Standard Practice for

Evaluation of Coating Systems

with Zinc-Rich Primers

AASHTO Designation: R 31-02

American Association of State Highway and Transportation Officials

444 North Capitol Street N.W., Suite 249
Washington, D.C. 20001
Standard Practice for

Evaluation of Coating Systems with Zinc-Rich

Primers

AASHTO Designation: R 31-02

1. SCOPE

1.1. This specification covers the testing criteria for evaluation of zinc-rich coating systems for use on
iron and steel surfaces.

1.2. The inorganic and organic zinc-rich primers with top coats are intended for use on bridges, similar
structural steel, and other ferrous metal surfaces, both new and existing, cleaned to a minimum of
SSPC-SP 10, which are subject to corrosive atmospheric environments, such as marine, industrial,
deicing chemicals, and high humidity.

1.3. The values stated in SI units are to be regarded as standard.

1.4. This standard may involve hazardous materials, operations, and equipment. It does not purport to
address all safety problems associated with its use. It is the responsibility of the user of this
standard to establish the appropriate safety and health practices and determine the applicability of
regulatory limitations prior to use.
Note 1—The testing format and suggested acceptance criteria for this standard have been
developed around a three-coat system consisting of a zinc primer, epoxy or urethane intermediate,
and an aliphatic urethane finish coat.

2. REFERENCED DOCUMENTS

2.1. Reference to standard specifications, testing procedures and other standard procedures contained
in this document shall be the latest edition of the published document at the date of this
“Evaluation Criteria”.

2.1.1. AASHTO Standards:

■ M 300, Inorganic Zinc-Rich Primer
■ Standard Specifications for Highway Bridges

2.1.2. ASTM Standards:

■ A 36, Specification for Carbon Structural Steel
■ B 117, Test Method of Salt Spray (Fog) Testing
■ D 476, Specification for Titanium Dioxide Pigments
■ D 512, Test Methods for Chloride Ion in Water
■ D 520, Specification for Zinc Dust Pigment
■ D 521, Test Methods for Chemical Analysis of Zinc Dust (Metallic Zinc Powder)
■ D 523, Test Method for Specular Gloss

TS-4c R 31-1 AASHTO

 ■ D 562, Test Method for Consistency of Paints Using the Stormer Viscometer
■ D 610, Test Method for Evaluating Degree of Rusting on Painted Steel Surfaces
■ D 714, Test Method for Evaluating Degree of Blistering of Paints
■ D 1186, Nondestructive Measurement of Dry Film Thickness of Nonmagnetic Coatings
Applied to a Ferrous Base
■ D 1475, Test Method for Density of Paint, Varnish, Lacquer, and Related Products
■ D 1640, Test Methods for Drying, Curing, or Film Formation of Organic Coatings at Room
Temperature
■ D 1652, Test Method for Epoxy Content of Epoxy Resins
■ D 1654, Test Method for Evaluation of Painted or Coated Specimens Subjected to Corrosive
Environment
■ D 2073, Test Methods for Total, Primary, Secondary, and Tertiary Amine Values of Fatty
Amines, Amidoamines, and Diamines by Referee Potentiometric Method
■ D 2196, Test Method for Rheological Properties on Non-Newtonian Materials by Rotational
(Brookfield) Viscometers
■ D 2240, Test Method for Rubber Property—Durometer Hardness
■ D 2244, Test Method for Calculation of Color Differences from Instrumentally Measured
Color Coordinates
■ D 2369, Test Methods for Volatile Content of Coatings
■ D 2371, Test Method for Pigment Content of Solvent-Reducible Paints
■ D 2697, Test Method for Volume Nonvolatile Matter in Clear or Pigmented Coatings
■ D 2698, Test Method for the Determination of Pigment Content of Solvent-Reducible Paints
by High Speed Centrifuging
■ D 3335, Test Method for Low Concentrations of Lead, Cadmium, and Cobalt in Paint by
Atomic Absorption Spectroscopy
■ D 3718, Test Method for Low Concentrations of Chromium in Paint by Atomic Absorption
Spectroscopy
■ D 3960, Practice for Determining Volatile Organic Compound (VOC) Content of Paints and
Related Coatings
■ D 4060, Test Method for Abrasion Resistance of Organic Coatings by the Taber Abraser
■ D 4400, Test Methods for Sag Resistance of Paints Using a Multinotch Applicator
■ D 4417, Test Methods for Field Measurement of Surface Profile of Blast Cleaned Steel
■ D 4541, Test Method for Pull-Off Strength of Coatings Using Portable Adhesion Testers
■ D 4940, Test Method for Conductimetric Analysis of Water-Soluble Ionic Contamination of
Blasting Abrasives
■ D 5894, Standard Practice for Cyclic Salt Fog/UV Exposure of Painted Metal
■ D 6580, Standard Test Method for the Determination of Metallic Zinc Content in both Zinc
Dust Pigment and in Cured Films of Zinc Dust Pigment and in Cured Films of Zinc-Rich
Coatings
■ E 11, Specification for Wire-Cloth Sieves for Testing Purposes
■ E 1349, Test Method for Reflectance Factor and Color by Spectrophotometry Using
Bidirectional Geometry
■ G 92, Practice for characterization of atmosphere test sites
■ G 140, Standard Method for Determining Atmospheric Chloride Deposition Rate by Wet
Candle Method

TS-4c R 31-2 AASHTO

2.1.3. Federal Standards1:
■ Fed. Std. No. 40, CFR 51.100(s) Volatile Organic Compound Definition
■ Fed. Std. No. 40, CFR 59.406(a) Volatile Organic Compound Compliance Provision
■ Fed. Std. No. 40, CFR Part 59, Subpart D, Section 59.400 Through 59.413 National Volatile
Organic Compound Emission Standards for Architectural Coatings
■ Fed. Std. No. 40, CFR 261.24, Table 1 Maximum Concentration of Contaminants for the
Toxicity Characteristic
■ Fed. Std. No. 595, Colors Used in Government Procurement
■ EPA-SW846, Method 1311 Toxicity Characteristic Leaching Procedure (TCLP)
■ American National Standards Institute (ANSI) B94.50, Style E

2.1.4. The Society for Protective Coatings (SSPC) Standards2:

■ AB-3, Abrasive Specification Number 3, Newly Manufactured or Re-Manufactured
Steel Abrasive
■ Guide 9, Guide for Atmospheric Testing of Coatings in the Field
■ PA 2, Measurement of Dry Paint Thickness with Magnetic Gages
■ Paint 20, Zinc-Rich Primers
■ SP 5, White Metal Blast Cleaning
■ SP 6, Commercial Blast Cleaning
■ SP 10, Near-White Blast Cleaning

2.1.5. Other Documents:

■ Commercial Item Description (CID) A-A-1689B; Tape, Pressure Sensitive Adhesive,
Plastic Film3
■ Commission Internationale de l’Eclairage (CIE) 1976 L*a*b*
■ Kentucky Transportation Cabinet Test Method 64-250, Analysis for Isocyanate Content
(See Appendix D.)
■ Kentucky Transportation Cabinet Test Method 64-257, Analysis for Hindered Amine Light
Stabilizers (HALS) (See Appendix E.)
■ “Appendix A, Testing Method to Determine the Slip Coefficient for Coatings Used in Bolted
Joints,” Specification for Structural Joints Using ASTM A 325 or A 490 Bolts, as approved by
the Research Council on Structural Connections4

3. TERMINOLOGY

3.1. Definitions:

3.1.1. Volatile Organic Compound (VOC)—any organic compound that participates in atmospheric
photochemical reactions, that is, any organic compound other than those which the U.S. EPA
Administrator designates as having negligible photochemical reactivity. For a list of compounds
that the U.S. EPA Administrator has designated as having negligible photochemical reactivity,
also referred to as exempt compounds, refer to 40 CFR 51.100(s).

