f ature oeus
BY RAYMUND SINGLETON, SINGLETON CORP., CLEVELAND, OHIO
Accelerated Corrosion Testing
A ccelerated corrosion testing of metals and coatings was first
developed in the late 1890s and early 1900s for testing products to
increase t heir useful perfo rmance and service life. This method of testing the corrodibility of ferrous and nonferrous metals and organic and inorganic coatings has since been improved and variations added to
bener rest new materials and help operators understand how they may perform in, and wirhsmnd, a wider range of real world environments.
Accelerated corrosion testing has also evolved from providing information to help determine durability of products, and their quality assurance during manufacturing, to use in product research and development. Professional trade, industry) military and standards organizations) such as: ASTM International (American Society for Testing and Materials), the Society of Automotive Engineers (SA E), the Fedetation of Societies for Coatings Technologies (FSCT), NACE International (National Association for Corrosion Engineers ») Society for Pro tective Coatings (SSPC) and others have developed a number of accelerated corrosion tests to meet the demands of changes) and advances, in technology, materials) and other performance requirements and environmental regulations.
For instance, water-based coatings have been developed as replacements for solvent-based liquid coating materials in response to environmental concerns. Some powder coatings and their application methods reduce the use of solven ts and ease application . In addition) the automotive industry has improved coatings and increased the number of surfaces coated as part of the response to market pressures for longer warranties.
121 metalfinishing I November/ December 2012
Some of the more widely used tests are the representative ASTM Standards detailed in this article and well known industry cyclic corrosion testS such as: General Motors GMW14872 (fotmerly GM9540P), and SAE J2334. There are many other tests in use; however, those mentioned also exhibit wider applicability and versati li ty and are, therefore, some of the more popular procedures. Other than the ASTM B1l7 Salt Fog tes t, most widely used for on-line process and product quality control, no other single corrosion test is as dominant because of the wide variety of service conditions, product industries and specific issues such as various materials, applications methods, properties) and varying surfaces.
O ther considerations to consider when choosing or specifYing a particular accelerated corroSIOn tes t include th e multitude of environments and customer demands faced by a product and industry. A variety of standard tests has been developed to address these issues.
One of the first- and still most widely utilized- accelerated corrosion tests developed is ASTM B 117 Operating Salt Spray (Fog) Apparatus. Early development of corrosion tests was initiated in order to evaluate the corrodibility of metals and protective properties of coatings in a marin e or "near shore)) environment. As corrosion testing was increasingly used also to evaluate product quality and materials llsed in product development) variations on the basic) o r original, corrosion test standard s have been added to
increase their usefulness for a wider range of environmen ts and materials. This process has resulted in the development of the various representative accelerated corrosion tests
to be di scussed in this update. The usefuln ess of testing coatings
for resistance to water, o r high humidity) as a good indicator of their service life in service environments of that type resulted in the ASTM 01735 Standard Practice for Testing Water Resistance of Coatings Using Water Fog Apparatus and the ASTM 02247 Standard Practice for Testing Water Resistance of Coatings in 100% Relative Humidity. Demand for improved evaluation of decorative copper/nickel/chromium or nickel/chromium coatings on steel, zinc alloys, aluminum alloys, and plastics designed for severe service resulted in the ASTM B368 Standard Test Method for Copper Accelerated Acetic Acid-Salt Spray (Fog) Testing, widely known by its acronym as the "CASS" test.
Additional needs for testing of product resistance to harsh industrial environments led to the development of the ASTM G85 Standard Practice for Modified Salt Spray (Fog) Testing with its 5 included corrosion test vatiations and the ASTM G87 Standard Practice for Conducting Moist S02 Tests. The ASTM G85 variations (tests): Annex 2, Annex 3, Annex 4, and Annex 5 along with ASTM G87 were developed to subject test pieces to cycles of differing environments to more closely resemble the changes occurring in pertinent real-world environments. See Table I for in formation on "static" versus "cyclic') environment tests.
With the wide variety of materials and coatings, their uses, and the service environments in which they may be lLsed, manufacturers and produce development personnel now can select an accelerated corrosion test [hat best suits their particular product and applicable environmental conditions. Table I is provided to give a guide to which ASTM test standard can be used for the representative situations listed. Along with the development of new accelerated corrosion tests ASTM Standards have been developed to give direction and resources for the preparation of test pieces prior to testing and evaluation of post test resu lts. A good example is
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featurefocus Table I. Static Versus Cyclic Tests
Static Corrosion Tests In static corrosion tests the exposure zone conditions of the test chamber stay the same (within
defined tolerance limits) throughout the duration of the test. The test duration (length of exposure) is the only variable.
