Australian Standard TM

Site testing of protective coatings

Method 4: Assessment of degree of cure

PREFACE
This Standard was prepared by the Australian members of the Joint Standards
Australia/Standards New Zealand Committee CH-003, Paints and Related Materials, to
supersede AS 3894.1-1991. After consultation with stakeholders in both countries,
Standards Australia and Standards New Zealand decided to develop this Standard as an
Australian Standard rather than an Australian/New Zealand Standard.

FOREWORD
A test for the degree of cure will assist in determining whether a coating is suitable for
service and whether quality control procedures, such as adhesion and pinhole testing, may
be performed.
The firmness of the surface of a coating or its solvent resistance does not necessarily
determine the degree of cure, as a coating may achieve surface dryness with a degree of
hardness and still be soft underneath. Some coatings, such as elastomeric urethane, are
permanently soft and pliable yet fully cured.
These field tests provide a guide for use with other tests in the AS/NZS 3894 series.

METHOD
1 SCOPE
This Standard provides guidance on practical procedures, for use in the field, to assess the
degree of cure or through-dry in coatings.
Applicable coatings include those that dry by oxidation (e.g., alkyd), solvent evaporation
(e.g., lacquers such as chlorinated rubber), those that set by chemical reaction with a liquid
curing agent (e.g., epoxy) and those that react with the atmosphere (e.g., inorganic zinc).
2 DEFINITIONS
For the purpose of this Standards the definition given in AS 2310 apply.
3 REFERENCED DOCUMENTS
The following documents are referred to in this Standard:
AS/NZS
1580 Paints and related materials Methods of test
1580.405.1 Method 405.1: Determination of pencil hardness of paint film
2310 Glossary of paint and painting terms


AS/NZS
3750 Paints for steel structures
3750.15 Part 15: Inorganic zinc silicate paint
ASTM
• 2240 Standard test method for rubber property Durometer hardness
• 2583 Standard test method for indentation hardness of rigid plastics by means of a
Barcol impressor
• 4752 Standard test method for measuring MEK resistance of ethyl silicate
(inorganic) zinc-rich primers by solvent rub
4 GENERAL
Four methods of assessing the degree of cure in the field are described in Clauses 4, 5, 6
and 7 as Methods A, B, C and D respectively.
Some of these test procedures may damage the coating to be tested, particularly in the early
cure stage. The preparation of test panels, appropriately coated, prepared at the same time
and held under identical conditions, may be used for testing and so avoid costly repairs to
the coating undergoing assessment. The surface hardness of all coatings, with the exception
of inorganic zinc coatings, is affected by temperature. If testing is performed outside the
range 15-25°C, the manufacturer's advice should be sought.
Table 1 shows the test methods recommended for assessment of the degree of cure on
various types of coatings.


TABLE 1
TEST METHODS APPLICABLE TO VARIOUS COATINGS

Reference
Coating Test * Comments
test method
Alkyd Pencil hardness AS/NZS 1580.405.1 Limits set by the coating
manufacturer. Limited field use
Durotest Limits set by the coating
manufacturer
Rub test (mineral turps) Easy to use. Limits set by the
coating manufacturer
Chlorinated rubber, vinyl Pencil hardness AS/NZS 1580.405.1 Limits set by the coating
manufacturer. Limited field use
Durotest Limits set by the coating
manufacturer
Epoxy, polyurethane, cross- Rub test (MEK or Easy to use
linked acrylic nominated solvent)

Inorganic zinc Rub test (MEK)- ASTM D 4752 Easy to use

Ultra high-build coatings
greater than 600 pm;
epoxy, polyester, vinylester,
polyurethane
Elastomeric coatings
solvent-borne material
Durotest Limits set by the coating
manufacturer
Pencil hardness AS/NZS 1580.405.1 Refer AS/NZS 3750.15
Barcol 935 hardness Limits set by the coating
i mpressor manufacturer. Easy to use
Shore A durometer ASTM D 2240 Easy to use
hardness tester

* These tests will damage uncured coatings, and may damage cured coatings if applied indiscriminately. The tests are
applied to the outermost layer of the coating. Before proceeding with a test, where recommended by the paint
manufacturer, it may be necessary to determine that there is no entrapped solvent within the deeper layers of the
coating.

