Paints and varnishes — Determination of resistance to cyclic corrosion conditions — Part 3: Testing of coating systems on materials and components in automotive construction

This document specifies a method based on a cyclic corrosion test for testing the corrosion protection of automobiles using coating systems on aluminium, steel or galvanized steel. The test method uses corrosive conditions (temperature and humidity ramps and salt spray) to create realistic corrosion patterns. These corrosion patterns are typical for automobiles, and they are comparable in the case of sufficiently similar protective coating systems. In particular, the accelerated test investigates the delamination/corrosion creep that results from defined artificial damage to a coating. Investigations of surface and edge corrosion or investigations of adhesive specimens or components are also covered. This cyclic corrosion test is also suitable for testing corrosion in flanged areas or near gaps. This document was developed for the assessment of coated substrates (test specimens, bodywork and mounted parts) in the automotive industry. Other applications, such as components with unpainted metallic coatings, were not part of the scope of the standardization work. This document was originally developed for coating systems on aluminium, steel or galvanized steel but it can also be used for the assessment of the corrosion resistance of coating systems on other metals and their alloys.

Peintures et vernis — Détermination de la résistance aux conditions cycliques de corrosion — Partie 3: Essais de systèmes de revêtements sur matériaux et composants en construction automobile

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Publication Date
06-Jul-2022
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6060 - International Standard published
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19-May-2023
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07-Jul-2022
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INTERNATIONAL ISO
STANDARD 11997-3
First edition
2022-07
Paints and varnishes — Determination
of resistance to cyclic corrosion
conditions —
Part 3:
Testing of coating systems on
materials and components in
automotive construction
Peintures et vernis — Détermination de la résistance aux conditions
cycliques de corrosion —
Partie 3: Essais de systèmes de revêtements sur matériaux et
composants en construction automobile
Reference number
ISO 11997-3:2022(E)
© ISO 2022
---------------------- Page: 1 ----------------------
ISO 11997-3:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on

the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below

or ISO’s member body in the country of the requester.
ISO copyright office
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Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
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ISO 11997-3:2022(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction .................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 2

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus and test equipment ............................................................................................................................................................. 2

6 Test specimen preparation ....................................................................................................................................................................... 4

7 Procedure ....................................................................................................................................................................................................................4

7.1 Test conditions – Test procedure ........................................................................................................................................... 4

7.2 Interruption of the test ................................................................................................................................................................... 7

7.3 Positioning of test specimens in the chamber ............................................................................................................ 7

8 Method for evaluating chamber corrosivity .......................................................................................................................... 8

9 Ev a luat ion ................................................................................................................................................................................................................... 8

10 Precision ....................................................................................................................................................................................................................... 8

11 Test report .................................................................................................................................................................................................................. 9

Annex A (informative) Preparation and post-treatment of the mass-loss coupons.......................................10

Annex B (normative) Climate data settings of the daily cycles ............................................................................................11

Annex C (informative) Sample of specified data for the programming of climate data ............................14

Annex D (informative) Details of interlaboratory testing .........................................................................................................15

Annex E (informative) Additional information on the test specimen ...........................................................................22

Bibliography .............................................................................................................................................................................................................................23

iii
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ISO 11997-3:2022(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to

the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see

www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee

SC 9, General test methods for paints and varnishes.
A list of all parts in the ISO 11997 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
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ISO 11997-3:2022(E)
Introduction
[9] [10]
This document was prepared on the basis of SEP 1850 and VDA 233-102 .
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INTERNATIONAL STANDARD ISO 11997-3:2022(E)
Paints and varnishes — Determination of resistance to
cyclic corrosion conditions —
Part 3:
Testing of coating systems on materials and components in
automotive construction
1 Scope

This document specifies a method based on a cyclic corrosion test for testing the corrosion protection

of automobiles using coating systems on aluminium, steel or galvanized steel.

The test method uses corrosive conditions (temperature and humidity ramps and salt spray) to

create realistic corrosion patterns. These corrosion patterns are typical for automobiles, and they are

comparable in the case of sufficiently similar protective coating systems. In particular, the accelerated

test investigates the delamination/corrosion creep that results from defined artificial damage to

a coating. Investigations of surface and edge corrosion or investigations of adhesive specimens or

components are also covered. This cyclic corrosion test is also suitable for testing corrosion in flanged

areas or near gaps.

