in the failure. In many cases, more than one factor will be suggested as having played a role in the failure. References to similar or related corrosion-related failures are often useful (2-8). The investigator may provide explanations and rationales for suggested corrective actions. 11. Report 11.1 General description of corrosion-related failure. 11.2 Operating conditions at time of failure. 11.3 Historical information. 11.4 Samples taken including photographs. 11.5 Evaluations conducted. 11.6 Results of evaluations. 11.7 Corrosion cause or causes of failure. 11.8 Suggested corrective actions, if any. 11.9 References. 11.10 Disposition of samples and records. 12. Keywords 12.1 corrosion; failure; failure analysis; sampling; type of corrosion

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APPENDIX
(Nonmandatory Information) X1. CORROSION-RELATED FAILURE ANALYSIS CHECKLIST

X1.1 The following checklist is intended as a guide. It should remind the user of important considerations in dealing with corrosion-related failure analysis. All items listed may not

apply to every situation. Similarly, additional items may be appropriate for some situations. The order of presentation has been found useful. X1.2 Identification of Key Factors: X1.2.1 Name of equipment. X1.2.2 Name and description (including dimensions) of failed part. X1.2.3 Date and time of failure. X1.2.4 Location of failure. X1.2.5 Accessibility of failure location. X1.2.6 Names of key personnel. X1.3 Overview of Failure Conditions (Use Notes, Sketches, Photographs, and Video Tapes) : X1.3.1 Physical arrangement. X1.3.2 Smells or odors. X1.3.3 Colors. X1.3.4 Deposits or residues. X1.3.5 Surrounding conditions. X1.3.6 Evidence of rearrangement or movement. X1.4 Overall Plan of Attack (Include Who, What, When, Where for Each Action): X1.4.1 Types of information. X1.4.2 Types of documentation. X1.4.3 Sampling. X1.4.4 Testing. X1.4.5 Evaluations. X1.4.6 Reporting. X1.5 Types of Information: X1.5.1 Conditions at Time of Failure: X1.5.1.1 Process variables. X1.5.1.2 Weather. X1.5.1.3 Observations by personnel. X1.5.1.4 Stability. X1.5.1.5 Normal or unusual. X1.5.1.6 Startup/shutdown/maintenance/layup/constuction. X1.5.2 History: X1.5.2.1 Design. X1.5.2.2 Construction/fabrication. X1.5.2.3 Materials of construction. X1.5.2.4 Modifications. X1.5.2.5 Operation. X1.5.2.6 Process changes. X1.5.2.7 Previous failures. X1.5.2.8 Maintenance practices. X1.5.2.9 Cleaning practices. X1.5.2.10 Repairs. X1.6 Types of Documentation: X1.6.1 Operating charts and logs. X1.6.2 Weather station observations. X1.6.3 Process materials specifications (including materials safety data sheets (MSDS)). X1.6.4 Materials of construction specifications and certifications. X1.6.5 Fabrication specifications. X1.6.6 As-built drawings. X1.6.7 Sampling plan (including identification system photographs, and locations). X1.6.8 Test reports. X1.6.9 Site inspection notes, sketches, photographs, and video tapes.

X1.6.10 Interview notes and tapes. X1.7 Sampling: X1.7.1 Metal (failed and unfailed). X1.7.2 Process materials. X1.7.3 Corrosion products. X1.7.4 Other deposits and residues. X1.7.5 Environmental (air, water, soil, and other). X1.8 Testing: X1.8.1 Metal composition. X1.8.2 Metal mechanical properties. X1.8.3 Metal physical properties. X1.8.4 Electrochemical test results. X1.8.5 Corrosion product composition. X1.8.6 Deposit and residue composition (including microbiological, if conducted). X1.8.7 Environment composition (including concentrations and contaminants). X1.8.8 Environment pH, temperature, and conductivity. X1.8.9 Process material composition. X1.8.10 Corrosion type and morphology (microstructures, fractography). X1.8.11 Process simulation exposures. X1.8.12 Surface analysis by EDS or other suitable technique. X1.9 Evaluations: X1.9.1 Test results versus specifications. X1.9.2 Corrosion mechanism. X1.9.3 Cause of corrosion. X1.9.4 Measurements and calculations of extent of corrosion. X1.9.5 Discrepancies (if any) between predicted and actual corrosion rates. X1.10 Reports: X1.10.1 Interim or progress.

