Astm D4752 20

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4752 − 20
Standard Practice for

Measuring MEK Resistance of Ethyl Silicate (Inorganic)
Zinc-Rich Primers by Solvent Rub1
This standard is issued under the fixed designation D4752; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D4138 Practices for Measurement of Dry Film Thickness of

1.1 This practice describes a solvent rub technique for Protective Coating Systems by Destructive, Cross-
assessing the MEK resistance of ethyl silicate (inorganic) Sectioning Means
zinc-rich primers. The MEK resistance of some two- D5402 Practice for Assessing the Solvent Resistance of
component ethyl silicate zinc-rich primers has been shown to Organic Coatings Using Solvent Rubs
correlate well with the cure of the primer as determined by D7091 Practice for Nondestructive Measurement of Dry
diffuse reflectance infrared spectroscopy.2 The technique can Film Thickness of Nonmagnetic Coatings Applied to
be used in the laboratory, field, or in the fabricating shop. Ferrous Metals and Nonmagnetic, Nonconductive Coat-
Practice D5402 is the preferred method for organic coatings. ings Applied to Non-Ferrous Metals
1.2 The values stated in SI units are to be regarded as the 3. Terminology
standard. The values given in parentheses are for information
only. 3.1 Definitions of Terms Specific to This Standard:
3.1.1 double rub, n—the act of rubbing a solvent saturated
1.3 This standard does not purport to address all of the
cloth in one complete forward and backward motion over a
safety concerns, if any, associated with its use. It is the
coated surface.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
4. Significance and Use
mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Section 6. Consult 4.1 Ethyl silicate zinc-rich primers cure by the reaction of
supplier’s Safety Data Sheet(s) for specific hazard information the vehicle with moisture, thereby providing a binder for the
relating to the solvent used. zinc. As relative humidity and temperature vary, so does the
1.4 This international standard was developed in accor- rate of cure. A certain minimum degree of cure is necessary
dance with internationally recognized principles on standard- prior to topcoating. It has been shown that the degree of cure
ization established in the Decision on Principles for the of ethyl silicate zinc-rich primers can be measured by the
Development of International Standards, Guides and Recom- chemical changes occurring using diffuse reflectance infrared
mendations issued by the World Trade Organization Technical spectroscopy.2 This solvent rub test has been shown to corre-
Barriers to Trade (TBT) Committee. late well with the infrared spectroscopic results of some
two-component ethyl silicate inorganic zinc systems.
2. Referenced Documents
4.2 The degree of cure rating (Resistance Rating in Table 1)
2.1 ASTM Standards:3
required prior to the application of specific topcoats must be
D740 Specification for Methyl Ethyl Ketone
agreed upon before the practice is used.
1
This practice is under the jurisdiction of ASTM Committee D01 on Paint and
Related Coatings, Materials, and Applications and is the direct responsibility of 5. Reagents and Materials
Subcommittee D01.46 on Industrial Protective Coatings.
Current edition approved Feb. 1, 2020. Published February 2020. Originally
5.1 Methyl Ethyl Ketone (MEK), in accordance with Speci-
approved in 1987. Last previous edition approved in 2015 as D4752 – 10 (2015). fication D740.
DOI: 10.1520/D4752-20.
2
Starr, T. L., Henton, L. E., Lewis, W. S., and Rideout, F. A., “Improved Field
5.2 100 % Cotton, Shop Cloth, approximately 300 by 300
Reliability of High Performance Coating Systems: Phase II—Develop Procedures mm (12 by 12 in.) contrasting in color to the primer to be
and Criteria in Critical Performance Areas,” available from SSPC: The Society for evaluated.
Protective Coatings, 800 Trumbull Drive, Pittsburgh, PA 15205, www.sspc.org.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5.3 Squeeze Bottle.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 5.4 Proper Safety Equipment, as determined from the sol-
the ASTM website. vent SDS, for example, solvent resistant gloves, respirator.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
Copyright by ASTM Int'l (all rights reserved); Mon Mar 30 16:21:08 EDT 2020
1
Downloaded/printed by
University of Michigan (University of Michigan) pursuant to License Agreement. No further reproductions authorized.
D4752 − 20
TABLE 1 Scale for Resistance Rating surface, until either the metal substrate is exposed or 50 double