This document was developed for the assessment of coated substrates (test specimens, bodywork and

mounted parts) in the automotive industry. Other applications, such as components with unpainted

metallic coatings, were not part of the scope of the standardization work. This document was originally

developed for coating systems on aluminium, steel or galvanized steel but it can also be used for the

assessment of the corrosion resistance of coating systems on other metals and their alloys.

2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 2409, Paints and varnishes — Cross-cut test
ISO 3574, Cold-reduced carbon steel sheet of commercial and drawing qualities
ISO 4618, Paints and varnishes — Terms and definitions

ISO 4628-1, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity

and size of defects, and of intensity of uniform changes in appearance — Part 1: General introduction and

designation system

ISO 4628-2, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity

and size of defects, and of intensity of uniform changes in appearance — Part 2: Assessment of degree of

blistering

ISO 4628-3, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity and

size of defects, and of intensity of uniform changes in appearance — Part 3: Assessment of degree of rusting

ISO 4628-4, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity

and size of defects, and of intensity of uniform changes in appearance — Part 4: Assessment of degree of

cracking
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ISO 11997-3:2022(E)

ISO 4628-5, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity and

size of defects, and of intensity of uniform changes in appearance — Part 5: Assessment of degree of flaking

ISO 4628-8, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity

and size of defects, and of intensity of uniform changes in appearance — Part 8: Assessment of degree of

delamination and corrosion around a scribe or other artificial defect

ISO 4628-10, Paints and varnishes — Evaluation of degradation of coatings — Designation of quantity

and size of defects, and of intensity of uniform changes in appearance — Part 10: Assessment of degree of

filiform corrosion
ISO 9227:2017, Corrosion tests in artificial atmospheres — Salt spray tests

ISO 17872, Paints and varnishes — Guidelines for the introduction of scribe marks through coatings on

metallic panels for corrosion testing

ISO 20567-1, Paints and varnishes — Determination of stone-chip resistance of coatings — Part 1: Multi-

impact testing
3 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 4618 apply.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle

WARNING — This document may involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety concerns, if any, associated with its use.

It is the responsibility of the user of this document to establish appropriate safety and health

practices and determine the applicability of regulatory limitations prior to use.

The test specimens are tested in a cyclic test that involves salt spray, humidity ramps and temperature

ramps. In this way, realistic corrosion patterns are created for coated substrates of steel, galvanized

steel and aluminium. The results of the tests are assessed based on subjective criteria that are agreed

beforehand between the contractual partners.
5 Apparatus and test equipment

The typical laboratory and glass or plastics apparatus, together with the following.

5.1 Corrosion test chamber

All parts of the test chamber that come into contact with salt spray, condensate or test solutions shall

be made of a material that is resistant to attack by the test solutions and does not itself affect the action

of the test solutions or the salt spray/condensate on the test specimens.

The test may be carried out in separate chambers as long as the climatic conditions for the cycles are

met. Chambers that can perform all conditions are available and recommended.

Test chambers shall consist of a cooling unit, heating, pressure equalization as well as the necessary

measurement and control equipment to set and maintain the climate data described in Annex B

(temperature ±2 °C, relative humidity ±5 %) as measured at a reference point in the closed chamber

at defined temperature/relative humidity values. When passing through temperature ramps in phases

with constant relative humidity, deviations in relative humidity of −8 % to +5 % are permitted.

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ISO 11997-3:2022(E)

The test chamber shall be designed in such a way that no drops fall from the ceiling or side walls onto

the test specimens positioned below them. A test solution that has already been sprayed shall not be

returned to the storage container.

The usable space for the test and/or the space for positioning the test specimens and test specimen

holders is only that part of the test chamber that is outside of the direct spray jet. In this space, it is

possible to demonstrate that there is a uniform distribution of the spray jet in accordance with 5.4.