3.1.2. VOC Content—the weight of VOC per volume of coating, calculated according to the procedures
in 40 CFR 59.406(a).

3.1.3. Dry Film Paint Thickness—the depth of coating to the top of the surface profile peaks, measured
in accordance with SSPC PA 2.

TS-4c R 31-3 AASHTO

4. CLASSIFICATION

4.1. Primer—Inorganic zinc primers shall conform to the material requirements of M 300. Organic
zinc primers shall conform to the material requirements of SSPC Paint 20, Type II. Other primers
will be considered if they meet the testing requirements.

4.2. Touch-Up Primer—The touch-up primer shall be as recommended by the manufacturer at the time
of application. Touch-up procedures for the intermediate and top coats shall be detailed in the
product data sheets or by written submission.

5. MATERIALS

5.1. The materials used in the manufacture of the system shall conform to the requirements of the
following specifications:

5.1.1. Zinc Dust—ASTM D 520, Type II

5.1.1.1. Manufacturers shall submit a certificate of analysis from the zinc suppliers showing conformance
with the requirements.

5.1.1.2. Prior to submittal for examination, each coating (primer, intermediate and topcoat) shall be
tested by an NLLAP (National Lead Laboratory Accreditation Program) accredited laboratory to
determine its total lead content. The total lead content shall be determined using a dry film sample
in accordance with ASTM D 3335. The percentage of total lead in each coating shall not exceed
0.01 percent (100 ppm).

6. REQUIREMENTS

6.1. Color—For production, the color of the coatings shall be as mutually agreed, except that the
intermediate coat shall contrast in color. For testing requirements, see 7.2.5.

6.2. Pigment—Prime pigments shall be used except for shaders. The pigment for the primer shall be
primarily zinc dust. Leachable heavy metal compounds shall not exceed the regulatory limits of
40 CFR, 261.24, Table 1, when tested in accordance with Section 6.4.3.18. Total levels of lead,
cadmium, and chromium shall not exceed 20 times the specified limits for these elements. If
titanium dioxide is used in the top coat, it shall meet the requirements of ASTM D 476, Type IV.

6.3. Volatile Organic Compounds—VOC requirements and classifications should be in accordance

with EPA National Volatile Organic Compound Emission Standards for Consumer and
Commercial Products, 40 CFR, Part 59, Subpart D, Sections 59.400 through 59.413.

6.4. Coating Quantitative Requirements

6.4.1. Slip Coefficient for Primer—Primer coatings for use on new and rehabilitated structures with
painted connections designed for Class B allowable stress shall meet the Class B slip coefficient
requirements specified in the AASHTO Standard Specifications for Highway Bridges. The coating
supplier shall supply test data to indicate compliance, and the data shall also state the cure time,
and maximum coating thickness for that coating as indicated by the tests.

6.4.2. A manufacturer shall provide certified test results verifying that the coating seeking approval
(in an as-manufactured mixed composition) has been tested for total lead and meets requirements.

TS-4c R 31-4 AASHTO

6.4.3. Properties (determined in a mixed condition) shall be stated on the certified Product Data Sheet
and/or the MSDS as follows:

6.4.3.1. Total solids, percent by mass in accordance with ASTM D 2369.

6.4.3.2. Pigment, percent by mass in accordance with ASTM D 2371.

6.4.3.3. Metallic zinc content, percent by mass in the primer shall be determined in accordance with
ASTM D 6580. An optional method to this is the Standard Test Method for the Non-Instrumental
Determination of Metallic Zinc, as described in Appendix D.

6.4.3.4. Total solids, percent by volume in accordance with ASTM D 2697.

6.4.3.5. Mass per volume (grams per liter) in accordance with ASTM D 1475.

6.4.3.6. Viscosity (Stormer at 25°C) KU in accordance with ASTM D 562 (Not suitable for viscosities
above 143 KU).

6.4.3.7. Viscosity (Brookfield at 25°C) cP in accordance with ASTM D 2196. The spindle size and
revolutions per minute shall be reported.

6.4.3.8. Pot life in hours, at specified temperature and specified humidity.

6.4.3.9. Sag resistance (Leneta) in micrometers wet film thickness in accordance with ASTM D 4400.

6.4.3.10. Recommended minimum and maximum dry film thickness in micrometers.

■ Maximum allowable dry film thickness for the primer on faying surfaces.

6.4.3.11. Theoretical coverage: (e.g., m2/liter for 25 micrometers dry film thickness or micrometers/m2/liter,
whichever is appropriate for the particular coating).

6.4.3.12. Minimum drying time to touch, to handle and to recoat (and maximum when applicable) in
accordance with ASTM D 1640 at 25°C and 50 percent relative humidity.

6.4.3.13. Mixing ratio for multi-component coatings by volume, mass or a combination of mass and
volume. This is not required for a pre-mixed (all in one) zinc primer.

6.4.3.14. Mixing ratio for multi-component coatings, by mass.

6.4.3.15. Shelf life of each component stored at 25°C.

6.4.3.16. Infrared analysis by using FT/IR spectroscopy.

6.4.3.17. Heavy metals testing for mixed coatings ASTM D 3335 and D 3718. Heavy metals to be tested
will include lead, chromium, and cadmium.

6.4.3.18. Dry film analysis for leachable heavy metals shall include Arsenic, Barium, Cadmium,
Chromium, Lead, Mercury, Selenium, and Silver for each coating. The dried film shall be
removed from a test panel and pulverized to pass through a 250 µm (No. 60) sieve. The pulverized
film passing the 250 µm (No. 60) sieve shall be extracted in accordance with the TCLP,

TS-4c R 31-5 AASHTO

 method 1311 of EPA SW -846. The extract shall then be analyzed for heavy metals using the
appropriate EPA SW-846 test method for each metal.

6.4.3.19. The manufacturer shall supply with the submitted coating system certified chemical test results
that will define the character and nature of the coating system being submitted. Actual results shall
be verified by the qualifying laboratory, and shall be part of the qualifying laboratory’s written
report. The type of information provided by the coating manufacturer should include, but not
necessarily be limited to, the following: epoxide values (for the epoxy component of two-
component epoxy coatings), amine value (for the component of epoxy coatings which contains
amine or amidoamine cross-linkers), isocyanate group content (for that component of a
polyurethane coating which contains the isocyanate component), and identification of hindered
amine light stabilizers (for any top coat which contains such additives). Note that for epoxy
coatings cross-linked with polyamide resin, there is currently no standardized test method for
determining amide content.

