Cass Test Astm B 368 PDF

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Designation: B 368 – 97 (Reapproved 2003)e1

Standard Test Method for


Copper-Accelerated Acetic Acid-Salt Spray (Fog) Testing
(CASS Test) 1
This standard is issued under the fixed designation B 368; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

This standard has been approved for use by agencies of the Department of Defense.

e1 NOTE—Sections 8.1 and 10.1.12 were editorially updated in July 2003.

1. Scope B 456 Specification for Electrodeposited Coatings of Cop-


1.1 This method prescribes the conditions required in per Plus Nickel Plus Chromium and Nickel Plus Chro-
copper-accelerated acetic acid-salt spray (CASS) testing for mium4
specification purposes. The standard does not specify the type B 537 Practice for Rating of Electroplated Panels Subjected
of test specimen or exposure periods to be used for a specific to Atmospheric Exposure4
product, nor the interpretation to be given to the results. B 602 Test Method for Attribute Sampling of Metallic and
1.2 This method is applicable to evaluating the corrosive Inorganic Coatings4
performance of decorative copper/nickel/chromium or nickel/ B 604 Specification for Decorative Electroplated Coatings
chromium coatings on steel, zinc alloys, aluminum alloys, and of Copper Plus Nickel Plus Chromium on Plastics4
plastics designed for severe service. It is also applicable to the D 1193 Specification for Reagent Water5
testing of anodized aluminum. The suitability of this test and E 50 Practices for Apparatus, Reagents, and Safety Consid-
correlation of results with service experience should be deter- erations for Chemical Analysis of Metals, Ores, and
mined before it is specified for coating systems or materials Related Materials6
other than those mentioned in this paragraph. 3. Significance and Use
NOTE 1—The following standards are not requirements. They are 3.1 The CASS test is widely employed and is useful for
referenced for information only: Practices B 537 and E 50, Specifications
specification acceptance, simulated service evaluation, manu-
B 456 and B 604, and Test Method B 602.
facturing control, and research and development. It was devel-
1.3 This standard does not purport to address all of the oped specifically for use with decorative, electrodeposited
safety concerns, if any, associated with its use. It is the nickel/chromium and copper/nickel/chromium coatings. Use of
responsibility of the user of this standard to establish appro- the test has improved the quality of electroplated parts and led
priate safety and health practices and determine the applica- to the development of new and superior electroplating pro-
bility of regulatory limitations prior to use. For more specific cesses.
safety precautionary information see 8.1.
4. Apparatus
2. Referenced Documents
4.1 The apparatus required for the CASS test consists of a
2.1 ASTM Standards: fog chamber, a salt-solution reservoir, a supply of compressed
B 117 Practice for Operating Salt Spray (Fog) Apparatus2 air, one or more atomizing nozzles, specimen supports, provi-
B 162 Specification for Nickel Plate, Sheet, and Strip3 sion for heating the chamber, and necessary means of control.
4.2 The size and detailed construction of the apparatus are
1
optional, provided the conditions meet the requirements of this
This method is under the jurisdiction of ASTM Committee B08 on Metallic and
Inorganic Coatings and is the direct responsibility of Subcommittee B08.10 on Test method. The construction of the apparatus is described in the
Methods. appendix of Test Method B 117. For the CASS test, however,
Current edition approved May 10, 2003. Published July 2003. Originally
approved in 1961. Last previous edition approved in 1997 as B 368 – 97.
The CASS test was developed by the initiative of the Research Board of the
4
American Electroplaters Society under AES Project 15. Annual Book of ASTM Standards, Vol 02.05.
2 5
Annual Book of ASTM Standards, Vol 03.02. Annual Book of ASTM Standards, Vol 11.01.
3 6
Annual Book of ASTM Standards, Vol 02.04. Annual Book of ASTM Standards, Vol 03.05.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
B 368 – 97 (2003)e1
the requirements for air pressure and temperature are typically regulator valve minimizes the possibility that the nozzle will be operated
0.08 to 0.12 MPa and 60 to 65°C, respectively. The actual air at its critical pressure.
pressure will be that required to produce the proper collection
rate (see 8.3.1). 7. Test Specimens
4.3 The apparatus shall be constructed so that drops of 7.1 The type and number of test specimens to be used, as
solution that accumulate on the ceiling or cover of the chamber well as the criteria for the evaluation of the test results, shall be
do not fall on the specimens being tested. Drops of solution defined in the specifications covering the material or product
that fall from the specimens shall not be returned to the being tested or shall be mutually agreed upon between the
solution reservoir for respraying. purchaser and the supplier.
4.4 Materials of construction shall not affect the corrosive-
ness of the fog, nor be themselves corroded by the fog. 8. Procedure
8.1 Preparation of Test Specimens— Clean metallic and
5. Test Solution metallic coated specimens. Unless otherwise agreed upon,
