Astm D7356 07
Astm D7356 07
Designation: D7356 − 07
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xenon-arc light source with daylight filter conforming to the
requirements of Practice G155. Specimens are sprayed with a
3. Terminology
simulated acid rain solution and requires the use of a
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3.1 Definitions—Definitions applicable to this standard can
horizontal, flat specimen array in order to allow the acid rain
be found in Terminology G113.
solution to remain on the test specimens for an extended period
of time. 3.2 Definitions of Terms Specific to This Standard:
1.3 There is no known ISO equivalent to this test ASTM
method.D7356-07
3.2.1 acid rain, n—cloud or rain droplets containing
pollutants, such as oxides of sulfur and nitrogen, to make them
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1.4 The values stated in SI units are to be regarded as
acidic.
standard. The values given in parentheses are for information
only. 3.2.2 acid rain spots, n—spots are produced when the sun
evaporates standing water on the vehicle’s surface.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.2.2.1 Discussion—They fall into two categories, mineral
responsibility of the user of this standard to establish appro- deposits and acid-etched spots. Mineral deposits are white
priate safety and health practices and determine the applica- calcium spots or salt deposits left on the surface after water
bility of regulatory limitations prior to use. evaporates. These deposits can be easily removed with a
pre-wax cleaner (polish) or a clay bar. Acid-etched spots are
depressions in the paint or clear coat, which cannot be easily
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint removed.
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.27 on Accelerated Testing.
Current edition approved June 1, 2007. Published June 2007. DOI: 10.1520/
4. Summary of Test Method
D7356-07. 4.1 The Automotive Clearcoat coating being evaluated is
2
The acid etch test method is covered by a patent. Interested parties are invited
to submit information regarding the identification of an alternative(s) to this applied to an automotive basecoat (typically black) that has
patented item to ASTM International Headquarters. Your comments will receive
careful considerations at a meeting of the responsible technical committee,1 which
you may attend.
3 4
Brennan, P. J, Marino, M., Boisseau, J. and Campbell, D., Accelerated Acid For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Etch, Part II: Refined Test Procedure to Reproduce Automotive Acid Etch Provides contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Improved Lab Practicality and Proven Correlation, FSCT, 2006 FutureCoat Pro- Standards volume information, refer to the standard’s Document Summary page on
ceedings. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
D7356 − 07
been coated onto a steel panel. All edges of the panel are sealed 6.3 pH meter capable of measuring to 60.2 units.
to prevent corrosion. Coatings applied to other types of panels
may also be used. 7. Reagents and Materials
4.2 Test specimens are placed in a xenon-arc device 7.1 0.02 N H2SO4 Sulfuric Acid Volumetric Solution, (accu-
equipped with a horizontal exposure rack and are exposed to rate to 61 part per 1000).
alternating periods of light, spray with acid rain solution, and
7.2 0.3 % HNO3 (Nitric Acid), by weight or v/v.
spray with water. The evaporation of the water from the acid
solution on the test specimen surface results in deposits with 7.3 0.02 N NaOH Sodium Hydroxide Volumetric Solution,
high acid concentration. (accurate to 6 1 part per 1000).
4.3 After 400 hours of exposure, test specimens are evalu- 7.4 0.01 M CaCl2, (Calcium Chloride Standard for water
ated and rated for etch. hardness testing).
5. Significance and Use 7.5 0.01 M KCl (Potassium Chloride) Conductivity
Solution, calibration standard solution 1413 micro-ohms.
5.1 Acid etch damage is an important warranty claim item
for automotive companies. As a result, acid etch resistance is 8. Apparatus Setup
an important parameter for automotive exterior coatings. The
method described in this test method has been shown to 8.1 Operate, maintain and calibrate the apparatus to manu-
simulate acid etch damage of automotive clearcoats that occurs facturer’s specifications. The test should not be interrupted
when such coatings are exposed from May through mid- once it has started (excluding daily panel reposition). Calibra-
August in Jacksonville, FL.3,5 The accelerated test described in tions and maintenance should be completed before the test
this standard allows year-round testing as opposed to the starts or after the test has completed.
limited outdoor exposure time available for the Jacksonville, 8.2 Water used for spray and humidification shall have a
FL exposures. maximum of 1 ppm total solids and a maximum of 0.2 ppm
silica. Unless otherwise specified, determine silica levels in
6. Apparatus
iTeh Standards
6.1 Xenon-arc exposure device conforming to Practice
accordance with Practice D4517. A combination of deioniza-
tion and reverse osmosis treatment can effectively produce
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G151 and Practice G155 with the following additional require- water with the desired purity.
ments.