Examples of Static Condition Corrosion Tests ASTM B 117 Salt (Fog) Spray ASTM B 368 Copper Accelerated Salt Spray ASTM D 1735 Water Fog Humidity ASTM D 2247 Condensing 100% humidity ASTM G 85, Annex 1 Acetic Add Salt Fog
Cyclic Tests In cyclic corrosion !ests the conditions in the exposure zone change for each step in the cycle in an
ordered, predefined sequence. The changeable conditions can include temperarure, various types of moisture application, different levels of humidity, different types of pollutant or electrolyte such as various salts, gases, etc" and various lengths of exposure for each,
Cycle Type A tests Temperature is constant Various types of moisture application, diff~rent levels of humidity, different types of pollutant or
electrolyte such as various salts, gases, etc., and various lengths of exposure for each step. Total test duration (length of exposure) is also a variable
Examples of Cyclic Type A Condition Corrosion Tests ASTM G 85 Annex 2 Acetic Acid Annex 3 Acidified SF Annex 4 SaltiSOz Spray
Cyclic Type B Tests Temperature is different for at least some steps in the cycle Various types of moisture application, different levels of humidity, different types of pollutant or
electrolyte, such as various salts, gases, etc., and differing lengths of exposure for various steps. Total test duration (length of exposure) is also a variable.
Examples of Cyclic Type B Condition ColTQ8ion Tests ASlM G 85 Annex 5 Modified SF (DEC) Dilute Electrolyte Cyclic FoglDry Test AS1M G 87 Moist SOz GM 9540P SAE J-2334
ASTM 0609 Standard Practice for Preparation of Cold-Rolled Steel Panels for Testing Paint Varnish, Conversion Coatings and Related Coating Products. This standard provides guidelines for the preparation of test pieces before they are introduced into the accelerated corrosion test. ASTM Standards: 01654 Standard Test Method for Evaluation of Painted or Coated Specimen Subjected to Corrosive Environments; D610 Standard Pracrice for Evaluating Degree of Rusting on Painted Steel Surfaces, and; 0714 Standard Test Method for Evaluating Degree of Blistering of Paints were developed to provide common standards for analyzing and reporting the results obtained from the corrosion tests and observed on the tested speci mens. These standards are summarized below.
ISSUES Primary issues that arise when discussing the usefulness of accelerated corrosion tests are comparison to real-world exposures and the consis-
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tency of test results. Accelerated corrosion tests are performed under controlled conditions with a limited number of variables, which generally do not duplicate the vast variety of variables that occur in anyone location in a real-world environment. Comparison standards can be used to compensate for this. Comparison standards are properly prepared, representative test pieces from a prod uct wi th a known "track record" of exhibiting acceptable perfOl'mance from exposure in applicable real-world environments and/or also acceptable corrosion resistance after being exposed to the specified accelerated corrosion test(s}. They then can be used as standards against which other tested pieces are compared. This process helps especially product developers and also quality professionals predict how a new product or production run of an existing product will perform when used. It is usually not possible, unless additional "long-term, realtime)), comparative outdoor or "inservice" exposure data is available,
to directly compare any given number o f hours in an accelerated corrosion test with a given number of years exposure in real-world environments. The development of additional variations on basic accelerated corrosion tests have allowed engineers, technicians, and quality professionals to better evaluate durability of products to be used in a wider variety of environments, under multiple corrosive influences, and under constantly changing service conditions.
The issues are: consistency in the accuracy of test results from subsequent runs of the same test in a single test chamber; and consistency for comparison of test results obtained from the same test run in other chambers. These issues have been addressed with the development of ASTM methods for evaluating this necessary consistency. This verification is called repeatability of results from subsequent runs of the same test in a single test chamber and reproducibility of results from subsequent runs of the same test in other test chambers (regardless of how many other corrosion test chambers are involved). These important verification procedures are covered in Section X3 of the Append", of the ASTM B117 test standard and incorporate "Mass Loss" Corrosion Coupons described in that sect ion. A similar variation of this Mass Loss Corrosion Coupon procedure is described in Paragraph 8.7 of ASTM B368, using nickel coupons for the "CASS" test.