5.1 Prepare the salt solution by dissolving 5 parts by weight clean decorative copper/nickel/chromium or nickel/chromium
of salt in 95 parts of water conforming to Specification D 1193, coatings immediately before testing by wiping significant
Type IV. The salt shall be sodium chloride (NaCl), ACS reagent surfaces with a cotton pad saturated with a slurry containing 10
grade, or equivalent. The pH of this solution shall be between g of pure magnesium oxide powder (ACS reagent grade) in 100
6.0 and 7.0. Impurities or contam-ination of either the salt or mL of distilled water. Upon rinsing in warm running water, be
the water, or both, should be suspected if the pH is outside of sure that the clean surface is free of water break. Anodized
this range (Note 2). aluminum parts may be cleaned with inhibited 1,1,1-
5.2 Add 0.25 g of reagent grade copper chloride (CuCl trichloroethane or other suitable organic solvent (see Warning).
2·2H2O) to each litre of the salt solution; dissolve and mix Do not clean organic and other nonmetallic coated specimens.
thoroughly. Other methods of cleaning, such as the use of a nitric-acid
5.3 The pH of the salt-copper solution shall be adjusted to solution for the chemical cleaning or passivation of stainless
the range of 3.1 to 3.3, as measured on a sample of the steel specimens, are permissible when agreed upon between
collected spray, by the addition of glacial acetic acid, ACS the purchaser and the supplier. Take care that the specimens
reagent grade, or equivalent (Note 3). The pH measurement after cleaning are not recontaminated by excessive or careless
shall be made electrometrically at 25°C. Before the solution is handling. Protect the cut edges of plated, coated, or multilay-
atomized, it shall be free of suspended solids (Note 4). ered materials and areas containing identification marks or in
NOTE 2—A solution having a specific gravity of 1.030 to 1.040, when
contact with the racks or supports with a coating that is stable
measured at a temperature of 25°C, will meet the concentration require- under the conditions of the test, such as wax, stop-off lacquer,
ment. It is suggested that a daily check be made. or pressure-sensitive tape. (Warning—1,1,1-Trichloroethane
NOTE 3—The initial solution may be adjusted to a pH of 3.0 to 3.1, with should be used in a well-ventilated area away from open
the exception that the pH of the collected fog will be within the specified flames.)
limits. Adjustment of the initial pH for makeup solution is based upon the 8.2 Positioning of Specimens—Position the specimens in
requirements to maintain the required pH of the collected samples. If less the CASS test chamber during the test so that the following
than 1.3 or more than 1.6 mL of the glacial acetic acid are required per litre
conditions are met:
of sodium chloride and copper solution to attain the specified pH, some
discrepancy in the system may be suspected (the purity of the water or 8.2.1 Support or suspend the specimens 15 6 2° from the
salt, or both; the accuracy of the pH meter; the general cleanliness of the vertical and preferably parallel to the principal direction of
system; etc.). horizontal flow of fog through the chamber, based upon the
NOTE 4—The freshly prepared salt solution may be filtered or decanted dominant surface being tested. Support or suspend automobile
before it is placed in the reservoir, or the end of the tube leading from the parts, however, so as to expose all significant surfaces at the
solution to the atomizer may be covered with a double layer of cheese general level of the condensate collectors. If the position on the
cloth to prevent plugging of the nozzle.
automobile is vertical, place the part in an incline position 15°
6. Air Supply from vertical to allow surface wetting by the condensate. If the
position on the automobile is facing down, rotate the part
6.1 The compressed air supply to the nozzle or nozzles for approximately 180° to test the significant surface. If there are
atomizing the test solution shall be free of oil and dirt (Note 5). several significant surfaces at different angles, expose each
Pressure shall be adequate to provide a specified condensate surface of one or more specimens.
rate. Pressure of 0.10 6 0.02 MPa has been found satisfactory 8.2.2 Make sure the specimens do not come in contact with
(Note 6). each other or any other metallic material or any material
NOTE 5—The air supply can be freed of oil and dirt by passing it capable of acting as a wick.
through a water scrubber or at least 60 cm of suitable cleaning material, 8.2.3 Place each specimen so as to permit free settling of fog
such as sheep’s wool, excelsior, slag wool, or activated alumina. Com- on all specimens.
mercial filters for compressed air may be used.
8.2.4 Make sure the salt solution from one specimen does
NOTE 6—Atomizing nozzles may have a critical pressure, at which an
abnormal increase in the corrosiveness of the salt fog occurs. If the critical not drip on any other specimen.
pressure of a nozzle has not been determined with certainty, control of 8.2.5 Place the specimens in the chamber just prior to
fluctuation in the air pressure within 60.0007 MPa by installing a pressure bringing the test chamber to the required temperature and