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X1.10.2 Final. REFERENCES

(1) Kearns, J.R., Little, B.J., eds. Microbiologically Influenced Corrosion Testing, ASTM STP 1232, ASTM, 1994 (PCN 04-012320-27). (2) Wyatt, L. M., Bagley, D. S., Moore, M. A., and Baxter, D. C., An Atlas of Corrosion and Related Failures, MTI Publication Series, Vol 18, St. Louis, MO, 1987. (3) Esaklul, Khlefa A., ed., Handbook of Case Histories in Failure Analysis, Vol 1 and Vol 2, ASM International, Metals, Park, OH, 1992-93. (4) Metals Handbook, Vol 13, 9th ed., Corrosion, ASM International, 1987. (5) Dillon, C. P., Forms of Corrosion: Recognition and Prevention, NACE International, Houston, TX, 1982. (6) Metals Handbook, Vol 11, 9th ed., Failure Analysis and Prevention, ASM International, Metals Park, OH, 1986. (7) McIntyre, D., Forms of Corrosion: Recognition and Prevention, NACE International, Houston, TX, 1997. (8) During, E.D. D., ed, Corrosion Atlas, Elsevier Publication, 1997.
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Corrosion of metals and alloys - Evaluation of pitting corrosion

1 Scope
This International Standard gives guidance on the selection of procedures that can be used in the identification and examination of pits and in the evaluation of pitting corrosion.

2 Normative reference
The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 8407:1991, Corrosion of metals and alloys Removal of corrosion products from corrosion test specimens.

3 Identification and examination of pits

3.1 Visual inspection
A visual examination of the corroded metal surface with or without the use of a low-power magnifying glass may be used to determine the extent of corrosion and the apparent location of pits. It is often advisable to photograph the corroded surface so that it can be compared with the clean surface after the removal of corrosion products. 3.1.1 If the metal specimen has been exposed to an unknown environment, the composition of the corrosion products may be of value in determining the cause of corrosion. Recommended procedures in the removal of particulate corrosion products should be followed and reserved for future identification. 3.1.2 To expose the pits fully, it is recommended that cleaning procedures should be used to remove the corrosion products and avoid solutions that attack the base metal excessively (see IS0 8407). It may be advisable during cleaning to probe the pits with a pointed tool to determine the extent of undercutting or subsurface corrosion (see figure I). However, scrubbing with a stiff-bristle brush will often enlarge the pit openings sufficiently by removal of corrosion products or undercut metal to make the pits easier to evaluate. 3.1.3 Examine the cleaned metal surface to determine the approximate size and distribution of pits. Follow this procedure by a more detailed examination

through a microscope using low magnification (approximately x 20). 3.1.4 Determine the size, shape and density of pits. 3.1.4.1 Pits may have various sizes and shapes. A visual examination of the metal surface may show a round, elongated or irregular opening, but it seldom provides an accurate indication of corrosion beneath the surface. Thus it is often necessary to cross-section the pit to see its actual shape and to determine its true depth. Several variations in the cross-sectioned shape of pits are shown in figure 1. 3.1.4.2 It is difficult to determine pit density by counting pits through a microscope eyepiece, but the task may be made easier by the use of a plastic grid. Place the grid, containing 3 mm to 6 mm squares, on the metal surface. Count and record the number of pits in each square, and move across the grid in a systematic manner until all the surface has been covered. This approach minimizes eye-strain because the eyes can be taken from the field of view without fear of losing the area of interest. Enlarged photographs of the area of interest may also be used to reduce eyestrain.

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IS0 11463:1995(E) @ IS0

a) Narrow, deep b) Elliptical 1.3 Wide, shallow d) Subsurface e) Undercutting (Horizontal) (Vertical) f) Microstructural orientation

Figure 1 - Variations in the cross-sectional shape of pits 3.1.5 To carry out a metallographic examination select and cut out a representative portion of the metal surface containing the pits and prepare a metallographic specimen in accordance with recommended procedures. If corrosion products are to be examined in cross-section, it may be necessary to fix the surface in a mounting compound before cutting. Examine microscopically to determine whether there is a relation between pits and inclusions or microstructure, or whether the cavities are true pits or might have resulted from metal loss caused by intergranular corrosion, dealloying, etc.