CRITERIA FOR CYCLIC TESTS The American Iron and Steel Institute, in cooperation with the Automotive Corrosion and Prevention Committee of the SAE, conducted a study of existing cyclic corrosion tests (completed in 2003, revised in 2007) in order to develop tests that could be used to rank pe·rformance of materials used in automotive "cosmetic" applications. Approximately 20 existing corrosion tests were selected for study. These included "static" exposure condition tests (tests where the exposure con-
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featu refocus
Fig. 1. Schematic drawing of a typical salt fog test chamber.
di rions do not vary over the duration of the test), such as ASTM B117, and "cyclic" exposure condition rests such as ASTM G8S Annex 5 and GMW14872 (form erly GM9540P), (tests which subject test pieces to a variety of different exposure atmospheres and condit ions over the du ration of the test). Ten di ffe rent test materials were exposed in each test. The results of the tes tS were compared [0 realworld exposure results from 10 sites around the globe utilizing duplicates of the same materials. It was concluded from results tha t an acceptable co rrosion test must: (1) simulate the rank order of performance of coatings in actual service; (2) produce the same type (charac ter) of failure as found in real-world experience (example: b listering); (3) be reproducible; (4) be of rela tively short duration; and (5) be feasib le and cost effective.
The test established as a result of this effort is t he SAE J2334 Laboratory Cyclic Corrosion Test. The SAE J2334, GMW14872 (fo rmerly GM9540P), and ASTM G85 , Annex 5 meet the above criteria and are some of the more commonly llsed cyclic corrosion tests in the u.s. and around t he world. The SAE J2334 and the GMW14872 were ori ginally developed for testing cosmetic finish es on automotive components. Fo rtu itou sly, they have been shown to produce more "realis tic" corrosion resul ts and, therefore) are llsed to test a
14 I metalfinishing I November/December 2012
Table II. Equlpment RequlremeDts for Various Test Standards
Standard
B 117
D 1735
D 2247
B 368
G 85
G 87
Chamber Requirements
Insulated cabinet made with inert materials or illert coating on the interior Salt solution reservoir ASTM D 1193, Type IV (On water supply Humidifying tower One or more fogging towen with atomizer and baffles Compressed air supply Bottom drain Exhaust Heating apparatus for humidifying tower and chamber exposure zone Tcmperarure displa~ for wet and dry bulb temperatures and hurrudifying tower Appropriate ,auges and safety apparatus Test piece supports B 117 chamber without any traces of salt B 117 salt solution reservoir is used for ASTM 0 1193. Type m (Ol) water B 117 chamber
~~~:::~~~~ ~o~~rOf ASTM 0 1193. Type IV water 00 bottom or large internal water taIW in chamber exposure woe Hoating apparatus for water aDd bottom 12 in. of chamber exposure tone Method A, no humidifying tower Method B. equipped to bubble humidified air through air manifold submerged in bottom of exposure wne water Humidifying tower, only if using bubble method B 117 chamber Add bypass on humidifying tower .
Annex 1
Annex 2 and Annex 3
Annex 4
Annex 5
B 117 Ownber
Modified or purpose built B 117 type test chamber with appropriate cyclic timing controls aDd automatic mechanical apparatus to execute required exposure zone temperature and atmosphere changes,
Modified or purpoae built B 117 type test chamber with appropriate cyclic timing controls and automatic mechanical apparatus to execute required oltposure wne temperature and atmosphere changes,
502 supply and dispersion method. Flow meter Modifi_ed or purpo8e built B 117 type test chamber with
app(opriate cyclic timing controls and-automatic mechanical apparatus to execute required exposure woe temperature and atmosphere changes,
Modified or purpose built B 117 type test chamber with appropriate cyclic timing controls and automatic mochanlca1 apparatus to ex~ required exposure zone temperature and atmosphere changes.
No fogging appararus or humidifying tower Internal capadty of 300 L Supply of sulfur dioxide and inlet rube 00 108s than 50 mm from floor of chamber Means to reliove exces. presaure Heat. externally on floor and lower wall, ExternaJ heater for water Metering apparatus Located away from pollution. direct sunlight. and draft
much wider variety of materials, finishes, and applications. ASTM G8S, Annex 5, is known to be particularly useful for testi ng both: architectural coatings and industrial maintenance paints as well as other applications.
ASTM B117 - Standard Practice for Operating Salt Spray (Fog) Apparatus The ASTM B1l7 Standard is primarily used to test the corrosion resistance of organic and inorganic coatings on metals. Examples a re paint or plated finishes on metal items and exposure of prod ucts to "marine" or "near-shore') environments. This standard will also be the base against which this article wit! describe other corrosion tests. The Bl1 7 Standard is a "static" (constant) condi tion, continuous test) preferably run in multiples of 24-hour periods, The test pieces are
TYPES OF TESTS In this case, ASTM B1l 7 is described first . The other ASTM Corrosion Test Standards discussed are described in terms of how they vary from the basic B 117 Standard. Only those aspects of these standards, which are different fro m the B1l7 standard) will be discussed .