6.4.3.19.1. Epoxide values can be determined in accordance with ASTM D 1652, Method A. This method
measures a quantity called the weight per epoxy equivalent (WPE), which is defined as the grams
of resin containing one gram equivalent of epoxy groups. However, since this method was
intended for raw materials, the WPE of the epoxy component of a two-component coating will
actually be the grams of that component (not the grams of actual resin) which contains one gram
equivalent of epoxy groups.
For clear components, the method can be used as is. For pigmented components, the sample
must first be weighed into a centrifuge tube, then thinned 50 to 100 percent with xylene or toluene.
If a glass stirring rod is used to aid in dispersing the sample in a thinner, it may be necessary to
use an additional small amount of thinner to rinse residues off of the rod and back into the
centrifuge tube.
The sample is then centrifuged to remove the pigment, and the supernatent should then be
transferred to the container in which the D 1652 procedure will be done. The pigment in the
bottom of the centrifuge tube should then be redispersed in 2 or 3 mL of solvent, recentrifuged,
and the supernatent combined with the original supernatent for analysis.

6.4.3.19.2. Amine values can be determined on the amine or amidoamine contained in the appropriate
component of two component epoxy coatings, in accordance with ASTM D 2073. This method is
only applicable to clear, unpigmented component. If the component is pigmented, the following
modification to D 2073 will be necessary:
Weigh 1.0 grams of the pigmented component to the nearest 0.1 milligram into a glass centrifuge
tube and thin with approximately 1 milliliter of methylene chloride. If a glass stirring rod is
required to disperse the pigmented component with the methylene chloride, it may be necessary to
use a small additional amount of methylene chloride to rinse any material off of the glass stirring
rod before removing it from the centrifuge tube.
Separate the pigment by high-speed centrifugation, and transfer the supernatant into a 25-milliliter
low-form beaker. The pigment in the bottom of the centrifuge tube should be redispersed in an
additional 2 to 3 milliliters of methylene chloride, recentrifuged, and the supernatant combined
with the original supernatant for analysis. At this point, follow the titration procedure described in
ASTM D 2073.
Note 2—Even though the titration is followed potentiometrically and the end points will not be
obscured by the color of the pigment, the pigment must still be removed to prevent the possibility
of any basic pigments reacting with the hydrochloride acid used in the titration procedure.

6.4.3.19.3. Isocyanate group content can be determined in accordance with Kentucky Transportation Cabinet
Test Method 64-250-96 (See Appendix E.), except that if appropriate, the initial centrifugation can
be done on less than 25 grams of sample.

TS-4c R 31-6 AASHTO

6.4.3.19.4. The presence of hindered amine light stabilizers (HALS) in the polyol portion of a two-component
urethane coating can be performed in accordance with Kentucky Transportation Cabinet Test
Method 64-257 (See Appendix E.) Modifications to the method including the following:
1. 60-milliliter glass centrifuge tubes are not required. Any centrifuge tube capable of holding at
least 10 to 15 milliliters of hexane/polyol mixture can be used.
2. A DB-5 or equivalent capillary column can be used.
3. Any appropriate gas chromatograph with a sensitive enough detector can be employed: it is
not necessary to use a Hewlett Packard 5890 Series II. Note that this procedure is qualitative
only, and will require that the coating manufacturer provide the laboratory with the identity of
the specific HALS being used. A control sample of this HALS will have to be obtained in
order to verify the retention time.
Note 3—If the manufacturer’s standard Product Data Sheet does not contain all of the above
required information, a supplemental sheet and/or an MSDS with the additional information shall
be provided.

6.5. Application Requirements—The following information shall be supplied by the

coatings manufacturer.

6.5.1. The minimum and maximum surface profile requirements (height in micrometers).

6.5.2. Application requirements for ambient temperature, surface temperatures, material temperature
and humidity.

6.5.3. Requirements for application by spray, brush, or roller.

7. TESTING REQUIREMENTS

7.1. General:

7.1.1. Tests must be administered or performed by an authorized testing facility as approved by

AASHTO’s National Transportation Product Evaluation Program (NTPEP). The principal facility
evaluating a specific coating system or any laboratory performing testing for the principal facility
must obtain prior approval from the NTPEP before initiating any testing.

7.1.2. All testing equipment shall be cleaned prior to performance of each testing cycle, unless
specifications require a more frequent cleaning.

7.2. Coating Evaluation Initiation Requirements:

7.2.1.1. Manufacturer—Before any testing, the manufacturer shall provide the following to the
NTPEP Lead State.

7.2.1.1.1. Name of the manufacturer of the coating system.

7.2.1.1.2. Names of the designated coatings that will be tested.

7.2.1.1.3. Product data sheet and information required by Section 6 for each coating system that will
be tested.

7.2.1.1.4. Indicate the dry film thickness, in micrometers, for each coat of the system tested.

TS-4c R 31-7 AASHTO

7.2.1.1.5. A clearly marked sample of the paint to be used for each coat of the system. The Sample kit shall
be a minimum of 12 liters.

7.2.1.2. NTPEP Lead State—The NTPEP Lead State will provide the following to the selected
testing laboratory:

7.2.1.2.1. Blind samples of the paint for each coat of the system, clearly marked with an identification code.

7.2.1.2.2. Coating information required to perform the requirements of this standard or for the preparation of
the final report.

7.2.1.2.3. Format requirements for the final report and the information to be included.

7.2.1.2.4. Completion date for the final report as mutually agreed between the NTPEP Lead State and the
testing laboratory.

7.2.1.2.5. The coating system that shall be used as a control.

7.2.1.3. Testing Laboratory—The following information will be provided to the NTPEP Lead State by the
testing laboratory:

7.2.1.3.1. Indicate what tests the Principal Testing firm will perform.

7.2.1.3.2. Identify what tests will be performed by an authorized outside firm, the name, address, and
telephone number of the firm and the contact person for the firm.

7.2.2. The laboratory performing the testing shall be responsible for application of protective coatings to
test panels.

7.2.3. The final report shall include testing results for all samples, panels, or tests performed. The final
report shall be forwarded to the NTPEP Lead State in two parts. Part one will include all of the
laboratory testing requirements. Part two will include the atmospheric testing. Manufacturers will
be allowed the option of not having the final test results for their system made public information.

7.3. Test Panel Requirements for Test (Applicable to Test Nos. 2 through 8)

7.3.1. All steel test panels, except Test No. 4 panels, shall be ASTM A 36, hot rolled steel or equivalent
with dimensions (in mm) as shown below. Certified mill test reports shall be provided as prepared
by the steel manufacturer or testing laboratory for all Grade 36 steel identifying actual physical
and chemical analysis of the material. Test panels for Test No. 4 shall be standard Taber panels,
meeting the requirements of ASTM D 4060.

Test Panel Dimensions

Test Width Length Thickness
2, 3, 5, 6 100 150 6
8 102 305 6

7.3.2. Three test panels shall be prepared for each complete system for each test, except Test 8, which
shall require five. Test 5 requires three additional test panels to be prepared with the primer only.