5 METHOD A-PENCIL HARDNESS TEST

5.1 Principle
The hardness of the surface is determined by marking it with pencil leads of various grades,
e.g., 2H, HB, 3B, and then examining the coating for the presence or absence of damage.
The method of test is similar to that outlined in AS/NZS 1580.405.1; however, the
procedure for the selection of leads is reversed, using the softest leads first to minimize
damage to the coating.
5.2 Apparatus
5.2.1 Pencil leads
A set of pencil leads with a diameter of 2 mm to fit a clutch-type pencil lead holder. The
following leads shall be included in the set:
6B, 513, 4B, 3B, 2B, B, HB, F, H, 2H, 3H, 4H, 5H, 6H, 7H and 8H (6B being the
softest and 8H the hardest).
Each lead shall be scratched by the next hardest lead above it in the series.
5.2.2 Pencil lead holder
A clutch-type mechanical lead holder suitable for use with the leads specified.


5.5 Report
The test report, if required, shall include the following:
(a) Product identification type and batch.
(b) Method of application of paint, curing conditions, and film thickness.
(c) Details of substrate and coating system.
(d) Grade and make of leads.
(e) The hardest lead that will not disturb the coating.
(f) Whether the coating was considered cured.
(g) Report number and date of test.
(h) Name of the testing authority.
(i) Reference to this Australian/New Zealand Standard, i.e. . AS/NZS 3894.4, Method A.
(j) Any deviations from this test method.
6 METHOD B-DUROTEST STYLUS
6.1 Principle
A hand-held, adjustable, spring-loaded scriber or stylus is applied at a constant pressure
while it is drawn across a coating surface. Starting with the softest spring setting, the test is
repeated with the spring tension progressively increased until the coating is cut or
scratched.
6.2 Apparatus-Stylus
A spring-loaded stylus held in a pencil-like device, utilizing a range of at least three
springs.
Table 2 indicates the spring range normally applicable to each type of coating.

TABLE 2
SPRING RANGE FOR DUROTEST STYLUS

Spring identification Range * Coating type

Plain 0-300 Alkyds, chlorinated rubber, vinyl

Red 0-1 000 Epoxy polyurethane, AS/NZS 3750.15 Type 4 zinc
Blue 0-2 000 silicate
AS/NZS 3750.15 Type 1, 2, 3 zinc silicate

* The limit of the reading varies within a generic coating range. The required full-cure readings may be
obtained from the coating manufacturer.

6.3 Procedure
The procedure is as follows:
(a) Fit the stylus with the plain spring (i.e.., the softest of the three springs).
(b) Ensure that the surface temperature of the coating does not exceed 40°C.
(c) With a set tension, hold the stylus perpendicular to the coating surface and draw it
towards the operator.
(d) Employing normal vision, inspect the coating for cutting or scratching by the stylus.
(e) If there is no damage, repeat Steps (b) and (c) with progressively higher tension
settings and, where necessary, with the next stiffer spring fitted to the stylus, until the
coating is damaged.


(f) Read the hardness from the scale corresponding to the first appearance of cutting or
scratching of the coating, e.g. R400, corresponding to a red spring setting of 400.
(g) Consult the limits recommended by the coating manufacturer and determine the
extent of cure.
6.4 Report
The test report, if required, shall include the following:
(a) Product identification type and batch.
(b) Method of application of paint, curing conditions, and film thickness.
(c) Details of substrate and coating system.
(d) The hardest spring and tension reading that will just damage the coating, e.g. R400.
(e) Whether the coating was considered cured.
(f) Report number and date of test.
(g) Name of the testing authority.
(h) Reference to this Australian/New Zealand Standard, i.e. . AS/NZS 3894.4, Method B.
(i) Any deviations from this test method.
7 METHOD C-RUB TEST
7.1 Principle
The surface of the coating is rubbed with a cloth saturated with a solvent suitable for the
coating being tested. Fully cured coatings will not be significantly affected by the solvent
whereas under-cured or partially cured coatings will have a tendency to dissolve. The cloth
and coating surface are inspected for discolouration, change of gloss, film thickness loss,
exposure of the underlying film or the metal substrate.
7.2 Apparatus and materials
7.2.1 Cotton cloth