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featu refocus
Fig. 2. Typical water·jacketed-type corrosion test chamber, mostly used for static condit ion tests.
Fig. 3. Typical large-size, drive-in-type corrosion test chamber.
exposed to a salt fog atmosphere from atomized solution made up of 5% sodi um chloride and 95% ASTM 01193 Type [V water by mass and held to purity standards specifYing chat it contain: not more than 0.3% by mass total impurities. Halides (Bromide, Flu oride, and Iodide) other than Chloride, shall constitute less than 0.1% by mass of the salt content. Copper content shall be less than 0.3ppm by mass. Sodium Chloride that has had anti-caking agents added shall not be used because sllch agents may acr as CO[
ros ion inhibiw[s. This solution is then atom ized in to the chamber exposure zone, which is maintained at a temperature of35 +/-2°C (95 +/ - 3 ° F) and a relative humidity of at least 95%, creating a fog rhar has a condensate collection rate of 1.0 to2.0 mljhr per 80 m2 of horizontal
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collection area. To maintain these conditions, the chamber is heated and best maintained with a wet bottom condit ion in the exposure zone. The equipment needed to maintain these test co ndition s will meet the requirements described in Table Il and be made such that all component parts that come in contact with the exposure zone, water, or solutions are made of, or coated with, inert materials. Typical tesr chamber components and operational connections are illustrated in Fig.!.
ASTM D1735 - Standard Practice for Testing Water Resis tance of Coatings Using Water Fog Apparatus The ASTM 01735 Standard uses a standard fog-generating chamber as used for the ASTM B117 Srandard. The primary variation s are the chamber temperature, which is held at 38°C (100°F) and the elimination of the corrosive salr (electrolyte). The fog is created by atomizing ASTM 01193 Type IV warer wirhout any salt whatsoever. This test method is used to gauge the life expectancy of coating systems by measuring their resistance to water penetration.
ASTM D2247 - Standard Practice for Testing Water Resistance of Coatings in 100% Relative H umidity The ASTM 02247 Standard is used to investigate how a coating resists water, which can help predict its useful life. This is generally a pass/ fail test; however, the time to fai lure and degree of fai lure can be measured. A coating sysrem typically passes if there is either no sign of water-related failure after the specified test period or less than an esrablished specified amount o f failure.
For the ASTM B2247 Standard the ASTM 01193 Type TV warer is placed in the bottom of the exposure zone to a depth of 6 to 8 in . and rhen heated. The area of the exposure zone above the water is not heated
\
~
i.:-® i !
t_~Jii_~ ./ \
- '::''''::::'-'''''
Fig. 4. Humidity test chamber schematic drawing.
directly in order to cause condensation on the test pieces. The water is introduced intO the chamber before the test pieces and maintained at a temperature approximately 5 to 10 °C (10- 20 ° F) higher than the temperature of the vapor above it. The major variation in the chamber is the elimination of the fogging tower. The 100% humidity results from the vaporization of the heated water in the bottom of the chamber and/or having heated humidified air pumped thro ugh the water. The humidifying tower is llsed when the oprion of having air pumped through the heated water is chosen. The exposure zone is maintained at 38° ± 2°C (100° ±4°F) and 100% relative hum idity. This test method is performed in water-jacketed chambers (see Fig.2) with the 6 to 8 in. of water mentioned above in the bottom of the exposure zone and the water jacket filled to 12 in. above the bottom to ensure that the immersion heaters are submerged. It can also be rlln in larger chambers, such as walk-in or drive-in size un its (see Fig. 3), equipped with heated water tanks in the exposure zone to generate the required humidity. A primary concern when conducting the ASTM 02247 resr is that rhe chamber be sufficiently insulated. Figure 4 is a schematic of a typical ASTM 02247 humidity test chamber configuration. To ensure that rhe ASTM 02247 test is being performed consistently, it is recommended that a control test piece with known durabiliry be included in each test run.