TS-4c R 31-8 AASHTO

 Control panels shall be coated in bulk lots by a single applicator for use by all selected
laboratories. The location and date of application shall be reported. All control panels utilized
during the testing evaluation of a system shall be from the same lot. The quantity of control
panels to be coated and the control system to be used shall be approved by NTPEP. During
transportation and storage, control panels shall be protected such that coating damage will not
occur. Beyond 30 days, the storage temperature and relative humidity for these panels shall be
25 ± 5°C and 50 ± 20 percent.

7.3.2.1. Suggested Acceptance Criteria—Two of three panels must pass for the complete system to pass.

7.3.3. The panels shall be cleaned in accordance with SSPC-SP 5 using recyclable metallic abrasives in
accordance with SSPC AB-3. The abrasives shall have a maximum chloride content of 15 ppm
determined in accordance with ASTM D 512 and a maximum conductivity of 150 micromhos per
cm determined in accordance with ASTM D 4940. The abrasive mixture shall be approximately
60 percent SAE shot number S230 and 40 percent SAE grit number G40. Both the shot and grit
shall have a Rockwell hardness of C45 ± 3. The surface profile of the cleaned panels shall be 40 to
65 µm (1.5 to 2.5 mils) when determined in accordance with ASTM D 4417, Method C. The
profile shall be clean, sharp and free of embedded friable material, with adequate roughness to
insure effective adhesion of the applied primer.
Note 4—The SP 5 is required rather than SP 10 only for the convenience of the laboratory in
order to guarantee that all panels are prepared identically and to assure comparative testing results.
Steel surfaces prepared to a lesser degree may not yield same performance.

7.3.4. Each coating shall be applied within the dry film thickness range recommended by
the manufacturer.

7.3.4.1. All products shall be applied using proper airless equipment except when this method is
specifically not allowed by the paint manufacturer. All paints shall be applied to panels mounted
vertically at a distance 530 mm (21 inches) from the tip of the spray gun. The equipment shall be
capable of developing sufficient pressure to properly atomize the coating. Orifice size, application
pressure, pump type and ratio, hose size and length and any atypical application requirements shall
be recorded. If the pressure used varies by more than 10 percent from the suggested pressure listed
in the manufacturer’s application data information, the actual pressure used and a statement
explaining the deviation shall be provided in the final report.

7.3.5. For testing purposes the color of the final top coat shall conform to Federal Standard No. 595,
Color Chip No. X4062 (green) (“X” signifies that the gloss is undesignated) and the color of the
intermediate coat shall be a contrasting color.

7.3.6. Each sample or panel shall be marked and identified by a NTPEP-assigned system code number.
The identification code number shall be placed on the back of each panel with permanent yellow
paint stick. It will also be typed and placed in front of the corresponding panel when photographs
are taken. The number will have a minimum height of 10 mm and will identify the following
information, which will be part of the final report:

7.3.6.1. Generic type of system.

7.3.6.2. Test number being performed.

7.3.6.3. Replica test being performed (i.e., salt #3).

7.3.6.4. Date of panel preparation.

TS-4c R 31-9 AASHTO

7.3.6.5. Date that the test evaluation was performed.

7.3.7. Test panels coated with the primer only and panels coated with the primer plus intermediate shall
be top coated at the minimum recoat time frame stated in the product data sheet. Curing of the
coated test panels, including control panels for the complete system, shall be a minimum of 30
days. The curing climate shall be at 25 ± 2°C and 65 ± 5 percent relative humidity. The back of all
test panels shall be coated with 75 to 100 µm of a high-quality epoxy or urethane barrier coat.

7.3.8. After preparation of the test panels with the coating system to be evaluated the edges shall be
sealed and protected by applying vinyl tape around the entire outside edge. The vinyl tape shall
extend 5 mm onto the coated surface from the edge of the panel and shall be applied after the
coating has cured. The vinyl tape shall meet the requirements of CID A-A-1689B and have an
approximate vinyl thickness of 110 micrometers with an approximate neoprene adhesive thickness
of 25 micrometers.

7.3.9. Test panels shall be scribed in accordance with ASTM D 1654 with a single “X” mark centered
on the panel. The rectangular dimensions of the scribes shall have a top width of 50 mm and a
height of 100 mm. The scribing tool shall be a straight-shank tungsten carbide tip, lathe cutting
tool (ANSI B94.50, Style E). The scribe cut shall expose the steel substrate as verified with
a microscope.

7.4. Photographic Requirements (Applicable to Test Nos. 1 through 7).

7.4.1. Color photographs of each sample or panel shall be taken as follows:

7.4.1.1. All photographs shall include the code identification number for each sample or panel and the
number of hours.

7.4.1.2. A photograph of the coated surface of each sample or panel shall be taken after application of each
coating to be evaluated.

7.4.1.3. Test No. 1—Surface of each sample prior to and after each test.

7.4.1.4. Test Nos. 2 and 3:

7.4.1.4.1. Each time frame designated.

7.4.1.4.2. Once blistering or rusting is observed, the panel shall be photographed and its condition
documented at the end of each 336-hour cycle for the ASTM D 5894 Cyclic Weathering
Resistance Test and 1,000 hours for ASTM B 117 Salt Fog Resistance Test.

7.4.1.4.3. Rust creepage evaluation: (1) after washing and prior to stripping of the scribe, and (2) after
stripping of the scribe.

7.4.1.5. Test Nos. 4, 5, and 6—At the completion of each test.

7.5. Measurement of Surface Profile and Dry Film Paint Thickness (Applicable to Test
Nos. 1 through 7).

7.5.1. Surface Profile—Measure the total surface profile thickness using a Testex kit in accordance with
ASTM D 4417, Method C.

TS-4c R 31-10 AASHTO

7.5.2. Dry Film Paint Thickness—The dry film paint thickness shall be taken in accordance with ASTM
D 1186, with the following exception:

7.5.2.1. Measure the dry film paint thickness on each test panel utilizing a Type II dry film thickness gage
as follows: Take two gage readings from the top third, the middle third, and the bottom third of the
test panel. Readings should be taken at least 25 mm from any edge. Discard any unusually high or
low gage reading that cannot be repeated consistently. The average of the acceptable gage
readings shall be no less than the manufacturer’s recommended minimum thickness. No single
gage reading shall be less than 80 percent of the manufacturer’s recommended minimum. The
average of the acceptable gage readings shall be no more than the manufacturer’s recommended
maximum thickness. No single gage reading shall be more than 120 percent of the manufacturer’s
recommended maximum. If no maximum thickness is recommended by the manufacturer, the
maximum shall be assumed to be the minimum thickness plus 50 micrometers or the minimum
thickness plus 35 percent of the minimum thickness, whichever is greater.

8. TESTS TO BE PERFORMED

8.1. Test No. 1—Slip Coefficient Test.

8.1.1. All primers shall be tested and the results reported for slip coefficient according to the AASHTO
Standard Specifications for Highway Bridges, Division I, Section 10.32.3.2.3. Tests are to be
performed in accordance with “Appendix A, Testing Method to Determine the Slip Coefficient for
Coatings Used in Bolted Joints,” Specification for Structural Joints Using ASTM 325 or A 490
Bolts, as adopted by the Research Council on Structural Connections (RCSC). Primers with a slip
coefficient of not less than 0.5 shall meet AASHTO Class B.

