Norma Iso 5630-Parte 5

BRITISH STANDARD BS ISO
5630-5:2008
Paper and board —

Accelerated ageing
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Part 5: Exposure to elevated
temperature at 100 °C
ICS 85.060
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BS ISO 5630-5:2008
National foreword
This British Standard is the UK implementation of ISO 5630-5:2008.
The UK participation in its preparation was entrusted to Technical

Committee PAI/11, Methods of test for paper, board and pulps.
A list of organizations represented on this committee can be obtained on

request to its secretary.
This publication does not purport to include all the necessary provisions
of a contract. Users are responsible for its correct application.
Compliance with a British Standard cannot confer immunity
from legal obligations.
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This British Standard Amendments/corrigenda issued since publication

was published under the
authority of the Standards
Policy and Strategy Date Comments
Committee on 31 July 2010
© BSI 2010
ISBN 978 0 580 56868 8

INTERNATIONAL ISO
STANDARD 5630-5
First edition
2008-12-15
Paper and board — Accelerated ageing —

Part 5:
Exposure to elevated temperature at
100 °C
Papier et carton — Vieillissement accéléré —
Partie 5: Exposition à une température élevée à 100 °C
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Reference number
ISO 5630-5:2008(E)
Copyright British Standards Institution © ISO 2008

BS ISO 5630-5:2008
ISO 5630-5:2008(E)
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Copyright British Standards Institution © ISO 2008 – All rights reserved
BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Contents Page
Foreword ............................................................................................................................................................iv
Introduction.........................................................................................................................................................v
1 Scope ......................................................................................................................................................1
2 Normative references............................................................................................................................1
3 Principle..................................................................................................................................................1
4 Apparatus ...............................................................................................................................................1
5 Calibration and preparation of tubes for ageing ................................................................................2
5.1 Calibration of the oven..........................................................................................................................2
5.2 Preparation of glass tubes for ageing.................................................................................................2
6 Sampling.................................................................................................................................................2
7 Conditioning ..........................................................................................................................................3
8 Preparation of test pieces.....................................................................................................................3
9 Procedure ...............................................................................................................................................3
9.1 Ageing of test pieces ............................................................................................................................3
9.2 Removal and equilibration of the aged test pieces ...........................................................................3
9.3 Testing of aged and unaged papers....................................................................................................4
10 Calculations ...........................................................................................................................................4
11 Test report ..............................................................................................................................................5
Annex A (informative) Interpretation and limitations of test ..........................................................................6
Annex B (informative) ASTM permission statement .......................................................................................7
Bibliography........................................................................................................................................................8
© ISO 2008 – All rights reserved

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iii
BS ISO 5630-5:2008
ISO 5630-5:2008(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 5630-5 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps, Subcommittee SC 2,
Test methods and quality specifications for paper and board.
ISO 5630 consists of the following parts, under the general title Paper and board — Accelerated ageing:
⎯ Part 1: Dry heat treatment at 105 °C
⎯ Part 3: Moist heat treatment at 80 °C and 65 % relative humidity
⎯ Part 4: Dry heat treatment at 120 or 150 °C
⎯ Part 5: Exposure to elevated temperature at 100 °C
⎯ Part 6: Exposure to atmospheric pollution (nitrogen dioxide)
iv © ISO 2008 – All rights reserved

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BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Introduction
Exposure of paper or board to a hostile environment, such as some type of radiation, elevated temperature or
chemical attack over a period of hours can provide information concerning the natural changes that may occur
in the material over a period of years.
The test method described in this part of ISO 5630, for accelerated ageing by exposure of moist paper to an
elevated temperature, is based on the method developed by ASTM[6] following an extensive research
programme. In this programme, 15 printing and writing papers were tested, representing a wide variety of
paper types (acid and alkaline, lignin-containing and lignin-free, and those without an alkaline reserve such as
calcium carbonate). This test method proved to give more accurate results than earlier methods regarding the
effect of elevated temperature on the mechanical strength and optical stability of such papers. For a full
understanding of the stability of the permanence of the paper, a combination of test methods for accelerated
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ageing should be used.