3.2 Non-destructive inspection

A number of techniques has been developed to assist in the detection of cracks or cavities in a metal surface without destroying the material. See [II in annex B. These methods are less effective for locating and defining the shape of pits than some of those previously described, but they merit consideration because they are often used in situ, and thus are more applicable to field applications. 3.2.1 Radiographic Radiation, such as X-rays, passes through the object. The intensity of the emergent rays varies with the thickness of the material. Imperfections may be detected if they cause a change in the absorption of Xrays. Detectors or films are used to provide an image of interior imperfections. The metal thickness that can be inspected is dependent on the available energy

output. Pores or pits must be as large as 0,5 % of the metal thickness to be detected. This technique has only slight application to pitting detection, but it might be useful for comparing specimens before and after corrosion to determine whether pitting has occurred and whether it is associated with previous porosity. It may also be useful to determine the extent of subsurface and undercutting pitting (see figure I). 3.2.2 Electromagnetic 3.2.2.1 Eddy currents may be used to detect defects or irregularities in the structure of electrically conductive materials. When a specimen is exposed to a varying magnetic field, produced by connecting an alternating current to a coil, eddy currents are induced in the specimen and they in turn produce a magnetic field of their own. Materials with defects will produce a magnetic field that is different from that of a reference material without defects, and an appropriate detection instrument is required to determine these differences. 3.2.2.2 The induction of a magnetic field in ferromagnetic materials is another approach that is used. Discontinuities that are transverse to the direction of the magnetic field cause a leakage field to form above the surface of the part. Ferromagnetic particles are placed on the surface to detect the leakage field and to outline the size and shape of the discontinuities. Rather small imperfections can be detected by this method. However, the method is limited by the required directionality of defects to the magnetic field, by the possible need for demagnetization of the material and by the limited shape of parts that can be examined.

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0 IS0 3.2.3 Sonics In the use of ultrasonics, pulses of sound energy are transmitted through a couplant, such as oil or water, on to the metal surface where waves are generated. The reflected echoes are converted to electrical signals that can be interpreted to show the location of flaws or pits. Both contact and immersion methods are used. The test shall be carried out from the nonpitted face. The test has good sensitivity, although it is unlikely to detect pits of less than 1 mm diameter or within 1 mm of a non-pitted face, and provides instantaneous information about the size and location of flaws. However, reference standards are required for comparison and training is needed to interpret the results properly. 3.2.4 Penetrants Defects opening to the surface can be detected by the application of a penetrating liquid that subsequently exudes from the surface after the excess penetrant has been removed. Defects are located by spraying the surface with a developer that reacts with a dye in the penetrant, or the penetrant may contain a fluorescent material that is viewed under ultra-violet light. The size of the defect is shown by the intensity

of the colour and the rate of bleed-out. This technique provides only an approximation of the depth and size of pits. 3.2.5 Replication Images of a pitted surface can be created by applying a material to the surface which conforms to the shape of the pits and can be removed without damaging its shape. This method will not work however, for pits of subsurface or undercut type. The removed material contains a replica of the original surface which, in some cases, is easier to analyze than the original. Replication is particularly useful for analysis of very small pits.

4 Extent of pitting 4.1 Mass loss

Metal mass loss is not ordinarily recommended for use as a measure of the extent of pitting unless general corrosion is slight and pitting is fairly severe. If uniform corrosion is significant, the contribution of pitting to total metal loss is small, and pitting damage cannot be determined accurately from mass loss. In any case, mass loss can only provide information about total metal loss due to pitting but nothing about density of pits and depth of penetration. However, mass loss should not be neglected in every case because it may be of value; for example, mass loss along with a visual comparison of pitted surfaces may be adequate to evaluate the pitting resistance of alloys in laboratory tests. Mass loss may also be useful to detect the existence of subsurface metal loss.

IS0 11463:1995(E) 4.2 Pit depth measurement

4.2.1 Metallography Pit depth may be determined by sectioning vertically through a preselected pit, mounting the cross-sectioned pit metallographically and polishing the surface. A better or alternative way is to section slightly away from the pit and slowly grind until the pit is in the cross-section. Sectioning through a pit can be difficult and one may miss the deepest portion. The depth of the pit is measured on the flat, polished surface by the use of a microscope with a calibrated eyepiece. The method is very accurate, but it requires good operator skill and good judment in the selection of the pit and good technique in cutting through the pit. Its limitations are that it is time-consuming, the deepest pit may not have been selected and the pit may not have been sectioned at the deepest point of penetration. The method, however, is the only suitable for the evaluation of the pit shape as in figure 1. 4.2.2 Machining See 121 and [31 in annex B. 4.2.2.1 This method requires a sample that is fairly regular in shape, and it usually involves the destruction of the specimen. Measure the thickness of the specimen between two areas that have not been affected by general corrosion. Select a portion of the surface on one side of the specimen that is relatively unaffected; then machine the opposite surface where the pits are located on a precision lathe, grinder or mill