8.1.2. Sample Preparation Requirements for Slip Coefficient:

8.1.2.1. The surface shall be prepared in accordance with SSPC-SP 5. Surface profile shall be between 50
and 90 micrometers. Surface preparation shall be shot blasted using 100 percent steel shot
(selected to create a worst-case scenario). The steel shot shall conform to the requirements of
SSPC AB-3, SAE shot number S 280. Hardness shall be Rockwell C 45 ± 3.

8.1.2.2. The thickness of coating to be tested on each surface shall be 50 micrometers greater than the film
thickness recommended in 6.4.3.10.1. The maximum thickness tested shall be reported by the
testing laboratory.

8.1.2.3. A minimum cure time as recommended by the manufacturer is required for primer testing. Curing
of the coated test panels shall be at 25 ± 2°C and 65 ± 5 percent relative humidity.

8.2. Test No. 2—Salt Fog Resistance Test.

8.2.1. A salt fog resistance test shall be performed in accordance with ASTM B 117. The complete
system shall be exposed for durations of 4,000 and 5,000 hours.

8.2.2. Evaluation—Full visual evaluations shall be performed at the intermediate and final hours shown
above. Rust creepage at the scribe and percent rushing at the scribed edges shall be evaluated at
intermediate hours and after scraping at 5,000 hours in accordance with ASTM D 1654, Method 2,
Scraping, (where applicable after cleaning). Blistering, rust creepage at the scribe, percent rusting
at the scribed edges, and a description of rusting in the scribe shall be reported in table format and
shall not exceed the acceptance criteria of 8.2.3.

TS-4c R 31-11 AASHTO

8.2.2.1. Blistering shall be evaluated in accordance with ASTM D 714. Blister size and frequency shall be
converted to a numerical value using Table 1.
Table 1—Blister Value Conversion Table (No blisters equals a conversion number of 10.)
Blister Blister Frequency
a
Size Few Medium Med Dense Dense
#8 9 8 7 6
#6 8 7 6 5
#4 7 6 5 4
#2 6 5 4 3
#1 5 4 3 2
a
If a specific number of blisters is reported under the frequency “Few” then use chemicals shown. (See examples.)

Examples
Number Blisters Value
1 x.8
2 x.6
3 x.4
4 x.2
5 or more x.0
Note: A report of two #6 blisters converts to a value of 8.6.

8.2.2.2. Rust Creepage at the Scribe—Rust creepage (a.k.a cutback, undercut, loss of adhesion,
deterioration, disbondment) shall be measured perpendicular from the center of the scribe to the
furthest point of cutback. Cutback shall be measured in millimeters to the nearest 0.5 mm. For
both intermediate and final evaluations, the maximum cutback shall be measured at 5 mm
intervals along the scribe on each side of the scribe. (For a 50 × 100 mm X-scribe, 23
measurements are required for each side of each leg of the X-scribe). Report the average and
maximum cutback measurements. Defects at the scribe having the appearance of a “blister” will
be defined to be rust creepage (cutback).

8.2.2.3. Percent Rusting at the Scribed Edges—The length of individual areas of rust creepage along both
edges of the scribe measured in 8.2.2.2 shall be added together to achieve an aggregate length of
rust creepage. This length of rusting shall be divided by the total length of the scribe on both sides
to yield a percent of rusting at the scribed edges. [e.g., (length of rust along both sides of scribe) ÷
(total length of scribe, which is 2 × 2 × 111.8 mm equaling 447.2 mm) = ( percent rusting at the
scribed edges)].

8.2.2.4. Rusting in the Scribe—In addition to the measurement of rust creepage in 8.2.2.2 and 8.2.2.3, a
general description of rusting in the scribe itself will also be reported. This description will state
whether the scribe is “clean, partially rusted, or completely rusted.”

8.2.3. Suggested Acceptance Criteria—After the designated hours of exposure, the coating shall exhibit
no spontaneous delamination (evaluated subjectively). Blistering, rust creepage at the scribe, and
percent rusting at the scribed edges shall not exceed the following acceptance levels:

TS-4c R 31-12 AASHTO

 Test Acceptance Criteria

Blister Criteria Rust Criteria (Max)

Conversion Creepage % Rusting at
8.2 Acceptance Hours Size/Freq Value Hours Max Avg Scribed Edges
Organic Zinc
Complete System 4000 #6 Medium 7 5000 4 mm 3%

Inorganic Zinc
Complete System 4000 #6 Few 8 5000 4 mm 3%

8.3. Test No. 3—ASTM D 5894 Cyclic Weathering Resistance Test.

8.3.1. A cyclic weathering resistance test shall be performed in accordance with ASTM D 5894 for the
following durations:

Test Panel Cycle Requirements

(Number of 336-hr Cycles)
Test panels: Complete System 3 6 9 12 15

8.3.2. Color change testing shall be performed in accordance with ASTM D 2244 to obtain calculations
of color differences from instrumentally measured color coordinates CIE 1976 L*a*b*. Testing
shall be performed in accordance with ASTM E 1349 using Illuminant D 65 and 2-degree
observer. Specular gloss retention shall be performed in accordance with ASTM D 523 using an
incidence angle of 60 degrees. The difference in color, gloss values and percent of gloss retention
shall be reported.

8.3.3. Evaluation—Follow evaluation procedures of 8.2.2.

8.3.4. Suggested Acceptance Criteria—After the designated hours of exposure the coating shall exhibit
no spontaneous delamination (evaluated subjectively). Blistering, rust creepage at the scribe, and
percent rusting at the scribed edges shall not exceed the following acceptance levels, which are to
be determined:

Test Acceptance Criteria

Blister Criteria Rust Criteria (Max)
Conversion Creepage, % Rusting at
8.3 Acceptance Cycles Size/Freq Value Cycles Max, Avg Scribed Edges
Organic Zinc
Complete System

Inorganic Zinc
Complete System

Note: Criteria to be determined later in the Program.

8.4. Test No. 4—Abrasion Resistance Test.

TS-4c R 31-13 AASHTO

8.4.1. A test for abrasion resistance shall be performed in accordance with ASTM D 4060 using a CS-17
wheel and 1 kg weight for 1,000 cycles. The test shall be performed on panels coated with the full
system to be tested (i.e., primer/intermediate/finish). The hardness of the abrasive wheel shall be
checked in accordance with ASTM D2240 for each test performed.

8.4.2. Reporting Data—The system shall be tested to identify its “wear index” in milligrams per cycle
and “weight loss” in milligrams and the results shall be reported only.

8.5. Test No. 5—Adhesion Test.

8.5.1. A test for adhesion shall be performed in accordance with ASTM D 4541, using apparatus under
Appendix D. The adhesive used to perform this test shall be a two-component epoxy, containing
no solvents (e.g., 100 percent solids). The test shall be performed on panels having the primer coat
only and on panels having the complete system. A minimum of four tests shall be performed on
each panel.

8.5.2. Suggested Acceptance Criteria—Systems with inorganic zinc-rich primers shall meet a minimum
value of 2.4 MPa. Systems with organic zinc primers shall meet a minimum value of 4.1 MPa.