The holders for the test specimens are to be produced from a durable, non-metallic non-conductive

material. The holder should be designed as such that the gathering of test solution on the holder

is prevented as much as possible. No conductive bridge is allowed between test specimens. If it

is necessary to hang up test specimens, the material used shall be a durable, non-metallic and non-

conductive material. The connection points on the test specimen should be at least 20 mm to the left or

right from the scribe.
5.2 Spray nozzle(s)

Nozzles that are suitable for the temperature range of the test and that fulfil the conditions in 5.4 are

used to generate the spray. Nozzles that use compressed air (see 5.5) to atomize the droplets shall be

used. It is necessary to set the flow rate to be constant so that it is within the limits specified in 5.4. It is

to be noted that the spray jet shall not point directly at the test specimens to be tested. The number and

arrangement of the spray nozzles are to be selected in such a way that the specifications in 5.4 for the

usable space are fulfilled.

The spray nozzles shall be made from a durable material such as glass or plastic.

5.3 Test solution

The initial solution in the storage container is a preparation of NaCl in distilled, demineralized or

deionized water with a maximum conductivity of 20 μS/cm at (25 ± 2) °C in accordance with ISO 9227

but having a NaCl concentration of 10 g/l. The purity of sodium chloride shall be as specified in ISO 9227.

This solution is to be used in such a way that the sodium chloride concentration of the sprayed and

collected test solution is (10 ± 1) g/l, as this can deviate from the prepared solution depending on the

chamber. The density of a corresponding solution is (1,005 ± 0,000 5) g/cm at 25 °C. The pH value

(6,5 to 7,2) is to be maintained. Use hydrochloric acid or sodium hydroxide to adjust the pH if necessary.

WARNING — Hydrochloric acid (CAS No. 7647-01-0) solution is toxic, corrosive, irritating and

very toxic to aquatic life. Refer to Safety Data Sheet for details. Handling of hydrochloric acid

solution shall be restricted to skilled personnel or conducted under their control. Care shall be

taken in the disposal of this solution.

WARNING — Sodium hydroxide (CAS No. 1310-73-2) solution is toxic, corrosive and irritating.

Refer to Safety Data Sheet for details. Handling of sodium hydroxide solution shall be restricted

to skilled personnel or conducted under their control. Care shall be taken in the disposal of this

solution.
5.4 Quantity and distribution of the spray

The quantity of test solution to be sprayed over a defined period of time in accordance with 5.3 is

selected in such a way that (3,0 ± 1,0) ml/h of sprayed solution is collected on average in each of the

collecting devices that are used. The collected quantity in the test chamber should be controlled when

the chamber is loaded with specimens in a manner similar to the test procedure. A period of at least

16 h of constant salt spray operation is recommended before the test and during regular checks of the

salt spray phase.
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ISO 11997-3:2022(E)

Glass or plastic funnels with a diameter of 100 mm which are fitted into a measuring cylinder made of

glass or plastic using a plug are examples of suitable collecting devices.

NOTE Funnels made of glass or plastic that have their pipe sections inside measuring cylinders have proven

themselves to be suitable collecting devices. Funnels with a diameter of 100 mm have a collection area of

approximately 80 cm .

To demonstrate the uniform distribution of the spray, at least two of the collecting devices – depending

on the size of the chamber – shall be placed in the zone where the test specimens are usually placed.

In the case of very large chambers (walk-in chambers), at least one collection device is to be used for

every 4 m of positioning area.

For calibration purposes and for the verification of the uniform distribution of the spray, follow the

procedure specified in ISO 9227:2017, 6.5.
5.5 Compressed air

The compressed air used to generate the salt spray shall be free of oil and solid contaminants. It shall be

at a suitable pressure depending upon the type of spray nozzle and adjusted so that the collection rate

of sprayed solution in the chamber and the concentration of sprayed solution collected are kept within

the specified limits.

NOTE Humidification of the spray air can be necessary to prevent evaporation of the spray during the test.

Saturation towers as described in ISO 9227 represent one common method to humidify the air.

5.6 Mass-loss coupons to demonstrate constant test conditions.

To test the apparatus, use at least three mass-loss coupons with dimensions of 150 mm × 70 mm and a

thickness of (0,9 ± 0,2) mm, made of CR4 steel in accordance with ISO 3574 with practically fault-free

surfaces (roughness Ra = 0,9 µm to 1,4 µm).

At least five mass-loss coupons should be used when the test chamber is being commissioned.

