Assessment of Degree of Cure

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Title

AS 3894.4-2002 Site testing of protective coatings - Assessment of degree of cure

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AS 3894.42002

Australian StandardTM
AS 3894.4
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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 3894.11991. 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 1580.405.1 2310
Standards Australia

Paints and related materials Methods of test Method 405.1: Determination of pencil hardness of paint film Glossary of paint and painting terms

AS 3894.42002

AS/NZS 3750 3750.15 ASTM D 2240 D 2583 D 4752

Paints for steel structures Part 15: Inorganic zinc silicate paint Standard test method for rubber propertyDurometer hardness Standard test method for indentation hardness of rigid plastics by means of a Barcol impressor 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 1525C, the manufacturers advice should be sought. Table 1 shows the test methods recommended for assessment of the degree of cure on various types of coatings.

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AS 3894.42002

TABLE 1 TEST METHODS APPLICABLE TO VARIOUS COATINGS


Coating Alkyd Test * Pencil hardness Durotest Rub test (mineral turps) Chlorinated rubber, vinyl Pencil hardness Durotest Epoxy, polyurethane, crosslinked acrylic Inorganic zinc Rub test (MEK or nominated solvent) Rub test (MEK) solvent-borne material Durotest Pencil hardness Ultra high-build coatings greater than 600 m; epoxy, polyester, vinylester, polyurethane Elastomeric coatings * Barcol 935 hardness impressor Reference test method AS/NZS 1580.405.1 AS/NZS 1580.405.1 ASTM D 4752 AS/NZS 1580.405.1 Comments Limits set by the coating manufacturer. Limited field use Limits set by the coating manufacturer Easy to use. Limits set by the coating manufacturer Limits set by the coating manufacturer. Limited field use Limits set by the coating manufacturer Easy to use Easy to use Limits set by the coating manufacturer Refer AS/NZS 3750.15 Limits set by the coating manufacturer. Easy to use

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Shore A durometer hardness tester

ASTM D 2240

Easy to use

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 APENCIL 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, 5B, 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.

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AS 3894.42002

5.2.3 Abrasive paper Of No. P600 grain size. 5.3 Preparation of leads The lead is placed in the holder, and dressed by rubbing the end against abrasive paper. With the pencil held perpendicular to the abrasive paper, the end of the lead is abraded until it is flat and free from chips or nicks. 5.4 Procedure The test procedure is as follows: (a) (b) (c) Allow the dressed lead to protrude 6 1 mm from the mechanical holder (see Figure 1). Ensure that the surface temperature of the coating does not exceed 40C. Hold the pencil at a writing angle of 45 to the paint surface and push forward, away from the operator (see Figure 2), along the surface a distance of 6 mm to 10 mm, using as much downward force on the pencil as will either cut the paint film or cause the tip of the lead to crumble. Make successive trials beginning with the softest lead and continuing with progressively harder ones until the appropriate lead that will cut or scratch the film is found. Using normal vision, carry out a minimum of three series of tests. A fresh edge of lead is required for each test. Either rotate the pencil to present a fresh edge, or redress the lead and adjust the protrusion to 6 1 mm. Note the hardness of the hardest lead that will not cut or scratch the coating. Consult the limits recommended by the coating manufacturer and determine the extent of cure.

(d)
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(e)

(f) (g)

DIMENSIONS IN MILLIMETRES

FIGURE 1 CLUTCH-TYPE PENCIL

FIGURE 2 POSITION OF LEAD DURING TEST


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AS 3894.42002

5.5 Report The test report, if required, shall include the following: (a) (b) (c) (d) (e) (f) (g) (h) (i) (j) Product identification type and batch. Method of application of paint, curing conditions, and film thickness. Details of substrate and coating system. Grade and make of leads. The hardest lead that will not disturb the coating. Whether the coating was considered cured. Report number and date of test. Name of the testing authority. Reference to this Australian/New Zealand Standard, i.e. AS/NZS 3894.4, Method A. Any deviations from this test method.

6 METHOD BDUROTEST STYLUS 6.1 Principle


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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 ApparatusStylus 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 Plain Red Blue Range * 0300 01 000 02 000 Coating type Alkyds, chlorinated rubber, vinyl Epoxy polyurethane, AS/NZS 3750.15 Type 4 zinc 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) (b) (c) (d) (e) Fit the stylus with the plain spring (i.e., the softest of the three springs). Ensure that the surface temperature of the coating does not exceed 40C. With a set tension, hold the stylus perpendicular to the coating surface and draw it towards the operator. Employing normal vision, inspect the coating for cutting or scratching by the stylus. 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.
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AS 3894.42002

(f) (g)

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. 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) (b) (c) (d) (e) (f) (g) (h) (i)
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Product identification type and batch. Method of application of paint, curing conditions, and film thickness. Details of substrate and coating system. The hardest spring and tension reading that will just damage the coating, e.g. R400. Whether the coating was considered cured. Report number and date of test. Name of the testing authority. Reference to this Australian/New Zealand Standard, i.e. AS/NZS 3894.4, Method B. Any deviations from this test method.