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B 368 – 97 (2003)e1
turning on the air, since storage in an idle chamber overnight, when measured at 25°C, will meet the concentration requirement. The
or for other significant length of time, can affect test results. concentration may also be determined as follows: Dilute 5 mL of the
collected solution to 100 mL with distilled water and mix thoroughly;
NOTE 7—Suitable materials for the construction or coating of racks and pipet a 10-mL aliquot into an evaporating dish or casserole; add 40 mL of
supports are glass, rubber, plastic, or suitably coated wood. Bare metal distilled water and 1 mL of 1% potassium chromate (K2CrO4) (ACS
should not be used. Specimens are preferably supported from the bottom reagent grade with less than 0.005% chloride) and titrate with 0.1 N silver
or the side. Slotted wooden strips are suitable for the support of flat panels. nitrate (AgNO3) (ACS reagent grade) solution to the first appearance of a
Suspension from glass hooks or waxed string may be used as long as the persistent red coloration. A test solution that requires between 3.9 and 4.9
specified position of the specimens is obtained. If necessary, such mL of 0.1 N Ag NO3 solution will meet the concentration requirements.
suspension may be made by means of secondary support at the bottom of NOTE 12—It has not been found necessary to check copper concentra-
the specimens. tion of the collected solution.
8.3 Conditions in the Salt-Spray Chamber—Maintain the NOTE 13—Factors that may contribute to dilution and evaporation of
exposure zone of the CASS test chamber at a temperature of condensate and make it difficult to control the concentration are lower
496 1°C during the exposure period (Note 8). After closing the temperature, inadequate cover insulation, and prolonged storage of test
solution at above room temperature.
test chamber, bring the temperature to 49°C before the fog is
turned on. The test duration shall commence when the tem- 8.3.2 Direct or baffle the nozzle or nozzles so that none of
perature is 49 6 1°C and fog is present in the chamber. Heat the spray can impinge directly on the test specimens.
the air supply by passing fine bubbles through heated distilled 8.4 Continuity of Test—Unless otherwise specified in the
or deionized water (see Specification D 1193, Type IV) so that specification covering the material or product being tested, the
the temperature of the air after expansion at the nozzle is 49 6 test shall be continuous for the duration of the entire test
1°C. Record the temperature within the exposure zone of the period. Continuous operation implies that the chamber be
closed cabinet (Note 9) twice a day at least 7 h apart (except closed and the spray operating continuously, except for the
Saturdays, Sundays, and holidays, when the salt-spray test is short daily interruptions necessary to inspect, rearrange, or
not interrupted for exposing, rearranging, or removing test remove test specimens, to check and replenish the solution in
specimens or to check and replenish the solution in the the reservoir, and to make necessary recordings as described in
reservoir). 8.3. Schedule operations so that these interruptions are held to
NOTE 8—This can be best accomplished by preheating the chamber to
a minimum.
49°C before starting solution atomization. 8.5 Period of Test—Designate the period of test by the
NOTE 9—A suitable method to record the temperature is by a thermom- specifications covering the material or product being tested or
eter that can be read from outside the closed cabinet. The recorded as mutually agreed upon between the purchaser and the
temperature must be obtained with the salt-spray chamber closed to avoid supplier.
a false low reading, because of wet-bulb effect when the chamber is open.
Automatic control of temperature in the chamber and a continuous record NOTE 14—Typical exposure periods are: 6, 16, 22, 48, 96, 192, 240,
of temperature are desirable. 504, and 720 h.