5.7 Balance, accurate to at least 0,001 g.
6 Test specimen preparation

If not otherwise specified, apply an artificial defect (prior damage) to the coating, for example:

— scribe in accordance with ISO 17872;
— stone impact in accordance with ISO 20567-1;
— cross cut in accordance with ISO 2409.
7 Procedure
7.1 Test conditions – Test procedure

The test duration is six test cycles (6 weeks), if not otherwise agreed. A test cycle lasts 7 days. It consists

of daily cycles A, B and C, the sequence of which is specified as shown in Figure 1.

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ISO 11997-3:2022(E)
Key
X test time, in hours
A, B, C daily cycle
Figure 1 — Test cycle with sequence of daily cycles A, B and C
The daily cycles are characterized by the following features:

— daily cycle A, in accordance with Figure 2 and Table B.1, with a salt spray phase of 3 h (10 g/l

NaCl solution);

— daily cycle B, in accordance with Figure 3 and Table B.2, with an assessment phase;

— daily cycle C, in accordance with Figure 4 and Table B.3, with a low-temperature phase.

NOTE The ramps specified in this document are based on the current status of the control technology for

the chambers. They are intended to ensure that the temperature and relative humidity loadings necessary for

the corrosion processes can be achieved. An example for the programming of the chambers is given in Table C.1.

The positioning of test specimens in the test chamber (or the removal of test specimens) is carried out

solely during the first daily cycle B of the assessment phase during the fourth, fifth and sixth hours

after the start of daily cycle B – see Figure 3.
Key
X time, in hours
Y1 temperature, in degrees Celsius (°C)
Y2 relative humidity, in percent (%)
1 temperature
2 relative humidity
3 salt spray phase (10 g/l NaCl solution)
Figure 2 — Daily cycle A with a salt spray phase of 3 h (10 g/l NaCl solution)
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ISO 11997-3:2022(E)
Key
X time, in hours
Y1 temperature, in degrees Celsius (°C)
Y2 relative humidity, in percent (%)
1 temperature
2 relative humidity
3 assessment phase
4 start of test after first placing test specimens in the chamber
Figure 3 — Daily cycle B with assessment phase
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ISO 11997-3:2022(E)
Key
X time, in hours
Y1 temperature, in degrees Celsius (°C)
Y2 relative humidity, in percent (%)
1 temperature
2 relative humidity
3 low-temperature phase (−15 °C),
4 temperature range <5 °C with undefined relative humidity
Figure 4 — Daily cycle C with low-temperature phase (−15 °C)
7.2 Interruption of the test

It is permitted to open the test chamber during the test cycle only in the assessment phases (fourth,

fifth and sixth hours) in daily cycle B. The test chamber shall not be switched off during this time.

7.3 Positioning of test specimens in the chamber

If not otherwise agreed, the surface to be assessed of the test specimen is positioned in the test chamber

at an angle of (20 ± 5)° to the vertical with the side to be tested facing upwards. The test specimens

shall not touch one another and shall not shield one another from the spray. The test specimens may

be arranged at different levels in the chamber if the solution does not drop from test specimens or test

specimen holders onto test specimens below them.

If two or more test chambers are used to carry out the different phases (salt spray, low-temperature

and climate phases), drying-out of the test specimens shall be avoided when the test specimens are

being transferred from one chamber to the other. If more than one chamber is used, this shall be stated

in the test report.

Vehicle components or special corrosion test plates may also be used as specimens for the test. In

the case of components, special care shall be taken to ensure that salt solution does not pool on the

specimen, as this will affect the test conditions (climate). If this cannot be avoided, such pooling shall be

removed at least once a week.
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ISO 11997-3:2022(E)
8 Method for evaluating chamber corrosivity

To check the repeatability of the test results of one set of apparatus and/or the reproducibility of the

test results of different sets of apparatus, appropriate regular checks are to be carried out using mass-

loss coupons (see 5.6).

Position the mass-loss coupons at an angle of (20 ± 5)° to the vertical. A suitable procedure for preparing

and post-treating the mass-loss coupons is described in Annex A. Other methods described in ISO 8407

for removing of corrosion products were not approved during the interlaboratory tests. They may be

suitable but need to be correlated with the pickling method.