8.6. Test No. 6—Freeze Thaw Stability.

8.6.1. Prepared panels shall be exposed to a 30-day freeze/thaw/immersion cycle. One 24-hour cycle
shall consist of 16 hours at approximately –30°C followed by 4 hours of thawing at 50°C and 4
hours tap water immersion at 25°C. This work is done with the panels remaining in the freezer
mode on weekends and holidays. Upon completion of the test, adhesion tests shall be performed as
required in section 8.5 (Test No. 5).

8.6.2. Suggested Acceptance Criteria—Tests shall indicate that there has been no loss in the adhesion
values, when compared with those obtained in Test No. 5, which exceeds the test variation
allowed by ASTM D 4541.

8.7. Test No. 7—Coating Identification Tests.

8.7.1. An analysis of vehicle solids by fourier transform infrared (FT/IR) spectroscopy consisting of
16 scans minimum per sample shall be performed as follows:

8.7.1.1. For zinc primer solvent-based coats infrared spectrum (2.5 to 15 micrometers) of each liquid
vehicle component via the potassium bromide sandwich technique.

8.7.1.2. For two-component, solvent-based topcoats infrared spectrum (2.5 to 15 micrometers) of each
single component via the potassium bromide sandwich technique, and of the mixed and dried
components in appropriate mixing ratios (dried film) via the potassium bromide single-pellet
technique, or alternately by the IR card sampling technique, which is called the polymer-coated
fiberglass screen or transparent film (PTFE) technique.

8.7.1.3. For zinc primer water-based coats infrared spectrum (2.5 to 15 micrometers) of the liquid vehicle
component after drying and applying the potassium bromide single-pellet technique, or alternately
by the IR card sampling technique, which is called the PTFE technique.

8.7.1.4. For two-component water-based topcoats infrared spectrum (2.5 to 15 micrometers) of each single
component after drying and applying the potassium bromide single-pellet technique, or alternately
by the IR card sampling technique, which is called the PTFE technique, and also, of the mixed and

TS-4c R 31-14 AASHTO

 dried components in appropriate mixing ratios (dried film) via the single-pellet technique or
alternately by the IR card sampling technique, which is called the PTFE technique.

8.7.2. The Volatile Organic Compound (VOC) content shall be determined in accordance with ASTM
D 3960 for primer and topcoats. Multi-component coatings will be blended together in the
specified mixing ratios prior to testing.

8.7.3. The applicable properties of Section 6.4.3 shall be tested and reported.

8.8. Test No. 8—Two-Year Atmospheric Testing.

8.8.1. Each complete system shall be subjected to a two-year atmospheric test at a severe marine site. A
severe marine site is defined as one located within 30 meters (100 ft) of the mean low tide at a
seacoast location. Corrosion rate of bare steel shall be a minimum of 50 micrometers (2 mils) per
year measured in accordance with ASTM G 92. The marine test site shall provide a very severe
corrosive environment. This will include sufficient ocean wave action to ensure that air-borne salt
is continually carried via wind and deposited on the test lot. The test site will also have a climate,
which affords a high humidity with relatively high ambient temperatures. Rainfall should be
sporadic to limit the washing off of the salt film build up on the test panels.

8.8.2. Five test panels meeting the materials, surface preparation, application and curing requirements of
Section 7.2 shall be prepared with the complete system. Panels shall be a 6 × 102 × 305 mm with a
single 100 mm scribe in the center of the panel. The panel edges shall be coated up to 6 mm in
from the edge with an embedding compound, such as Morton International A-12 epoxy resin, after
the complete system has cured. Panels will be oriented to face the ocean and be inclined from the
ocean side at an angle of 30° from level along the long leg. The panels shall be exposed for two
years and then inspected and photographed in accordance with ASTM D 1654, D 610 and D 714.
The results shall be reported in the format shown in Table 2. No creepage at the scribe, bold
surface rust or blisters should be observed for ideal coating performance.

TS-4c R 31-15 AASHTO

Table 2—Evaluation of NTPEP Test Panels Exposed in the 30-Meter Atmospheric Test Lot
Exposure Date: Orientation: 30° Facing Ocean (East)
Inspection Date: Exposure Period: 2 Years

Code Panela Scribeb Blistersc

Company:
Paint System:
Primer:
Intermediate:
Finish Coat:

a
Per ASTM D-610.
b
Per ASTM D-1654.
c
Per ASTM D-714.

8.8.3. During the test period chloride content in the air will be measured on a monthly basis with the wet
candle technique in accordance with ASTM G 140. Also total UV, total solar energy, temperature
(minimum, maximum, average), relative humidity (minimum, maximum, average), average dew
point, time of wetness and rain fall will be monitored and documented in a monthly summary.
These values along with the air chloride levels will be made part of the final report.

9. FIELD HISTORY REQUIREMENTS

9.1. As a means of verifying the performance of each coating system seeking approval, a manufacturer
will be required to furnish certified documentation of field history that the proposed system has
performed for a minimum of two years on five projects from one of the following climatic
regions: hot/dry; cold/dry; hot/wet; and cold/wet. Field performance documentation must be
furnished in each of the climate regions where approval will be requested. For eligibility a project
shall have applied a minimum of 400 liters (combination of primer, intermediate and top coat) of
the system seeking approval. The document shall include the name, address and telephone number
of the propriety agency (including the names of a responsible contact person), the location of each
structure involved and approximate the beginning and ending dates of each coating application.
The checklist for conducting a field evaluation is given in Appendix A for SSPC Guide 9. Forms
for recording data on the structure and condition and on the application history are provided in
Appendices B and C, respectively, of Guide 9.

9.2. Suggested Acceptance Criteria—When a coating system has successfully completed laboratory
performance testing but has no field history, the coating system may be accepted conditionally
pending submission within three years following notification of system approval of successful 2-
year field history.

TS-4c R 31-16 AASHTO

10. INSPECTION OF TESTING

10.1. Authorized specifying agency representatives will be permitted (at any time) access to inspect
testing procedures being performed and/or review test records of any coating systems being
evaluated for approval under this specification.

11. TEST REPORT AND PROTECTIVE COATING INFORMATION

11.1. The principal testing firm will be responsible for compiling and submitting final copies of the test
report to the specifying agency.

11.2. The title page of the report shall be titled “(specifying agency) TEST REPORT” followed by:

11.2.1. Name of the principal testing firm.

11.2.2. Date of the report.

11.2.3. Name of the manufacturer of the system being tested.

11.2.4. Trade name of the coating system being tested (one report for each system).

11.2.5. Names of any subcontracted testing firms.

11.3. The contents of the report shall be bound in a presentable form and contain, as a minimum, the
following information:

11.3.1. Certificate of compliance (See Figure 1).

TS-4c R 31-17 AASHTO

Figure 1—Certificate of Compliance
ORGANIZATION LETTERHEAD
(Testing Firm)

“AASHTO” CERTIFICATE OF COMPLIANCE

We hereby certify that this coating system manufactured by

(coating manufacturer)

,
(prime cost) (intermediate coat) (finish coat)

was tested in accordance with the requirements for each applicable test as defined by AASHTO R 31, its support
specifications, and that all information presented is truthful and without bias.

All record and documents pertaining to this certificate and not submitted herewith will be maintained available by
the undersigned for a period of not less than seven years.