Copyright British Standards Institution v
BS ISO 5630-5:2008
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BS ISO 5630-5:2008
INTERNATIONAL STANDARD ISO 5630-5:2008(E)
Paper and board — Accelerated ageing —

Part 5:
Exposure to elevated temperature at 100 °C
1 Scope
This part of ISO 5630 specifies a method for accelerating the ageing of printing and writing papers, through
the use of elevated temperature, and assessing its effect on the mechanical properties of fold number and
tearing resistance, for the purpose of predicting stability to long-term natural ageing.
It is applicable to all cellulose-based printing and writing papers, including coated papers and filled papers.
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2 Normative references
The following referenced documents are indispensable for the application 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 186, Paper and board — Sampling to determine average quality
ISO 187, Paper, board and pulps — Standard atmosphere for conditioning and testing and procedure for
monitoring the atmosphere and conditioning of samples
ISO 638, Paper, board and pulps — Determination of dry matter content — Oven-drying method
ISO 1974, Paper — Determination of tearing resistance (Elmendorf method)
ISO 5626, Paper — Determination of folding endurance
3 Principle
Conditioned paper samples are placed inside airtight glass tubes and aged at an elevated temperature for a
certain time. By comparing fold number and tearing resistance before and after the ageing, a measure of the
stability of paper strength is obtained.
4 Apparatus
4.1 Laboratory forced-ventilation oven, capable of maintaining a uniform temperature of
100,0 °C ± 1,0 °C, with sufficient racks to allow horizontal orientation of glass tubes.
4.2 Airtight glass tubes, of sufficient internal height to accommodate the test pieces.
The internal volume shall be of a convenient magnitude to meet the mass of test pieces per internal volume of
tube specification (see Clause 8). The tubes shall have screw-on caps, fitted with O-rings or gaskets that
ensure a hermetic seal of the interior contents during the ageing. The materials (glass, cap and O-ring or
gasket) should be thermally stable at, or preferably well above, the ageing temperature of 100 °C, and
chemically resistant to acid corrosion.
Copyright British Standards Institution © ISO 2008 – All rights reserved 1

BS ISO 5630-5:2008
ISO 5630-5:2008(E)
4.3 Balance, accurate to 0,01 g, for weighing test pieces and, when required, additional portions of sample
to ensure that the required mass of sample per unit volume of tube is met (see 9.1).
4.4 Device for cutting additional portions of sample, when required, to meet the required mass of sample
per unit volume of tube (see 9.1).
5 Calibration and preparation of tubes for ageing
5.1 Calibration of the oven
Calibrate the oven with sufficient frequency to ensure a temperature of 100,0 °C ± 1,0 °C.
5.2 Preparation of glass tubes for ageing
5.2.1 Used glass tubes
Prior to the insertion of test pieces, thoroughly clean used glass tubes.
The required cleaning sequence is as follows.
a) Wash tubes thoroughly with non-ionic detergent and tap water.
b) Rinse tubes thoroughly with tap water to remove all residual soap.
c) Rinse three more times with distilled water and allow the tubes to drain.
d) Dry the tubes in an oven at about 105 °C.
e) Condition the complete tube assembly (opened) for a minimum of 24 h in the atmosphere used for
conditioning the paper samples (Clause 7).
5.2.2 New glass tubes
When starting with new tubes, caps, O-rings or gaskets, dry them at 105 °C for at least 24 h.
Condition the complete tube assembly (opened) for a minimum of 24 h in the atmosphere used for
conditioning the paper samples (Clause 7).
5.2.3 Storage of tubes
After conditioning, cap the tubes and maintain them capped until use.
6 Sampling
Always handle the paper samples with clean cotton gloves.
If the average quality of a lot is to be determined, sampling shall be carried out in accordance with ISO 186. If
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another type of sample is to be tested, make sure that the specimens taken are representative of the sample
received.
If the sheets are much larger than A4 in size[1], cut them into sheets approximately A4 in size.
If possible, randomize the sheets. Select enough sheets for testing of aged and unaged paper, including
additional material sufficient to meet the required mass of sample per unit volume of tube (9.1) and to allow for
invalid tests.
If the sheets are less than A4 in size, select a similar area of paper sufficient for the tests to be performed.
2
BS ISO 5630-5:2008
ISO 5630-5:2008(E)
7 Conditioning
Condition the sheets, including those which will not be aged, in accordance with ISO 187 immediately prior to
the ageing period.
The sheets which will not be aged shall be kept in the standard atmosphere until their properties are tested.
8 Preparation of test pieces