7 METHOD CRUB 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) (b) (c) (d) Clean all chalking and contamination from the test surface. Ensure that the surface temperature of the coating does not exceed 40C. Saturate the cloth with the solvent, so that it drips from the material. Rub the test surface with the saturated cloth and the middle and index fingers using 10 double strokes (i.e., 10 complete oscillations), applying a moderate force not greater than 2 kg. Allow the surface to dry and recover for 5 min. Examine the cloth for deposits or discolouration and note the appearance of the surfaces and any loss of coating.
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(e) (f)

Standards Australia

AS 3894.42002

(g) (h)

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. Consult the recommendations of the coating manufacturer and determine the extent of cure.
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. 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. ASTM 4752 provides a rub test for ethyl silicate zinc-rich primers.

NOTES: 1

2 3

7.4 Report The test report, if required, shall include the following: (a) (b) (c)
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Product identification type and batch. Method of application of paint, curing conditions, and film thickness. Details of substrate and coating system. The solvent used for the test. Whether the coating was considered cured. Report number and date of test. Name of the testing authority. Reference to this Australian/New Zealand Standard, i.e. AS/NZS 3894.4, Method C. Any deviations from this test method.

(d) (e) (f) (g) (h) (i)

8 METHOD DBARCOL 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) (b) Calibrate the instrument in accordance with the instrument manufacturers instructions. Ensure that the surface temperature of the coating does not exceed 40C.

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AS 3894.42002

(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. 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.

(d)

(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) (b) (c) (d)
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Product identification type and batch. Method of application of paint, curing conditions, and film thickness. Details of substrate and coating system. The Barcol hardness reading. Whether the coating was considered cured. Report number and date of test. Name of the testing authority. Reference to this Australian/New Zealand Standard, i.e. AS/NZS 3894.4, Method D. Any deviations from this test method.

(e) (f) (g) (h) (i)

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FIGURE 3 DIAGRAM OF BARCOL IMPRESSOR

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AS 3894.42002

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AS 3894.42002 10

NOTES

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11

NOTES

AS 3894.42002

AS 3894.42002

12

This Australian Standard was prepared by Committee CH-003, Paints and Related Materials. It was approved on behalf of the Council of Standards Australia on 29 March 2002 and published on 7 June 2002.

The following are represented on Committee CH-003: Australian Paint Approval Scheme Australian Paint Manufacturers Federation AUSTROADS Building Research Association of New Zealand Institution of Professional Engineers New Zealand Master Painters Australia National Association of Testing Authorities Australia New Zealand Abrasive Blasting Association New Zealand Manufacturers Federation New Zealand Painting Contractors Association Surface Coatings Association Australia Telstra Corporation Water Corporation Western Australia Additional interests participating in the preparation of this Standard:
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Australian Institute of Protective Coatings Blast Cleaning and Coating Association Qld Sydney Water Corporation

Keeping Standards up-to-date Standards are living documents which reflect progress in science, technology and systems. To maintain their currency, all Standards are periodically reviewed, and new editions are published. Between editions, amendments may be issued. Standards may also be withdrawn. It is important that readers assure themselves they are using a current Standard, which should include any amendments which may have been published since the Standard was purchased. Detailed information about Standards can be found visiting the Standards Australia web site at www.standards.com.au and looking up the relevant Standard in the on-line catalogue. Alternatively, the printed Catalogue provides information current at 1 January each year, and the monthly magazine, The Australian Standard, has a full listing of revisions and amendments published each month. We also welcome suggestions for the improvement in our Standards, and especially encourage readers to notify us immediately of any apparent inaccuracies or ambiguities. Contact us via email at [email protected], or write to the Chief Executive, Standards Australia International Ltd, GPO Box 5420, Sydney, NSW 2001.

Originated as AS 3894.41993. Second edition 2002.

This Standard was issued in draft form for comment as DR 01388.

COPYRIGHT
Standards Australia International All rights are reserved. No part of this work may be reproduced or copied in any form or by any means, electronic or mechanical, including photocopying, without the written permission of the publisher. Published by Standards Australia International Ltd GPO Box 5420, Sydney, NSW 2001, Australia
ISBN 0 7337 4479 6 Printed in Australia

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