ASTM B368 - Standard T est Method for Copper Accelerated
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featu refocus Acetic Acid-Salt Spray (Fog) Test (or CASS Test) The ASTM B368 Standard, originally developed by the Natio nal Association for Surface Fin.ishing (NASF), is used primarily in the development of coated metal products, incl uding decorative coatings, which will be exposed to severe serv· ice and more corrosive environments and also to evaluate the perfo rmance and protective properties of more durable coatings which would not be affec ted by the typical ASTM B117 type salt fog test. This test method is particula rly applicable to the evaluation of the perfo rmance of decorative copper/ nickel/chromium or nickel/ch romium coatings on steel, zinc alloys, aluminum alloys, anodized alum inum and plastics designed for
Fig. 5. Typical cyclic-type corrosion test chamber with PLC control for automatic operation of changeable atmospheres. temperatures, and durations of various steps in cyde.
severe service. This test meetS the challenges of providing a simulated service evaluation to test prod uct specifications in research and development and provide manufacturing controls for environmental changes caused by human intervention.
The B368 Standard is a variation on th e basic ASTM Bl17 Salt Spray (Fog) Test. For this variation, adjust the pH of the 5% salt solution into the range 6.0 to 7.0, and then add 0.25 grams of reagent-grade copper chloride per liter of salt solution. The test is not considered to start
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until the tem perature with in the exposure zone has reached 49 ° C + /-1°C (120° +/- 2_0 F) and is then run continuously for 6 to 170 hours as agreed upon between purchaser and seller pri or to th e start of the tes t. It is required that the temperature within the exposure zone be checked twice a day only on regular business days when the chamber may be periodically opened for "short" durations (preferably less than 5 min) to work with test pieces and/ or replenish solution.
Another variation from the standard salt spray (fog) test is in the mandatory verification fo r consistency of test exposu re conditions. In ASTM B using "Nickel Mass Loss Coupons" rather than steel (as used in the B 11 7 Practice, Section X3 [non-mandatory]). T he B368 Standard uses corrosion test chamber apparatus that meets the requirementS for the ASTM B 117 Standard and will withstand the increased temperature and stronger electrolyte solu tion used for this test.
ASTM G8S - Standar d Practice for Modified Salt Spray (Fog) Testing Five variations of this standard have been developed to accommodate its use to different purposes. The variation that is used by interested parties in any situation must be agreed upon prior to the start of testing. Followi ng are brief explanations of each of the five individual test variations:
Annex l-Acetic-Salt Spray (Fog) Testing The Acetic Acid-Salt Sp ray (Fog) Test is llsed to test ferrou s and nonferrous metals and inorganic and organic coatings for resistance to additional and more corrosive environments than the ASTM B117 Standard. Thi s test is designed as a continuous exposure test without interruptions. [t uses a 5 ± 1 part by mass solution of sodium chloride in 95 parts of ASTM 0 1193 Type IV water. The pH of the solution is adjusted with the addition o f glacial acetic acid to be within the range of 3.1 to 3.3. This solution is then
atomized into the exposure zone to
create a fog that has a condensate collection rate of 1.0 to2.0 m l/hr per 80 m 2 of horizontal collection area while the temperature of the exposure zone is being held at a constant 35 ° +/- 2 °C (95° +/- 3°F). This variation IS particularly useful 111
research when evaluating the effect of altering the parameters of an electroplating process or evaluating the quality of the process on decorative chromium plating. It is used primarily for steel and zinc die-casting substrates. It should be noted by llsers that even though this test is utilized as a more severe alte rnative to the ASTM Bl17 Salt Spray (Fog) test, the type of actual corrosion produced is not necessarily of a "like-kind" to that result ing from the B 117 test on the same test specimen material.
Annex 2- Cyclic Acidified Salt Fog Test For this variation the pH of the test solution is adjusted to a range of 2.8 to 3.0} the exposure zone temperature is raised to 49°C (120 °F), and the humidifying tower temperature is raised ro 57°C (135°F); however, the most significant change is the wet and dry cyclic nature of the test. Thi s change in the tes t requires that the test chamber be equipped with apparatus to produce differing atmospheres for the various steps in the test cycle and timing apparatus that wi ll cause the atmosphere within the cham ber co vary as follows. Every 6 hours, the test pieces will be exposed to 3/4 of an hour spray of atomized salt solution, then a 2-hr dry period, during which the chamber is pu rged of humidi ty. The final cycle is 1 % h ou rs of high humidity as described by the temperature and collection rates specified. Adding the cycles to this test increases its effectiveness if evaluating how products per fo rm in a continuously changing environment.