From the sheets, cut the required number of test pieces of the appropriate dimensions for the tests to be
performed on both unaged and aged material (see 9.3). Follow the instructions in ISO 1974 for preparation of
test pieces for tearing resistance and the instructions in ISO 5626 for folding endurance (fold number).
NOTE It may be advisable to cut additional material to allow for invalid tests, see ISO 1974 and ISO 5626.
Determine the dry matter content of the conditioned sheets in accordance with ISO 638, and calculate the
oven-dry mass.
9 Procedure
9.1 Ageing of test pieces
Calculate the number of airtight glass tubes (4.2) needed such that each tube will contain
(0,027 8 ± 0,000 07) g of oven-dry sample per cubic centimetre internal volume of tube. If the calculation does
not give an integer number, select the next highest number.
Insert the material to be aged into the glass tubes such that each tube contains approximately the same mass
of paper. Pieces which form the tearing resistance test pieces should be rolled together prior to insertion and
then inserted in the tubes. The fold-number test pieces should then be inserted inside these.
If the mass of oven dry sample per unit volume of tube is lower than that specified (after selecting the
appropriate number of glass tubes), cut additional portions of sample and add to the tubes as required to
comply with the specification. As an example, a tube of (145 ± 5) cm3 internal volume shall contain
(4,0 ± 0,1) g (oven-dry mass) per tube. Three tubes of this size may be sufficient for test pieces for fold
number and for tearing resistance. The actual number of tubes and the need for additional portions to make
up the required grams per cubic centimetre of volume depend on the oven-dry grammage of the sample, the
specific dimensions of the test pieces and the number of pieces per test.
Put the caps into place on the tubes and secure (hand-tight) to provide a complete seal. Mark the exterior of
the glass tubes for identification of the paper samples inside.
Insert loaded tubes into the heated oven (4.1) and place them one layer deep on each rack. Age the test
pieces for (120 ± 0,5) h.
9.2 Removal and equilibration of the aged test pieces
Upon removal from the oven, allow the hot tubes to equilibrate unopened to room temperature for a minimum
of 1 h. Note any observable differences in the appearance of samples, without uncapping them.
IMPORTANT — If the samples in some tubes have a lighter colour than the original samples, the tube
may not have been airtight. Such samples shall be discarded.
Uncap the tubes in the same standard atmosphere as that used to initially condition the test specimens
(Clause 7), and then allow the test pieces to equilibrate for at least 24 h in the tubes. Remove the additional
portions of sample, if applicable, and the test pieces with tweezers, taking care to assure that no creases or
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folds are made in the test pieces.

BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Carefully unroll the individual pieces comprising the tearing resistance test pieces and place them on a flat,
clean, inert surface. Cover the individual pieces with a sheet of glass or acrylic plastic. In order to provide a
total weight of approximately 1 kg applied evenly over the full surface of the pieces, add weight at the top of
the sheet of glass or acrylic plastic, as required. Leave the weight in place for at least 12 h, then carefully
remove any additional weight and the sheet of glass or acrylic plastic from the pieces.
The uniform, low-pressure application of force on the surface of the tearing-resistance test pieces is required
to reduce the curl at the time of their testing.
Allow the test pieces to reach equilibrium in the same atmosphere as used for the initial conditioning
(Clause 7).
9.3 Testing of aged and unaged papers
Test the tearing resistance of the aged and unaged papers in the cross direction (CD) in accordance with
ISO 1974, and fold number in the machine direction (MD) in accordance with ISO 5626.
10 Calculations
Calculate the results in accordance with the instructions in the relevant ISO standard.
Calculate the retention of the fold number, to the nearest percentage, using Equation (1):
F2 × 100
R1 = (1)
F1
where
R1 is the retention of fold number, as a percentage;
F2 is the fold number (MD) of the aged sample;
F1 is the fold number (MD) of the unaged sample.
Calculate the retention of the tearing resistance, to the nearest percentage, using Equation (2):
T × 100
R2 = 2 (2)
T1
where
R2 is the retention of the tearing resistance, as a percentage;
T2 is the tearing resistance (CD) of the aged sample;
T1 is the tearing resistance (CD) of the unaged sample.
4
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BS ISO 5630-5:2008
ISO 5630-5:2008(E)
11 Test report
The test report shall include the following information:
a) reference to this part of ISO 5630;
b) reference to the International Standards used for testing the changes in properties due to ageing, if
different from those that appear in this part of ISO 5630;
c) all information necessary for complete identification of the sample;
d) the date and place of testing;
e) the temperature and relative humidity of the atmosphere used to condition the samples;
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f) the number of tests carried out, if different from this part of ISO 5630;
g) the MD fold numbers and the mean values of the CD tearing resistances of the aged and unaged
samples, and the antilogarithms of the standard deviations of the folding endurances and the standard
deviations of the CD tearing resistances of the aged and unaged samples;
h) the retentions of the MD fold number and CD tearing resistance, as percentages;
i) any deviations from the relevant International Standard from this part of ISO 5630, or any circumstances
or influence which might have affected the test results.

BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Annex A
(informative)
Interpretation and limitations of test
A.1 Interpretation of test results
A.1.1 General
The test method in this part of ISO 5630 is based on the method developed by ASTM[6] following an extensive
research programme (see Introduction). The papers were tested when freshly made and after accelerated
ageing. The results give guidance as to which papers will prove to be mechanically stable for long periods of
time as opposed to those that will quickly lose stability. Values for fold number retention and internal
tearing-resistance retention were discovered to be useful for this test method to gain a reliable estimate of the
long-term stability of test papers in natural ageing experience. (For guidance, see Reference [9], p. 44.)
NOTE A high fold number and a high tearing-resistance retention suggest a more stable paper.
A.1.2 Additional mechanical strength testing
Other mechanical strength tests may be performed at the discretion of the testing authority, in accordance
with the relevant ISO test method, and may include:
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a) tensile energy absorption (TEA), in accordance with ISO 1924-2 or ISO 1924-3;
b) zero-span tensile strength, in accordance with ISO 15361.
NOTE No paper stability determination guidance from the ASTM Paper ageing research programme can be given for
these alternative tests.
A.1.3 Determination of stability
For a paper to be classified as stable, all of the paper stability determination results should be classified as
stable. That is to say, if the paper stability determination results for internal tearing resistance are classified as
stable but the results for fold number retention are classified as unstable, the paper should be judged unstable.
A.2 Limitations of the temperature test

It should be mentioned that natural ageing is variously the result of the action of heat, light and chemicals
(e.g. pH), including pollutants from the air that become entrained into the paper. This part of ISO 5630 is
intended to characterize only thermally induced reactions. In natural ageing, an infinite range of conditions can
be found with a different “mix” of these elements. Therefore, for the greatest understanding of possible future
ageing effects, the investigator may wish to accelerate paper ageing separately by elevated temperature, by
elevated light flux, and by increased concentration of common pollutant gases. Relevant ISO standard test
methods are appropriate means to evaluate these influences.
6
BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Annex B
(informative)
ASTM permission statement
This part of ISO 5630 is based on ASTM D6819-02e2 (Standard Test Method for Accelerated Temperature
Aging of Printed and Writing Paper by Dry Oven Exposure Apparatus), copyright ASTM International, 100 Barr
Harbor Drive, West Conshohocken, PA 19428, USA. Reprinted by permission of ASTM International.
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Copyright British Standards Institution 7
BS ISO 5630-5:2008
ISO 5630-5:2008(E)
Bibliography
[1] ISO 216, Writing paper and certain classes of printed matter — Trimmed sizes — A and B series, and
indication of machine direction
[2] ISO 4046 (all parts), Paper, board, pulps and related terms — Vocabulary
[3] ISO 1924-2, Paper and board — Determination of tensile properties — Part 2: Constant rate of
elongation method (20 mm/min)
[4] ISO 1924-3, Paper and board — Determination of tensile properties — Part 3: Constant rate of
elongation method (100 mm/min)
[5] ISO 15361, Pulps — Determination of zero-span tensile strength, wet or dry
[6] ASTM International, Paper aging — ASTM’s Paper aging research report program: RR: D06-1004.
CD-ROM (containing all five reports, listed below as References [7] to [11], in their entirety), 2002
[7] ATALLA, R., BOND, J., HUNT, C. and AGARWAL, U. Quantification and prediction for aging of printing and
writing papers exposed to light: ASTM Research program on the effect of aging on printing and writing
papers; USDA Forest Service, Forest Products Laboratory, Madison, WI, August 2000
[8] FORSSKÅHL, I. Light aging test method development: ASTM/ISR Research program on the effect of
aging on printing and writing papers; KCL, August 2000
[9] KAMINSKA, E., BÉGIN, P., GRATTAN, D., W OODS, D. and BÜLOW , A. ASTM/ISR Research program on the
effects of aging on printing and writing papers: Accelerated aging test method development, Canadian
Conservation Institute, January 2001
[10] SHAHANI, C., LEE, S.B., HENGEMIHLE, F.H., HARRISON, G., SONG, P., SIERRA, M.L., Ryan, C.C. and
WEBERG, N. Accelerated aging of paper: I. Chemical analysis of degradation products; II. Application of
arrhenius relationship; III. Proposal for a new accelerated aging test: ASTM Research program on the
effect of aging on printing and writing papers. Preservation Research and Testing Division, Library of
Congress, Washington, DC, February 2001
[11] REILLY, J.M., ZINN, E. and ADELSTEIN, P. Atmospheric pollutant aging test method development. Report
to ASTM; Image Permanence Institute at Rochester Institute of Technology, Rochester, NY,
June 2000
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8 Standards Institution
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BS ISO 5630-5:2008
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BS ISO 5630-5:2008
ISO 5630-5:2008(E)
ICS 85.060
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BS ISO 5630-5:2008
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BRITISH STANDARD BS ISO