8.3.1 Place at least two clean fog collectors within the 8.6 Cleaning Tested Specimens—Unless specified in the
exposure zone so that no drops of solution will be collected specifications covering the material or product being tested,
from the test specimens or any other source. Position the carefully remove specimens at the end of the test, rinse gently
collectors in the proximity of the test specimens, one nearest to in clean, running, warm water (38°C, max) to remove salt
any nozzle and the other farthest from all nozzles. A preferred deposits from their surfaces, and then dry immediately. To dry
arrangement is shown in Fig. 1. Make sure that the fog is such the specimens use a stream of clean, compressed air at 0.25 to
that for each 80 cm2 of horizontal collecting area each collector 0.30 MPa gage pressure.
collects from 1.0 to 2.0 mL/h of solution, based on a typical run NOTE 15—If steel parts are rinsed immediately after removal from the
of at least 22 h (Note 10). Maintain the sodium chloride test chamber, small rust spots or flakes of rust may lift off and be rinsed
concentration of the collected solution between 4.5 and 5.5 away. It is then difficult to tell where the spots had been. If, after removal
mass % (Note 11 and Note 12). Dilution and evaporation of from the test chamber, the part is allowed to dry 30 to 60 min before
condensate should be avoided (Note 13). rinsing, all corrosion spots are easily visible. This not does not apply to
zinc-die castings.
NOTE 10—Suitable collecting devices are glass funnels with the stems
inserted through stoppers into graduated cylinders. Funnels with a 8.7 Calibration of Corrosive Conditions—This procedure
diameter of 10 cm (area of about 80 cm2) and 50-mL cylinders are for calibration and standardization of the corrosive conditions
preferred. within the cabinet involves exposure of nickel test panels and
NOTE 11—A solution having a specific gravity of from 1.030 to 1.040, determination of their mass loss in a specified period of time.
This may be done monthly or more frequently to make sure the
cabinet is operating within the limits specified in 8.7.4.
8.7.1 Use nickel panels that are 7.5 by 10 cm, approximately
0.09 cm thick, and made from the higher carbon grade (0.15%
max) given in Specification B 162.
8.7.2 Place one weighed nickel test panel in each corner of
the cabinet with the 10-cm length inclined 30° to the vertical
using plastic supports that are about 1.5 by 4 by 7.5 cm. The
FIG. 1 Arrangement of Fog Collectors four test panels should be on the inboard side of the condensate

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B 368 – 97 (2003)e1
collectors parallel to the cabinet length. Make sure the top of 10.1.4 Daily records of data obtained from each fog collect-
the panels are at the same level as the top of the condensate ing device, including the following:
collectors. 10.1.4.1 Volume of salt solution collected in (mL/h)/8 cm 2,
8.7.3 Expose the test panels to 22 h of CASS testing, 10.1.4.2 Concentration or specific gravity at 25°C of solu-
recording test operating conditions on the data sheet as usual. tion collected, and
Remove the panels from the cabinet and rinse each in reagent 10.1.4.3 pH of solution collected,
grade water (see Specification D 1193, Type IV) to remove 10.1.5 Nickel panel corrosion rate calibration,
salt. Immerse each panel in 20% by volume hydrochloric acid 10.1.6 Type of specimen and its dimensions, or number, or
prepared with distilled water for 2 min at 20 to 25°C using description of part,
nickel-copper alloy 400 (UNS N04400) tongs. The tongs may 10.1.7 Method of cleaning specimens,
be nonmetallic or another material that will not affect the mass 10.1.8 Method of supporting or suspending the article in the
loss of the nickel by galvanic action. Rinse each panel in water salt-spray chamber,
at room temperature and then in warm (38°C) flowing water. 10.1.9 Description of protection used as required in 8.1,
Dry panels in an oven at 100°C for 10 min. Allow the panels 10.1.10 Exposure period,
to reach room temperature and weigh immediately on an 10.1.11 Interruptions in the test, cause and length of time,
analytical balance. and
8.7.4 Determine the mass loss of each panel by subtracting 10.1.12 Results of inspections.
its weight after exposure from its initial weight. Determine the NOTE 16—If any of the atomized salt solution that has not come in
corrosive loss by dividing the mass loss by the area of one face contact with the test specimens is returned to the reservoir, it is advisable
of the test panel (77.5 cm2). The corrosive rate shall be 0.45 to to record the concentration or specific gravity and the pH of this solution
0.85 mg/cm2 to satisfy the requirements of this method. also.
NOTE 17—Round robin testing revealed the inability to exhibit repeat-
9. Evaluation of Results ability of the mass loss requirements of 8.7.4. Further testing is ongoing
9.1 A careful and immediate examination shall be made for to clarify the root causes.
the extent of corrosion of the dry-test specimens; or for other
failure, as required by the specifications covering the material 11. Precision and Bias
or product being tested; or by agreement between the purchaser 11.1 The reliability, reproducibility, and accuracy of the
and the supplier. CASS test depends on proper and consistent control of a
number of factors, including:
10. Records and Reports 11.1.1 Cleaning of the test samples,
10.1 The following information shall be recorded, unless 11.1.2 Positioning of the specimens and samples in the test
otherwise prescribed in the specifications covering the material cabinet,
or product being tested: 11.1.3 Rate of condensation within the test cabinet,
10.1.1 The title, designation and year of issue of this 11.1.4 CASS solution makeup,
method. 11.1.5 Cabinet maintenance, and
10.1.2 The salt, water, copper chloride, and acetic acid used 11.1.6 Calibration of corrosive conditions.
in preparing the salt solution, 11.2 The precision and bias of the CASS test is being
10.1.3 All readings of temperature within the exposure zone determined and will include study of the reproducibility of the
of the chamber, calibration procedure described in 8.7.

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