Annex 3- Acidified Synthetic Sea Water (Fog) Test The addition of 42 g of synthetic sea salt and 10 ml of glacial acetic acid
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featu refocus per liter of solution, in this variation, is to increase its usefulness for production control of exfoliationresistant heat treatments used in producing 2000, 5000, and 7000 series aluminum alloys. The pH is adjusted into the tange 2.8 to 3.0 and the test is performed at a tempetature of 49 °C (120°F). When using this variation to test organic coatings on metallic substrates the test is performed at a pre-selcC[ed temperature in the range 24 to 35°C (75-95 ° F). The collection tate specification for fog cycles of this test is unchanged from the B ll7 Standard at 1 to 2 mljht of operation; however, 2-hr cycles are used throughout the test period. Because of the cyclic nature of this tcst, prior to starting the test a separate 16-pOllf salt fog test is necessary (0 establish and verify proper condensate collection rates. The rest chamber m ust be equipped with apparatus and C011-
troIs that will cycle the exposure zone repeatedly through a lJ2 -hr spray step then 1 Ih hours of soak time at 98% relative humidity (see Fig 5).
An n ex 4- Salt/S02 Spray (Fog) Test In this test ei ther a sodium chloride or synthetic sea salt solution can be used. The determination of which will be used is dependent on the product being tested and the requirements of the interested parties. A primary difference in this test procedute is the addition of sulfur dioxide (S02) to the exposure zone using a predetermined cycle. The requirement of the ASTM G85, Annex 4 standard is that all the cycles during the test period be equal in length. Introducing S02 into the exposure zone on a periodic basis requires addi tional apparatus. T he chamber can be equipped with a device that wi ll disburse the S02 evenly throughout the chamber without directly impinging on any test pieces. The S02 supply source attached to the chamber must have a regulator, flow meter, and timer to allow for accurate introduction of
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S02 in accordance wi th any set cycle. It is impetative to address all safety issues: equipm ent, personnel, apparatus, and procedures prior to testing with S02' since it is a very hazardous highly toxic gas. Note that the primary changes to the chamber a re to allow for the correct introduction of the S02' All parts of the chamber that come in to contact with the S02 must be made of materials that are inert to S02 gas.
Annex 5- 0 ilu te Electro lyte Cyclic Fog/D ry Test For this test the electrolyte solution contains 0.05% sodium chloride and 0.35% ammonium sulfate in 0.60% by mass of ASTM 01193 Type IV water. This solution is much more dilure than the standard salt spray (fog) test and is run using 2-hr cycle times comprised of I-hr fog at ambient 24°C ±3°C and relative humidity below 75%, followed by 1-hr dry off at 35 ° C. That is, the test pieces are exposed to 1 hour of spray fog at controlled "room" temperature, then 1 hour d ry-off time at 35°C (95° F). T he collected condensate shall have a pH within the range of 5.0 to 5.4. Because of the cyclic nature of this test, a separate 16-hr salt fog test is necessary to establish and verifY proper condensate collection rates prior to starting the cyclic test. Because of the differences in humidity in this test method and the cyclic nature of the tes t, the chamber will need to have a separate air line and valve to allow the atomizing air to bypass the humidifying tower and timing apparatus to control the cycle times, temperature changes, spray, and airflow. This test is a modification of the British Rail uProhesion" test developed in the 1960s for th e industrial maintenance coatings industry. This test is best suited for the testing of paints on steel.
ASTM G87- Conducting M oist S02 Tests The ASTM G87 standard is an adaptation of the sulfur dioxide tests used in Europe and is particularly effective in producing easily visible
Fig. 6. Custom-sized. computer-controlled corrosion test chamber for cyclic testing.
corrosion on metals as would be observed in an industrial or marine environment. This test requires 2 ±0.2 L (122 in3 ±12 in 3) Type N water in the bottom of the test chamber and does not use a fogging apparatus. The apparatus used to generate the necessary humidity is the same used in the ASTM 02247 test. The gas introduction apparatus is the same as used in the ASTM G8S Annex 4 test. Once the test pieces are placed in the chamber 0.2, 1, or 2 L (12, 61, or 122 in3 ±12 in3) of sulfur dioxide (S02) with a purity of 99.9% (liquid phase) is introduced. Then the temperature of the chamber is raised to 40 ±oC (104 ±5.4°F) in 1 1(,
hours and remains at this level for the duration of the test cycle. One test cycle is 24 hours. A test can be run for as many cycles as are agreed upon between the purchaser and seller; however, the S02 and water must be changed for each 24-hr cycle.