Resistance Rating Description rubs have been completed. If the former, record the number of
5 No effect on surface; no zinc on cloth after 50 double rubs when the substrate is exposed.
rubs
4 Burnished appearance in rubbed area; slight amount of 6.6 Select an adjacent area to be used as a control. Repeat
zinc on cloth after 50 double rubs 6.1 – 6.5, except use a dry cloth to establish the effect of
3 Some marring and apparent depression of the film after
50 double rubs
burnishing without the influence of MEK. Use this area as the
2 Heavy marring; obvious depression in the film after 50 control to visually show the appearance of No Effect.
double rubs
1 Heavy depression in the film but no actual penetration to 6.7 Inspect the test areas and the cloths. Rate the results in
the substrate after 50 double rubs accordance with Table 1.
0 Penetration to the substrate in 50 double rubs or less
7. Report
7.1 Report, as a minimum, the following information:
6. Procedure
7.1.1 Dry film thickness of the primer.
6.1 Select areas on the primer surface at least 150 mm (6 in.) 7.1.2 Elapsed time between the application of the primer
long on which to run the tests. Clean the surface with tap water and test performance.
or dry cloth to remove loose material. 7.1.3 Number of tests conducted.
NOTE 1—Tap water may influence the cure of the zinc-rich primer. 7.1.4 Resulting Resistance Rating(s) from Table 1.
7.1.5 In the case of a zero Resistance Rating, the number of
6.2 Measure the dry film thickness of the primer in the
double rubs conducted that exposed the substrate.
selected areas in accordance with Practice D7091 or Practices
7.1.6 Field and Fabricating Shop Tests—Identification of
D4138. Mark a 150- by 25-mm (6- by 1-in.) rectangular test
the area or piece tested.
area on the undamaged cleaned surface using a pencil or other
suitable solvent resistant marker. 8. Precision and Bias
6.3 Fold the cloth into a pad of double thickness and 8.1 Precision—It is not practicable to specify the precision
saturate it to a dripping wet condition with the methyl ethyl of this procedure since the rating scale is arbitrary and standard
ketone. Do not allow more than 10 s to elapse before methods for conducting round-robin studies and analyzing data
proceeding to the next steps. based on an arbitrary rating scale are not available. See
6.4 Place the properly protected index finger into the center Appendix X1 “Goodness.”
of the pad while holding excess cloth with the thumb and 8.2 Bias—Since there is no acceptable reference material,
remaining fingers of the same hand. With the index finger at a bias cannot be determined.
45° angle to the test surface, rub the rectangular test area with
moderate pressure first away from the operator and then back 9. Keywords
towards the operator. Complete each double rub (one forward 9.1 curing characteristics; double rub method; drying or
and back motion) in about 1 s. curing; ethyl silicate (inorganic) primer; methyl ethyl ketone;
6.5 Continue rubbing the surface with the MEK saturated MEK (methyl ethyl ketone) resistance; primer; solvent rub
pad, wetting the pad as necessary without lifting it from the method; visual examination; zinc-rich primer
APPENDIX
(Nonmandatory Information)
X1. GOODNESS
X1.1 An intra-lab round-robin evaluation was conducted in information have been in Table X1.1 for each cure period/film
order to access the “goodness” of this practice. Using the thickness combination.
procedure outlines in this practice, eight different operators
were asked to rate, in triplicate, the methyl ethyl ketone (MEK) X1.2 An analysis of the means, (ANOM), was conducted on
rub resistance of a particular inorganic zinc-rich primer. The the performance data of Table X1.1. Figs. X1.1-X1.4 illustrate
primer was separately applied to multiple test panels at two the raw scores and the mean score reported by each operator.
different dry film thickness ranges; 2.7-4.5 mils and 6.8-8.0 The 95 % confidence limits of the overall mean score (com-
mils. Separate test panels corresponding to each coating bined average score of the eight operators) are represented on
thickness category were scored after a 6-h cure period and a each of the figures by dashed lines. The following observations
24-h cure period. Performance ratings and general statistical were made through this analysis:
2
D4752 − 20
TABLE X1.1 Round Robin Resistance Rating
Case 1: Thin Film, 6-hr cure
Operator ID Rub 1 Rub 2 Rub 3 Range Mean Standard Deviation
A 0 3 3 3 2.0 1.4
B 3 3 3 0 3.0 0.0
C 0 0 1 1 0.3 0.5
D 3 3 3 0 3.0 0.0
E 4 2 3 2 3.0 0.8
F 0 1 0 1 0.3 0.5
G 3 3 3 0 3.0 0.0
H 1 0 1 1 0.7 0.5
Overall Average 1 1.9 0.5
Case 2: Thin Film, 24-h cure