(OPTIONAL) (1)
(Signature of Manufacturer’s Representative)

(Name – Type or Print)

(2)
(Signature of Testing Supervisor)

(Name – Type or Print)

(3)
(Signature of Principal – Testing Firm)

(Name – Type or Print)

Title:
(Title of Testing Firm Principal)

Subscribed and sworn before me this

day of , 20

(Notary Public)

with commission expiring on

(date)

TS-4c R 31-18 AASHTO

11.3.2. Table of contents.

11.3.3. Summary of results.

11.3.4. Test Panel Photo Log—Color photographic prints or color copies of photographic prints.

11.3.5. Individual test results of all panels tested.

11.3.6. Field history.

11.3.7. Specification information for the specific coating system contained in the report as follows:

11.3.7.1. Name, address, telephone number and fax number of the manufacturer, the manufacturer’s sales
representative and the manufacturer’s technical representative.

11.3.7.2. Product name and/or identification number for each coating tested (primer, intermediate and
top coat).

11.3.7.3. Is the system intended for shop applied conditions, field applied conditions or both?

11.3.7.4. The minimum and maximum dry film thickness (in micrometers) for each coating (primer,
intermediate and topcoat).

11.3.7.5. The minimum dry (recoat) time, in hours, at 25°C between application of each coating.

11.3.7.6. Minimum application temperature, in degrees Celsius, for each coating.

11.3.7.7. The manufacturer shall identify the acceptable methods for application of each coating (spray,
brush or roller).

11.3.7.8. Requirements of Section 6.4.

11.3.8. A sufficient number of reports shall be submitted to the specifying agency for distribution so that
each owner (e.g., DOT, Authority, etc.) may receive one copy. The specifying agency shall
specify before testing starts the number of reports to be furnished.

12. REQUALIFICATION

12.1. Requalification shall occur every five years from the date of system acceptance. If changes in
formulation occur at any time, complete retesting will be required. Any change in an ingredient
amount, quality, or type will constitute a formulation change. If the formulation has remained
unchanged, the five-year requalification will include only the physical property tests, and chemical
property tests (includes instrumental identification test). Requalification at ten years will require
complete retesting. Continued requalification will require this testing cycle be continued at five-
year intervals. Significant changes in the testing standard could result in partial or complete
retesting at the end of any five-year cycle as determined by NTPEP.

TS-4c R 31-19 AASHTO

APPENDICES

A1. CHARACTERIZATION TESTS FOR PRODUCT VERIFICATION

Nonmandatory Information

A1.1. The following tests are recommended for determining if the coatings supplied are the same quality
as the manufacturer’s materials originally tested and certified for acceptance. The most pertinent
and feasible ones may be selected to verify compliance.

A1.2. Group I Tests—Most commonly used tests that are applicable to both zinc-rich primers and to
various topcoats.

A1.2.1. Infrared analysis: see requirements of Section 8.7.1.

A1.2.1.1. For zinc prime coats infrared spectrum (2.5 to 15 micrometers) of the vehicle component.

A1.2.1.2. For two-component topcoats infrared spectrum (2.5 to 15 micrometers) of each single component
and also of the mixed components (when applicable) in appropriate mixing ratios.

A1.2.2. Viscosity of mixed coating determined in accordance with ASTM D 562.

A1.2.3. Mass per volume (grams per liter) of mixed coating in accordance with ASTM D 1475.

A1.2.4. Total solids, percent by mass of mixed coating in accordance with ASTM D 2369.

A1.2.5. Dry time of mixed coating in accordance with ASTM D 1640.

A1.2.6. Pigment, percent by mass of total solids of mixed coating in accordance with ASTM D 2371.

A1.3. Group II Tests—Less frequently used tests because they pertain to zinc content and are useable
only with zinc primers.

A1.3.1. Metallic zinc, percent by mass in the primer; see requirements of 6.4.3.3.

A1.3.2. Total zinc, percent by mass of pigment (zinc dust) in accordance with ASTM D 521.

A1.3.3. Metallic zinc, percent mass of pigment (zinc dust) in accordance with ASTM D 521.

A1.3.4. Zinc oxide, percent mass of pigment (zinc dust) in accordance with ASTM D 521.

A1.3.5. Lead and cadmium content of the mixed coating in accordance with D 3335.
Note 5—The coating evaluation tests use standard colors for uniform analysis of results. Use of
different colors than those tested may change some of the baseline parameters.

TS-4c R 31-20 AASHTO

B1. GUIDE FOR PROJECT VERIFICATION TESTING
Nonmandatory Information

B1.1. The extracted pigment upon analysis shall conform to the originally approved batch and the
pigment content, percent by mass, shall not vary more than a minus 2 percent or plus 3 percent.
Allowances for the topcoats will be permitted in order to produce the desired color.

B1.2. Vehicle

B1.2.1. The vehicle solids shall not be more than ±2 percent from the initially approved batch.

B1.2.2. The infrared spectra of the vehicle/resin shall match that of the initially approved batch.

C1. STANDARD TEST METHOD FOR THE NON-INSTRUMENTAL

DETERMINATION OF METALLIC ZINC
Nonmandatory Information

C1.1. For inorganic zinc-rich coatings in which the zinc-dust pigment is supplied as a separate, dry
pigment, the percent metallic zinc in the dried film can be determined as follows: a sample of the
liquid coating shall be prepared by mixing weighed amounts of the zinc-dust pigment with
weighted amounts of the liquid component(s), using mix ratios by weight supplied by the paint
manufacturer. The quantity of paint to be mixed should be at least 100 grams, with weights
obtained to the nearest 1/10 of a gram. This mixed sample of paint is then analyzed for weight
solids in accordance with ASTM D 2369. Note that it is extremely important to keep the sample
well agitated immediately prior to performing the D 2369 procedure, so as not to allow the zinc
dust to appreciably settle out of the sample. By dividing the percent pigment in the wet paint
(obtained by calculation from the mixing information provided by the manufacturer) by the weight
solids of the mixed paint (as determined by D 2369), one obtains the percent pigment in the dried
film. By using ASTM D 521, the percent of metallic zinc in the initial, dry pigment is determined.
Finally, the percent of metallic zinc in the dried coating film is calculated by knowing the weight
of pigment in the dried coating film and the percent of metallic zinc in the zinc dust pigment.

C1.2. If the coating supplied by the manufacturer already contains the zinc dust pigment premixed with
a liquid component, a procedure similar to the above can be utilized, but extra steps must be taken
to determine the percent pigment in the liquid sample, and to also isolate this pigment for analysis
by D 521. Again, the manufacturer would have to supply mixing information by weight, rather
than volume. A sample of paint would then have to be mixed in accordance with these instructions
with the weights determined to the nearest 1/10 gram, as described above. A portion of this sample
should then be analyzed for percent pigment, in accordance with ASTM D 2371 (high speed
centrifugation). The dried pigment sample obtained from the D 2371 procedure should then be
analyzed for percent metallic zinc in accordance with ASTM D 521. The weight solids of the
mixed, liquid paint should also be determined in accordance with ASTM D 2369. At this point,
since one now knows the percent pigment in the wet paint, the weight solids of the wet paint, and
the percent metallic zinc in the dried, isolated pigment, one can then calculate the percent metallic
zinc in the dried coating film in a manner similar to that as described above.