The 24-hr test cycles are executed in one of the following ways: 1. Continuous - change of water and S02 with as little disturbance as possible 2. Alternating Exposute - 8-hr exposure; drying in ambien t for 16 hours with 20- 30°C (68- 86°F) and 75% relative humidity The variations differing from the B ll7 practice are that for this test method all test pieces be placed on the same horizontal plane and all test pieces in a given test run be of similar reactivity. NOTE: While adding corrosive gases may expedite degradation of the protective properties of the coating on the steel substrate, the purpose of the test must be kept in mind. This gas introduction may be acceptable when testing materials used in an environment that may include similar acids, such as roofing materials,
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featurefocus
Table m. Typical Uses aud Products Tested Under Various Test Standards
Research and Development, Quality Assurance. Marine Exposure Environments
Re&earch Studies. Quality Assurance
Research and Development, Quality Assurance
Quality A&5unmce, Development of heat treatment perimeters, and simulation of marine or near-shore environments or applications
Research and Development, Quality Assurance, and
,simulation of industrial, marine, or ncar-shore envirorunents or applications
Research and Development, Quality Assurance
Specification Acceptance, Service Evaluation. and Quality Assurance for severe iCtVice conditions
Evaluating Service Ufe for watcr.resistance coatings
Evaluating contamination of subltrate, inadequate surface preparation. and deficiencies in coatings
Research and Development, Quality Assurance
Product
Inorganic and organic coatings, aluminum. and other metals
Decorative chromium plate and materials resistant to long-tonn B 17 exposure as well as exfoliation of aluminum alloys
Electroplating and cadmium plating on steel or zinc die castings as well IIJ exfoliation of aluminum alloys
Exfoliation-resistant heat treatments on 2000, 5000, and 70Cl0 series aluminum alloys and materials, coatings, or equipment utilized in marine-type environments
Decorative electroplating. and materia]l, coatings. or equipment u,ti lized in industrial. aerpspace. and marine.type environments where corrosive pollutants. exhaust gases, or acid rain effects may be pre·sent
PalDts on steel
Anodized aluminum, decorative electroplating, design for severe service
Coatings, substrate treatments. and coating systems
Coating systems
Metals. coatiogs, and equipment used io lndustriaJ and marine-type environments where -, corrosive pollutants. exhaust gases, or acid rain effects may be present
ASTM Standard
B 117 Operating Salt Spray (Fog) Apparatus
G 8S-Annex 1 Acetic Acid Salt Spray
G 8S-Annex 2 Cyclic Acidified Salt Spray
G 8S-Annex 3 Acidified Synthetic Sea Water
G 8S-Annex 4 Salt SpraylSOz
G 85-Annex 5 Dilute Electrolyte Cyclic Fog/D'J'
B 368 Copper Accelerated Acetic Acid
o 1735 Water Fog Humidity
D 2247 100% Condensing Humidity
G 87 Moist SOz
that could be exposed to acid rai n. record ing capabili ties. Program mable logic con troller (PLC) syStems provide for increasingly sophisticated data acquisition, manipulation, and display (see Fig. 6). As a tesult, both test chambers with manual ly entered settings for automatic operation, and test chambers with increasingly sophisticated program mable controls for au tomatic temperature changes; varying levels of controlled hu midity; automatic changes fo r diffe rent envi ronmental atmosphere cycles; and au tomatic data logging/accumulatio n, record keeping, and output wi th graphic data display, are available through a variety of suppliers. These com prehensive capabilities allow each laboratory to find accelerated corrosion tes ting equipment that
EQU IPMENT With con tinued developmen ts in accelerated corrosion tes ting, basic changes and im provements h ave been made to the equipment. T he basic requiremen ts for accelerated corrosion testing equipment are listed on Table II under the ASTM Bll? Standard. The adjustments required for each variation on th e accelerated corrosion-tes ting model are t hen listed next to the appropt iate ASTM standard. Typical applications are listed in Table III. Along wi th the basic opera ting requirements, improvements h ave been made in the materials used in th e conStruction of the chambers, the hardware and software coo t roIs, and data
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meets their specific n eeds.