8.3 Acid Rain Solution—The composition for the acid rain
6.1.1 Specimen rack that is within 63 degrees of horizontal.
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solution is as follows:
6.1.2 Means to spray pure deionized water and acid rain
8.3.1 Add 977.5 g of deionized water to a 1 litre flask and
solutions independently, and without cross contamination,
from one another. then add the following:
15.0 grams – 0.02 N H SO4 (Sulphuric Acid)
NOTE 2—Use of dual spray systems, one for acid solutionASTM D7356-072.2 grams – 0.3 % HNO2 3 (Nitric
and the other Acid)
for high purity water has been found to be effective for eliminating cross
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contamination.
2.5 grams – 0.02 N NaOH (Sodium Hydroxide)
1.8 grams – 0.01 M CaCl2 (Calcium Chloride)
6.1.2.1 The volume of spray water shall be sufficient to 1.0 grams – 0.01 M KCl (Potassium Chloride)
flood (with excess) the surface of the specimen within the 8.3.2 This provides a 1000 g (1 L) solution with a pH of 3.3
one-minute spray time. A spray delivery rate of 3 litres per to 3.5, which is similar to that of Jacksonville rain water.
minute per square metre has been found suitable.
8.3.3 After the water has cooled to room temperature and
6.1.3 Use of a single spray system has not been evaluated. If
stirred for 24 hours, measure the pH of the solution with a pH
a single spray system is used, the following shall be included
meter following Practice D1293. If the solution pH is not
with the test report:
between 3.3 and 3.5 make a new solution.
6.1.3.1 If a single spray system is used for both the acid
solution and high purity water, data verifying that there is no 8.4 Expose the test specimens to the cycle shown in Table 1.
cross contamination between the acid spray and the high purity 8.4.1 Refer to Table X.3.2, Operational Fluctuations on
water spray. Exposure Conditions, in Practice G155 for the maximum
6.1.4 Xenon-arc apparatus shall be equipped with daylight allowed fluctuations about the set points. If the operational
filters that meet the requirements of Practice G155. fluctuations are greater than the maximum allowed after the
6.1.5 Xenon-arc apparatus shall be able to simultaneously equipment has stabilized, discontinue the test and correct the
and automatically control irradiance, black panel temperature, cause of the problem before continuing.
relative humidity and chamber air temperature.
6.2 Xenon-arc apparatus shall be equipped with an uninsu- 9. Test Procedure
lated black panel complying with Practice G151. 9.1 Apply coating to be evaluated to the desired substrate.
After coating is applied and dried or cured, seal any cut edges
5
Boisseau, J. and Pattison, L., BASF Corporation, and Henderson, K. and Hunt,
of the test specimens. An air-dry primer or silicone sealant has
R., Bayer Material Science, “The Flaws in Accelerated Weathering of Automotive been found to be suitable for sealing cut edges. The exposed
OEM Coatings,” Paint and Coatings Industry, June 2006. surface of all test specimens must be clean and free from finger
2
D7356 − 07
TABLE 1 Accelerated Acid Etch Exposure Cycle Sequence
Accelerated Acid Test Exposure Cycle
Step 1 1 min Dark exposure; with acid rain spray
Step 2 3 hr 50 min Dark exposure; 40°C uninsulated black panel (B.P.) temperature (monitored not controlled); 40°C chamber air
temperature; 80 % RH
Step 3 12 hr Light exposure; 0.55 W/m2/nm at 340 nm; daylight filters; 65°C uninsulated B.P.; 50°C chamber air temperature; 80 %
RH
Step 4 27 min Dark exposure; 40°C uninsulated B.P. temperature (monitored not controlled); 40°C chamber air temperature; 80 % RH
Step 5 1 min Dark exposure; with pure water (DI) spray
Step 6 3 hr 50 min Dark exposure; 40°C uninsulated B.P. temperature (monitored not controlled); 40°C chamber air temperature; 80 % RH
Step 7 1 min Dark exposure; with pure water (DI) spray
Step 8 3 hr 50 min Dark exposure; 40°C uninsulated B.P. temperature (monitored not controlled); 40°C chamber air temperature; 80 % RH
Note–Chamber air temperature and black panel temperature are controlled during the light period. Chamber air is controlled during the dark steps and the uninsulated
black panel temperature is monitored. The % RH is controlled during light and dark periods where specified.