D1. STANDARD TEST METHOD FOR ANALYSIS FOR ISOCYANATE

CONTENT
Nonmandatory Information

D1.1. Scope—This method is designed for the determination of isocyanate content of the resin system
found in acrylic polyurethane paints.

TS-4c R 31-21 AASHTO

D1.2. List of Equipment and Chemicals:

D1.2.1. Automatic titrator with stirrer;

D1.2.2. pH electrodes;

D1.2.3. Methanol, ACS reagent grade;

D1.2.4. o-Xylene, reagent grade;

D1.2.5. Dibutylamine, 99 percent assay;

D1.2.6. Buffer solutions, pH 4.00 and pH 7.00;

D1.2.7. Beaker or jar with stopper or cap, 200 mL minimum volume;

D1.2.8. Dibutylamine solution, 1.7 N, 290 mL dibutylamine dissolved in and diluted to 1 L with o-xylene;

D1.2.9. Hydrochloric acid solution, 1.0 N; and

D1.2.10. Bromophenol (if manual titration is performed).

D1.3. Procedure:

D1.3.1. In order to test a one-component primer, the resin system must first be separated from the paint.
This is done by placing a 25 g sample of the paint into a high-speed centrifuge tube and
centrifuging at 5000 to 6000 rpm until the pigment and resin have completely separated.

D1.3.2. For a two-component paint, there is no separation required. The resin is generally labeled “curing
agent” or “part B”.

D1.3.3. Place 25 mL of o-xylene and 20.00 mL of dibutylamine solution into an appropriate size beaker or
wide-mouth jar. Then weigh in the appropriate amount of resign, based on the percent isocyanate
content outlined in the specification for the coating system being used. Refer to the calculation
section for examples.
Note 6—The use of a Pasteur pipet is a convenient way of drawing the resin sample. Record the
sample weight to the nearest 0.1 mg. Cap the container immediately and swirl until the sample
is dissolved.

D1.3.4. Allow the sample to stand for a minimum of 30 minutes but no longer than 60 minutes at room
temperature.

D1.3.5. Prepare a blank in the same manner, omitting the resin sample.

D1.3.6. Calibrate the titrimeter and pH electrodes with standard pH 7.00 and pH 4.00 solutions.

D1.3.7. Wash down the sides of the containers with 100 mL of methanol.

D1.3.8. Titrate the stirred blank with 1.0 N hydrochloric acid through the end point that occurs at pH 5.0
Record the volume of titrant used to the nearest 0.01 mL.

TS-4c R 31-22 AASHTO

D1.3.9. Titrate the stirred sample with 1.0 N hydrochloric acid through the end point that occurs at pH 4.5.
Record the volume of titrant used to the nearest 0.01 mL.

D1.3.10. For manual titrations, follow the above sample preparation and add 0.5 mL of bromophenol blue
indicator to each container after washing with methanol. Then titrate the rapidly stirred blank and
sample with 1.0 N hydrochloric acid solution until a yellow color is obtained that persists for 15
seconds. Record the amount of titrant used to the nearest 0.01 mL.

D1.4. Calculations:

D1.4.1. Calculation of the appropriate amount of resin sample to be used:

W = 84/NCO (1)
where:
W = weight in grams of the resin sample to be used, and
NCO= expected percent isocyanate in the resin system.

D1.4.2. Calculation of the weight percent NCO of the sample:

%NCO = [(B – S) × N × 42/(Ws × 1000)] (100) (2)
where:
B = amount of titrant used to titrate the blank in mL;
S = amount of titrant used to titrate the sample in mL;
N = normality of the hydrochloric acid solution in equivalents per liter;
Ws = weight of the sample in grams;
42 = equivalent weight of an NCO group in grams per equivalent; and
1000 = conversion factor from liters to milliliters.

D1.5. Report:

D1.5.1. The weight of the sample should be reported to the nearest milligram, 0.001 g. The percent NCO
of the sample should be reported to the nearest 0.01 percent.
Note 7—Kentucky Method 64-250-00

TS-4c R 31-23 AASHTO

E1. STANDARD TEST METHOD FOR ANALYSIS FOR HINDERED AMINE
LIGHT STABILIZER (HALS)
Nonmandatory Information

E1.1. Scope—This method is designed to determine the presence of hindered amine light stabilizer
(HALS) in the polyol portion of a two-component, acrylic urethane coating.

E1.2. List of Equipment:

E1.2.1. Pure HALS sample;

E1.2.2. Polyol component;

E1.2.3. Hexane, HPLC grade

E1.2.4. 10 cc Disposable syringe;

E1.2.5. 60 mL glass centrifuge tube;

E1.2.6. Centrifuge;

E1.2.7. Pasteur pipette;

E1.2.8. Sample vial;

E1.2.9. Gas Chromatograph—HP-5890 Series II with FID

E1.2.10. Column:

E1.2.10.1. DB-5, 30 m × 0.25 mm × .025 µm;

E1.2.10.2. Helium Flow—2.4 mL/min.

E1.2.10.3. Injection Port—275°C

E1.2.10.4. Injection Size—1 µl

E1.2.10.5. Initial Pressure—33.0 psi

E1.2.10.6. Splitless Injection—0.5 min.

E1.2.10.7. Flame Ionization Detector—325°C

E1.2.10.8. Oven Program—50°C hold 2 min., ramp 20°C/min., 300°C hold 2.5 min.

TS-4c R 31-24 AASHTO

E1.3. Procedure:

E1.3.1. Prepare standards by adding pure HALS compounds to Hexane to obtain the desired
concentrations. These standards will be used to obtain retention time data incidental to the
specific HALS.

E1.3.2. Prepare samples by mixing 2 parts Hexane to 1 part polyol in sixty (60) mL centrifuge tube. Ten
(10) mL of Hexane and five (5) mL of polyol insures a suitable working volume. Then cap the
centrifuge tube and centrifuge for ten (10) minutes at five thousand (5000) rpm. After
centrifuging, fill a sample dial with the resulting supernatent.

E1.3.3. Analyze the standards and sample by gas chromatography utilizing the stated column and
conditions. This procedure, as written, is only qualitative. However, with the addition of the
appropriate internal standard, a quantitative analysis can be developed using a calibration plot to
determine the percent composition.

E1.4. Report:

E1.4.1. Report the specific hindered amine light stabilizer compound present.
Note 8—Kentucky Method 64-257-00

1
Available from GSA Specification Department, Federal Supply Services, Specification Section, 470 East L’Enfant
Plaza, S.W., Suite 8100, Washington, DC 20407.
2
Available from The Society for Protective Coatings, Bldg. 40, 24th Street, Pittsburgh, PA 15222-4645.
3
Available from GSA Specification Department, Federal Supply Services, Specification Section, 470 East L’Enfant
Plaza, S.W., Suite 8100, Washington, DC 20407.
4
Available from American Institute of Steel Construction, Inc., One East Wacker Drive, Suite 3100, Chicago, IL
60601-2001.

TS-4c R 31-25 AASHTO