A 5 4 4 1 4.3 0.5
B 5 4 4 1 4.3 0.5
D 4 4 4 0 4.0 0.0
F 4 5 5 1 4.7 0.5
G 5 5 5 0 5.0 0.0
H 4 4 5 1 4.3 0.5
I 4 4 4 0 4.0 0.0
J 4 4 4 0 4.0 0.0
Overall Average 0.5 4.3 0.2
Case 3: Thick Film, 6-h cure

A 4 4 4 0 4.0 0.0
B 4 4 4 0 4.0 0.0
C 4 4 4 0 4.0 0.0
D 3 3 3 0 3.0 0.0
E 4 3 3 1 3.3 0.5
F 0 4 5 5 3.0 2.2
G 3 3 3 0 3.0 0.0
H 3 4 3 1 3.3 0.5
Case 4: Thick Film, 24-h cure

A 4 4 5 1 4.3 0.5
B 5 4 4 1 4.3 0.5
D 4 3 4 1 3.7 0.5
F 4 5 4 1 4.3 0.5
G 5 5 5 0 5.0 0.0
H 4 5 5 1 4.7 0.5
I 5 3 4 2 4.0 0.8
J 4 4 4 0 4.0 0.0
X1.2.1 Rub results are cure time dependent, that is, higher limits of the overall score was found to occur in the case of the
rub scores are associated with longer cure periods, lower rub thin film 24-h cured primers.
scores are associated with shorter cure periods.
X1.2.4 All operators had mean scores within the 95 %
X1.2.2 Rub results are dependent on coating thickness, that confidence limits of the overall mean score when this practice
is, higher rub scores are associated with thick coatings films, was applied to either thick, 6-h cured primers or thick, 24-h
lower rub scores are associated with thinner coating films. cured primers.
X1.2.3 From the plots, the largest number of operators
whose mean score deviated from the 95 % confidence limits of X1.3 The findings of this practice’s round-robin evaluation
the overall mean score was found to occur when this practice have been offered in this appendix to serve as a reference or
is applied to thin film, 6-h cured primers. The second largest guide for operators wishing to utilize this practice.
number of operators whose mean score deviated from the 95 %
3
D4752 − 20
FIG. X1.1 Thin Film, 6-Hour Cure
4
D4752 − 20
FIG. X1.2 Thin-Film, 24-Hour Cure
5
D4752 − 20
FIG. X1.3 Thick Film, 6-Hour Cure
6
D4752 − 20
FIG. X1.4 Thick Film, 24-Hour Cure
7
D4752 − 20
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in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

Standard Practice for

1. Scope D4138 Practices for Measurement of Dry Film Thickness of

Overall Average 1 1.9 0.5

Case 2: Thin Film, 24-h cure

Overall Average 0.5 4.3 0.2

Case 3: Thick Film, 6-h cure

Overall Average 0.9 3.5 0.4

Case 4: Thick Film, 24-h cure

Overall Average 0.9 4.3 0.4

FIG. X1.1 Thin Film, 6-Hour Cure

FIG. X1.2 Thin-Film, 24-Hour Cure

FIG. X1.3 Thick Film, 6-Hour Cure

FIG. X1.4 Thick Film, 24-Hour Cure

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