until all signs of corrosion have disappeared. Some difficulty from galling and smearing may be encountered with soft metals and pits may be obliterated. Conversely, inclusions may be removed from the metal thus confusing examination. Measure the thickness of the specimen between the unaffected surface and subtract from the original thickness to give the maximum depth of pitting. Repeat this procedure on the unmachined surface unless the thickness has been reduced by 50 % or more during the machining of the first side. 4.2.2.2 This method is equally suitable for determining the number of pits with specific depths. Count the visible pits then machine away the surface of the metal in measured stages and count the number of visible pits remaining at each stage. Subtract the number of pits at each stage from the count at the previous stage to obtain the number of pits at each depth of cut. Count at the previous stage to obtain the number of pits at each depth of cut. 4.2.3 Micrometer or depth gauge 4.2.3.1 This method is based on the use of a pointed needle attached to a micrometer or calibrated depth gauge to penetrate the pit cavity. Remove surrounding corrosion products or debris thoroughly then zero the instrument on an unaffected area at the lip of the pit.

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IS0 11463:1995(E) @ IS0

Insert the needle in the pit until it reaches the base. The distance travelled by the needle is the depth of the pit. It is best to use constant-tension instruments to minimize metal penetration at the base of the pit. It may be advantageous to use a stereomicroscope in conjunction with this technique so that the pit can be magnified to ensure that the needle point is at the bottom of the pit. The method is limited to pits that have a sufficiently large opening to accommodate the needle without obstruction. This eliminates those pits which have undercutting or strong directional orientation. 4.2.3.2 In a variation of this method, attach the probe to a spherometer and connect it through a microammeter and battery to the specimen (see I31 and [41 in annex B). When the probe touches the bottom of the pit, it completes the electrical circuit and the probe movement is a measurement of pit depth. This method is limited to very regularly shaped pits because contact with the side of the pit or conductive debris would give a false reading.
4.2.4 Microscopy

This method is particularly valuable when pits are too narrow or difficult to penetrate with a probe type of instrument. The method is amenable to use as long as light can be focused on the bottom of the pit. This would not be possible in the case of example (e) in figure 1. 4.2.4.1 Use a metallurgical microscope with a magnification

range from x 50 to x 500 and a calibrated fine-focus knob (for example, 1 division G 0,001 mm). If the latter is not available, a dial micrometer can be attached to the microscope in such a way that it will show movement of the stage relative to the microscope body. 4.2.4.2 Locate a single pit on the metal surface and centre it under the objective lens of the microscope at low magnification (e.g., x 50). Increase the objective lens magnification until the pit area covers most of the field under view. Focus the specimen surface at the lip of the pit, using first the coarse and then the finefocusing knobs of the microscope. Record initial readings from the fine-focusing knob, refocus on the bottom of the pit with the fine-focusing knob, and record the reading. The difference between the initial and the final readings on the fine-focusing knob is the pit depth. 4.2.4.3 Repeat the steps in 4.2.4.2 to obtain additional measurements or until satisfactory duplication has been obtained. The repeatability of pit depth measurements on a single pit at four magnifications is shown in annex A. 4.2.4.4 A variation of this technique employs the use of an interference microscope. A beam of light is split and one portion is projected on to the specimen and the other on to the surface of a reference mirror. The reflected light from these two surfaces is recombined, and interference fringes are formed that provide a topographical map of the specimen surface. These fringes can be used to measure vertical deviations on the metal surface. However, the method is limited to the shallower pits, that is, less than 25 urn, because the number of fringes increases to the point where they are difficult to count.

5 Evaluation of pitting
5.1 General
There are several ways in which pitting can be described, given a quantitative expression to indicate its significance or used to predict the life of a material. Some of the more commonly used methods are described in this clause, although it is often found that no single method is sufficient by itself.

5.2 Standard charts

See [31 in annex B. 5.2.1 Rate the pits in terms of density, size and depth on the basis of standard charts, such as those shown in figure 2. Columns A and B relate to the extent of pitting at the surface of the metal (that is, column A is a means for rating the number of sites per unit area and column B a means for showing the average size of these sites). Column C rates the intensity or average depth of attack. A typical rating might be A-3, B-2, C-3, representing a density of 5x IO4 pits/m*, an average pit opening of 2 mm* and an average pit depth of I,6 mm. 5.2.2 This method offers an effective means of communication between those who are familiar with the charts and it is a simple means of storing data for comparison with other test results. However, it is tedious

and time consuming to measure all pits and the time is usually not justified because maximum values (e.g. pit depths) usually have more significance than average values.

5.3