Evaluate the mass-loss specimens gravimetrically by determining the mass change after the corrosion

test. Weigh the mass-loss coupons to an accuracy of 1 mg. Divide the calculated mass loss by the area

of the exposed surface of the mass-loss coupons to obtain the mass loss of metal per square metre of

mass-loss plate.

If the average mass loss of at least three mass-loss coupons is outside the range specified in Table 1,

the mass-loss procedure is not working in conformance with this document. In case the mass loss of

the mass-loss coupons is not within the range specified in Table 1, check the test procedure and the

preparation of the mass-loss coupons.

If an individual mass-loss coupon shows larger differences to the average than stated in Table 1, the

reason shall be clarified.
Table 1 — Average mass loss of at least three mass-loss coupons
Test duration Mass loss per unit area
g/m
1 test cycle 240 ± 75
2 test cycles 570 ± 160
3 test cycles 900 ± 220
Calculation without cut edges.
9 Evaluat ion

At the end of the specified test duration, remove the test specimens from the chamber and rinse them

with water to remove residues of salt solution from the surface.

If not otherwise agreed, immediately check the test surfaces for damage in accordance with ISO 4628-1,

ISO 4628-2, ISO 4628-3, ISO 4628-4, ISO 4628-5, ISO 4628-8 and ISO 4628-10 or, if demanded, carry out

further load tests such as a stone-impact test or cross-cut test.
10 Precision

Interlaboratory testing was carried out with selected materials (see Annex D for further information).

It is not possible to make a normative statement on precision on the basis of this interlaboratory testing.

Precision depends on a range of parameters, including the evaluation procedure, the preparation of

the test specimens, the film thickness of the coating, drying and conditioning of the test specimens, the

application of scribes to the test specimens, and other prior damage.
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ISO 11997-3:2022(E)
11 Test report
The test report shall contain at least the following information:
a) all details necessary for the identification of the tested specimen;
b) a reference to this document, i.e. ISO 11997-3:2022;
c) additional information on the test specimen (see Annex E), if necessary;
d) the type of prior damage (see Clause 6);

e) the result of the test in comparison with the specified requirements (see Clause 9);

f) every deviation from the specified test method;
g) every unusual observation (deviation) during the test;
h) the date of the test.
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ISO 11997-3:2022(E)
Annex A
(informative)
Preparation and post-treatment of the mass-loss coupons
A.1 Preparation

Degrease the plates with n-heptane, white spirits or ligroin (not isopropanol or acetone).

Protect the rear side of the plates with a suitable removable adhesive tape. Leave the cut edges free.

A.2 Post-treatment

The corrosion effect leads to the formation of thick, strongly attached corrosion product layers that

shall be removed mechanically, by bending and/or hammering for example, before pickling is carried

out. Remove adhesive tape and, if necessary, adhesive residues from the rear side.

Then pickle the plates with freshly prepared, chemically pure hydrochloric acid solution, c (HCl) = 18 %,

with hexamethylenetetramine c = 3,5 g/l as an inhibitor, for 20 min at a maximum of 40 °C. All visible

corrosion products shall be removed. Subsequently, rinse twice with hot water and dry.

WARNING — Hexamethylenetetramine (CAS No. 100-97-0) is flammable, toxic, and may cause

allergic skin reaction. Refer to Safety Data Sheet for details. Handling of hexamethylenetetramine

shall be restricted to skilled personnel or conducted under their control. Care shall be taken in

the disposal of this solution.

Alternative methods, such as those specified in ISO 8407, are permitted if the repeatability and

reproducibility are approved.
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ISO 11997-3:2022(E)
Annex B
(normative)
Climate data settings of the daily cycles
Table B.1 — Daily cycle A (salt spray cycle; total duration 24 h)
Test time Temperature Relative humidity Note
h:min °C %
0:00
1:00
35 constant 100 constant salt spray
2:00
3:00
4:00
ramp 35 → 50
5:00
6:00
7:00
ramp 100 → 50
8:00
9:00
10:00
11:00
12:00 50 constant
13:00 50 constant ramp 50 → 70
14:00
15:00
ramp 70 → 90
16:00
17:00
18:00 90 constant
19:00 ramp 90 →
...

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