Clean material that is not affected by the solvent, and of a colour contrasting with that of
the coating being tested.
NOTE: Clean cotton material is used to give consistent results.
7.2.2 Solvent

Methyl ethyl ketone (MEK), or mineral turpentine for alkyd coatings, or other solvents
advised by the coating manufacturer.
NOTE: When using solvents, occupational health and safety legislation is to be observed.
7.3 Procedure
The procedure is as follows:
(a) Clean all chalking and contamination from the test surface.
(b) Ensure that the surface temperature of the coating does not exceed 40°C.
(c) Saturate the cloth with the solvent, so that it drips from the material.
(d) Rub the test surface with the saturated cloth and the middle and index fingers using
1 0 double strokes (i.e.., 10 complete oscillations), applying a moderate force not
greater than 2 kg.
(e) Allow the surface to dry and recover for 5 min.
(f) Examine the cloth for deposits or discolouration and note the appearance of the
surfaces and any loss of coating.


(g) Select an adjacent area to be used as a reference. Repeat Steps (c) through (e) using a
water-dampened cloth. Note the effect of rubbing without the influence of solvent.
(h) Consult the recommendations of the coating manufacturer and determine the extent of
cure.
NOTES:
I An unmodified chemically cured coating, such as epoxy or polyurethane that is fully cured,
should be unaffected with no loss of dry film thickness and no deposit on the cloth. After the
recovery period, there may be a slight change in gloss without significant softening of the
surface.
2 Some modified chemically cured two-pack coatings may soften but will eventually recover to
normal hardness with a slight trace of colour on the cloth.
3 ASTM 4752 provides a rub test for ethyl silicate zinc-rich primers.
7.4 Report
The test report, if required, shall include the following:
(a) Product identification type and batch.
(b) Method of application of paint, curing conditions, and film thickness.
(c) Details of substrate and coating system.
(d) The solvent used for the test.
(e) Whether the coating was considered cured.
(f) Report number and date of test.
( g) Name of the testing authority.
(h) Reference to this Australian/New Zealand Standard, i.e. . AS/NZS 3894.4, Method C.
(i) Any deviations from this test method.
8 METHOD D-BARCOL HARDNESS IMPRESSOR
8.1 Principle
A hand-operated, model 935 Barcol impressor is used to obtain an indentation reading on
the coating surface. The reading obtained will indicate the degree of cure associated with
the coating material.
NOTE: The test method, using the model 934 Barcol impressor described in ASTM D 2583, is
applicable to rigid plastics and is not suitable for assessing partly cured materials or soft plastics.
8.2 Apparatus
8.2.1 Indentor
A model 935 Barcol impressor, consisting of an indentor with an indicating dial (see
Figure 3).
8.2.2 Calibration standards
Discs supplied by the manufacturer of the instrument to allow calibration.
8.3 Procedure
The test procedure is as follows:
(a) Calibrate the instrument in accordance with the instrument manufacturer's
instructions.
(b) Ensure that the surface temperature of the coating does not exceed 40°C.


(c) Place the impressor on the test surface. Set the point sleeve to the top of the coating.
Set the legs on the coating so that the indentor is perpendicular to the surface being
tested.
(d) Grasp the case of the instrument firmly between its legs and the point sleeve. Apply
quickly, by hand, a uniformly increasing force on the case until the dial indication
reaches a maximum reading. Immediately note the dial reading at the instant of
needle deflection.
NOTE: The reading will decrease with time due to creep.
(e) Check the indentor reading obtained against the required cure figures supplied by the
coating manufacturer.
8.4 Report
The test report, if required, shall include the following:
(a) Product identification type and batch.
(b) Method of application of paint, curing conditions, and film thickness.
(c) Details of substrate and coating system.
(d) The Barcol hardness reading.
(e) Whether the coating was considered cured.
(f) Report number and date of test.
(g) Name of the testing authority.
(h) Reference to this Australian/New Zealand Standard, i.e. . AS/NZS 3894.4, Method D.
(i) Any deviations from this test method.
FIGURE 3 DIAGRAM OF BARCOL IMPRESSOR