TEST PIECE PREPARATION! CLEANING In order for any of th e above accelerated corrosion tests to obtain comparable results, all test pieces must start the test in a similar condition without contaminants p resen t on the surface of interest. The ASTM tes t standards discussed above indicate reference standards to be used for the preparation and cleaning of tes t pieces. Pa rticular a ttention must be paid to the wide variety of materials being cleaned an d recognition of diffe ring specialized matetial and coating operations. ASTM test s tandards s tate that th e cleaning method is to be dependen t on the p roduct being cleaned and then refet to ASTM D 609 Standard Practice fo r Preparation of ColdRolled Steel Panels for Testing Paint, Varnish, Conversion Coatings and Related Coating Prod ucts where required. This stan dard describes five cleaning and preparation methods. The preparation method s described are: Procedure AConversion Coating; Procedure BVapor D egreasin g; Procedure CSolvent Brushing; Procedu re D Solvent Wiping; and Procedure EAlkaline Cleaning. Procedure A (Conversion Coating) addresses the issue of ensuring that th e test piece be protected from rusting between the manufacturing process and the corrosion test. Procedure B (Vapor Degreasing) exposes the test pieces to solvent vapors within controlled conditions to remove contaminants. Th is procedure is currently discouraged for environmen tal reasons. Procedures C (Solvent Brushing) and D (Solvent Wiping) both use Mineral Spiri t s as t he clean ing agent. Procedure E (Alkali ne Cleaning) desctibes methods for cleaning with an alkaline cleaning agent that is appropriate fo r the product. T he cleaning method and cleaning agent chosen for any test run should be as agreed upon between the purchaser and seller. ASTM D609 refers to the water break test as a method of checking test
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featu refocus pieces for contaminants. The procedure is simply to run a small amount of water over the surface of the tcst piece. If it is free of oils and contaminants the water will run over it in a sheet and off in one fall with no breaks. Finally, ASTM 0609 discusses the handling of cleaned test pieces and storage in paper impregnated with volatile corrosion inhibitor (VCI) if the test pieces are not to be run immediately after cleaning.
EVALUATION OF RESULTS Some primary ASTM Standards that have been developed to assis t in the evaluation of corrosion test results are: ASTM 01654- Standard Test Method fo r Evaluation of Painted or Coated Specimen Subjected to
Co rrosive Environments; ASTM 0610-Standard Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces; ASTM 0714-Standard Test Method for Evaluating Oegtee of Blistering of Paints; and ASTM B537-Standard Practice for Rating of Electroplated Panels Subjected to Atmospheric Exposure. Irrespective of the title wording, the text of ASTM B537 states that it is also used to evaluate panels subjected to laboratory accelerated corrosion tests. Other standards are also available for evaluation of specific materials and finishes.
ASTM 0 1654 is used for the evaluation of substrates, pretreatments, coating systems, or a combination thereof. This standard is also used when the coating has been scribed prior to exposure to the corrosive environment. ASTM 01654 recommends a straight-shank tungsten carbide tip or equivalent scribing tool to produce a cut through the coating to the substrate of the test piece. The scribe serves as a deliberate failu re of the coating system prior to corrosion testing. Once the test piece has been thro ugh the selected accelerated corrosion test it is then cleaned by rinsing with a gentle stream of water at 45°C (llO°F). Loose coating is then removed using compressed air to blow it off or a scraper to scrape it off. The "creep-
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back)) (perpendicular distance of failure from the scribe line) of the coating is measured at uniform intervals and the rating sys tem described in the standard appl ied.
ASTM 0610 provides a series of photographic reference standards that demonstrate degrees of rust on the surface of a test piece. The rest pieces are first gently cleaned then the amount of rust observed is reported from comparison to the photographic standards and the additional use of established standardized terminology from the test standard. It is important to compare only rust and nOt surfaces stained by rust.
ASTM 0714 is used to evaluate coating adhesion by observing the amount of blistering that has occurred. The test pieces are first gently cleaned then compa red to the series of included photographic references and the additional use of the appropriate "standardized)) terminology indicated in the test standard. They are graded first by the size of the blisters that appear on the surface and then the number of blisters that appear per unit area.
products and materials. T hese standards have been developed, evolved and refined through cooperative efforts of experts and interested parties from: ASTM International, industry, government, and oth er trade o rganizations worldwide.
ABOUT THE AUTHOR Ray Singleton is the Chairperson for the ASTM Cabinet Corrosion Tests (committee G.D1.0S. 03) and Vice-Chairperson for ASTM Corrosion of Metals (committee G.01) and Vice-Chairperson for ASTM Laboratory Corrosion Tests (committee G.0l-05) as well as the composer/ instructor for the ASTM TPT (Technical Professional Training) Corrosion Testing course for the last 14 years. He has written various magazine articles and contributed to industry directories on this topic over the years. Singleton was also presented with the Francis L LaQue award by ASTM in 2010 for contributions corrosion testing and the field of corrosion technology.
CONCLUSION Th e corrOSIOn tests discussed in this article are some of the most utilized tests of this type. They also demonstrate the diversity of the tests and some of the advancements in accelerated corrOSIOn testing and complexity of th e subject. They also provide a solid basis for evaluating the performance of a wide variety of www.metalfinishing.com/advertisers
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