prints or other surface contaminants. All other procedures for 10. Evaluation Report
specimen handling and identification shall be in accordance 10.1 The evaluation of acid damage is performed visually
with Practice G147. and the test specimen is rated on a scale from 0 (best) to 10
9.2 Place specimens in the xenon-arc exposure device and (worst). A summary of the rating scale is shown in Table 2 and
program the device to run the exposure cycle described in
Table 1, starting at Step 1 (dark exposure with acid spray). TABLE 2 Acid Etch Evaluation Ratings
Unless otherwise specified, set the device timer to provide a
Rating Description
400 hour exposure. Refer to the device manufacturer’s instruc- 0 to 3 The etch spots are very faint and only noticed by a trained observer
tions for proper operation. 4 to 6 The etch spots are slight to moderate and in some cases noted by a
9.2.1 Once the exposure has started, do not interrupt the vehicle owner (untrained observer)
iTeh Standards
7 to 10 The etch spots are severe enough that many vehicle owners would
exposure more than once per day. The single test interruption notice and complain
shall be for specimen repositioning and placement or removal.
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Additional interruptions may increase variability of test results.
9.3 The volume of water and acid spray for the test must be Table 3. Other evaluations can be used if agreed up by parties
excessive, running off the panels. A spray volume of at least 3
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litres per min per square metre has been found acceptable. Preview
concerned. Example of pictorial ratings are shown in Appendix
X2.
9.4 Periodic repositioning of specimens during the exposure
period is required to ensure that each receives an equal amount 11. Exposure Report
ASTM
of exposure to the acid solution and pure water spray. Repo- D7356-07
11.1 The exposure report is as agreed upon by contractual
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sition the panels daily during the light cycle. Follow the parties.
manufacturers guidelines for the repositioning pattern. See Fig. 11.2 The Exposure Control/Report form shall include the
1 for an example of how samples are repositioned. Reposition- following additional information:
ing of specimens on the weekends is not required. 11.2.1 Laboratory Name.
9.5 Report the acid damage as agreed upon by contractual 11.2.2 Type and serial number of exposure equipment.
parties. 11.2.3 Month and Year of equipment operation.
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D7356 − 07
TABLE 3 Detailed Acid Etch Ratings
Rating Description Skill Level
0 No damage N/A
1 Slight pitting damage, no acid etch spots trained observer
2 Moderate pitting – no acid etch spots trained observer
3 Few full or partial acid etch spots start trained observer
4 Full acid etch spots start to appear (light) untrained observer
5 Full acid etch spots, inc. frequency, few deeper spots untrained observer
6 Inc. frequency, inc. depth, borderline paint repair untrained observer
7 Frequency and depth would require repaint all observers
8 Start to see acid etch spots overlap previous spots all observers
9 Inc. frequency, depth of spots, overlap all observers
10 High % area damaged, spots overlap, discoloration all observers
11.2.4 Test method. 12.1.1 The Spearman rank correlation coefficient was 1.0
11.2.5 Frequency of operation verification, for example, for all possible comparisons between the different sets. The
three or seven day intervals. Pearson linear correlation coefficients for comparisons of the
11.2.6 Daily record of black panel temperature (BPT). data in the different sets were as follows:
11.2.7 Daily record of chamber temperature. Set 1 to Set 2 = 0.92
11.2.8 Daily record of irradiance. Set 1 to Set 3 = 0.93
Set 1 to Set 4 = 0.98
12. Precision and Bias
Set 2 to Set 3 = 0.99
12.1 The test results are a visual comparison to a pictorial Set 2 to Set 4 = 0.94
standard and the ranking of the test sets. The repeatability
standard deviation (Table 4) has been determined to be: 12.2 The reproducibility of this test method is being deter-
TABLE 4 Repeatability for Lab A mined and will be available on or before 2012.
iTeh Standards
Standard
Coating Set #1 Set #2 Set #3 Set #5 Mean
13. Keywords Deviation
Paint A 3 5 4 6 4.5 1.29
Paint B 6 6 6 7 13.1 accelerated weathering; acid etch; acid rain; automo-
6.25 0.50
Paint C
Paint D
7
10
9
10
9
10(https://standards.iteh.ai)
8
10
8.25 0.96
tive; clearcoats; Jacksonville; xenon-arc
10 0.00
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APPENDIXES
ASTM D7356-07
(Nonmandatory Information)
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X1. ACCELERATED WEATHERING XENON ACID ETCH TEST FOR AUTOMOTIVE CLEARCOATS
X1.1 Acid etch images. See Fig. X1.1, Fig. X1.2, Fig. X1.3,
and Fig. X1.4.