Paper and board —

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

This British Standard is the UK implementation of ISO 5630-5:2008.

The UK participation in its preparation was entrusted to Technical

A list of organizations represented on this committee can be obtained on

This British Standard Amendments/corrigenda issued since publication

ISBN 978 0 580 56868 8

Copyright British Standards Institution

Paper and board — Accelerated ageing —

Copyright British Standards Institution © ISO 2008

COPYRIGHT PROTECTED DOCUMENT

© ISO 2008 – All rights reserved

⎯ Part 1: Dry heat treatment at 105 °C

⎯ Part 3: Moist heat treatment at 80 °C and 65 % relative humidity

⎯ Part 4: Dry heat treatment at 120 or 150 °C

⎯ Part 5: Exposure to elevated temperature at 100 °C

⎯ Part 6: Exposure to atmospheric pollution (nitrogen dioxide)

iv © ISO 2008 – All rights reserved

Copyright British Standards Institution

© ISO 2008 – All rights reserved

Copyright British Standards Institution

Paper and board — Accelerated ageing —

ISO 186, Paper and board — Sampling to determine average quality

ISO 1974, Paper — Determination of tearing resistance (Elmendorf method)

ISO 5626, Paper — Determination of folding endurance

Copyright British Standards Institution © ISO 2008 – All rights reserved 1

5 Calibration and preparation of tubes for ageing

5.1 Calibration of the oven

5.2 Preparation of glass tubes for ageing

5.2.1 Used glass tubes

The required cleaning sequence is as follows.

a) Wash tubes thoroughly with non-ionic detergent and tap water.

d) Dry the tubes in an oven at about 105 °C.

5.2.2 New glass tubes

5.2.3 Storage of tubes

8 Preparation of test pieces

9.1 Ageing of test pieces

9.2 Removal and equilibration of the aged test pieces

folds are made in the test pieces.

Copyright British Standards Institution © ISO 2008 – All rights reserved 3

9.3 Testing of aged and unaged papers

R1 is the retention of fold number, as a percentage;

F2 is the fold number (MD) of the aged sample;

F1 is the fold number (MD) of the unaged sample.

R2 is the retention of the tearing resistance, as a percentage;

T2 is the tearing resistance (CD) of the aged sample;

T1 is the tearing resistance (CD) of the unaged sample.

Copyright British Standards Institution © ISO 2008 – All rights reserved

The test report shall include the following information:

a) reference to this part of ISO 5630;

c) all information necessary for complete identification of the sample;

d) the date and place of testing;

h) the retentions of the MD fold number and CD tearing resistance, as percentages;

Copyright British Standards Institution © ISO 2008 – All rights reserved 5

Interpretation and limitations of test

A.1 Interpretation of test results

A.1.2 Additional mechanical strength testing

b) zero-span tensile strength, in accordance with ISO 15361.

A.1.3 Determination of stability

A.2 Limitations of the temperature test

ASTM permission statement

© ISO 2008 – All rights reserved