SIST ISO 302:2011

Pulps -- Determination of Kappa number

This International Standard specifies a method for the determination of the Kappa number of pulp. The Kappa number is an indication of the lignin content or bleachability of pulp.
This International Standard is applicable to all kinds of chemical pulps and semi-chemical pulps within the Kappa number range 1 to 100. For pulps with a Kappa number exceeding 100, use the chlorine-consumption procedure (ISO 3260) to describe the degree of delignification.
To achieve the greatest precision and accuracy, the sample size should be adjusted so that the consumption of permanganate falls between 20 % and 60 % of the amount added.
NOTE There is no general and unambiguous relationship between the Kappa number and the lignin content of pulp. The relationship varies according to the wood species and delignification procedure. All compounds oxidized by KMnO4, not only lignin, will increase the consumption of KMnO4, and thereby increase the Kappa number (see [7]). If the Kappa number is to be used to derive an index of pulp lignin content, specific relationships will have to be developed for each pulp type.

Pâtes -- Détermination de l'indice Kappa

Vlaknine - Določanje števila Kappa

Ta mednarodni standard opredeljuje metodo za določevanje števila Kappa v vlakninah. Število Kappa je označba vsebnosti lignina ali zmožnost beljenja vlaknin.
Ta mednarodni standard velja za vse vrste kemičnih vlaknin in polkemičnih vlaknin s številom Kappa v razponu od 1 do 100. Za vlaknine s številom Kappa, ki presega 100, se za opis stopnje odstranjevanja lignina uporabi postopek porabe klora (ISO 3260).
Za doseganje največje natančnosti in točnosti mora biti velikost vzorca prilagojena tako, da je poraba hipermangana med 20 % in 60 % dodane količine.
OPOMBA: Ne obstaja splošno in nedvoumno razmerje med številom Kappa in vsebnostjo lignina v vlaknini. Razmerje se razlikuje glede na vrsto lesa in postopek odstranjevanja lignina. Vse sestavine, oksidirane s KMnO4, ne le lignin, povečajo porabo KMnO4 in zato povečajo število Kappa (glej [7]). Če naj se število Kappa uporablja za izpeljavo indeksa vsebnosti lignina v vlakninah, bo treba razviti posebno razmerje za vsako vrsto vlaknine.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 29-Mar-2011
• Publication Date: 13-Apr-2011
• Withdrawal Date: 17-May-2016
• ICS: 85.040 - Pulps
• Technical Committee: VPK - Pulp, paper, board and products
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 18-May-2016
• Due Date: 10-Jun-2016
• Completion Date: 18-May-2016
• Ref Project: ISO 302:2004 - Pulps — Determination of Kappa number

Relations

• Revised: SIST ISO 302:1995 - Pulps -- Determination of Kappa number
• Effective Date: 01-May-2011
• Replaced By: SIST ISO 302:2016 - Pulps -- Determination of Kappa number
• Effective Date: 01-Jun-2016

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 302
Second edition
2004-07-01


Pulps — Determination of Kappa number
Pâtes — Détermination de l'indice Kappa




Reference number
ISO 302:2004(E)
©
ISO 2004

---------------------- Page: 1 ----------------------
ISO 302:2004(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.


©  ISO 2004
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland

ii © ISO 2004 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 302:2004(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 2
5 Reagents and materials. 2
6 Apparatus and equipment. 3
7 Sampling and preparation of sample. 3
7.1 Sampling . 3
7.2 Sample preparation. 3
8 Procedure. 3
8.1 General. 3
8.2 Blank. 4
8.3 Determination . 4
9 Calculations. 6
9.1 Kappa number 5 to 100. 6
9.2 Kappa number 1 to 5. 7
9.3 Expression of results. 8
9.4 Example of calculation . 8
10 Precision . 8
10.1 Reference pulp . 8
10.2 Repeatability. 8
10.3 Reproducibility . 9
11 Test report. 9
Bibliography . 10

© ISO 2004 – All rights reserved iii

---------------------- Page: 3 ----------------------
ISO 302:2004(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 302 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps, Subcommittee SC 5, Test
methods and quality specifications for pulps.
This second edition cancels and replaces the first edition (ISO 302:1981), which has been technically revised.
iv © ISO 2004 – All rights reserved

---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 302:2004(E)

Pulps — Determination of Kappa number
1 Scope
This International Standard specifies a method for the determination of the Kappa number of pulp. The Kappa
number is an indication of the lignin content or bleachability of pulp.
This International Standard is applicable to all kinds of chemical pulps and semi-chemical pulps within the
Kappa number range 1 to 100. For pulps with a Kappa number exceeding 100, use the chlorine-consumption
procedure (ISO 3260) to describe the degree of delignification.
To achieve the greatest precision and accuracy, the sample size should be adjusted so that the consumption
of permanganate falls between 20 % and 60 % of the amount added.
NOTE There is no general and unambiguous relationship between the Kappa number and the lignin content of pulp.
The relationship varies according to the wood species and delignification procedure. All compounds oxidized by KMnO ,
4
not only lignin, will increase the consumption of KMnO , and thereby increase the Kappa number (see [7]). If the Kappa
4
number is to be used to derive an index of pulp lignin content, specific relationships will have to be developed for each
pulp type.
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 638, Pulps — Determination of dry matter content
ISO 7213, Pulps — Sampling for testing
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
oxidation capacity
relative amount of permanganate oxidized (expressed as MnO ) of the total oxidation capacity
2
3.2
total oxidation capacity
2+
oxidation capacity (permanganate consumption) when all permanganate is oxidized into Mn
3.3.
Kappa number of pulp
number of millilitres of 0,02 mol/l potassium permanganate solution consumed under the specified conditions
by one gram of pulp (calculated on an oven-dry basis)
NOTE The results are corrected to a value corresponding to that obtained when 50 % of the total oxidation capacity
of the permanganate is consumed in the test at a temperature of 25 °C.
© ISO 2004 – All rights reserved 1

---------------------- Page: 5 ----------------------
ISO 302:2004(E)
4 Principle
Disintegrated pulp is allowed to react with a specified amount of potassium permanganate solution for a given
time. The amount of pulp is chosen so that about 50 % of the total oxidation capacity of the permanganate is
left unconsumed at the end of the reaction time.
The main reactions are as follows:
− +
1) Residual lignin + other oxidable compounds + MnO + 4H → oxidized lignin + other oxidized
4
−
compounds + excess MnO + MnO + 2H O
4 2 2
− − +
2+
2) 2MnO + 10I + 16H → 2Mn + 5I + 8H O
4 2 2
+ −
2+
3) MnO + 4H + 2I → Mn + 2H O + I
2 2 2
2− 2− −
4) 2S O + I → S O + 2I
2 3 2 4 6
NOTE By theoretical calculation and experimental observation, a consumption of 60 % (mass/mass) is actually the
endpoint of the consumption for the permanganate ions, at which point the ions have been reduced to MnO . Further
2
oxidation, performed by means of MnO should be considered as “out of range”. By adding potassium iodide solution, the
2
reaction is terminated and the free iodine is titrated with sodium thiosulfate solution. The value so obtained is corrected to
50 % consumption of the total oxidation capacity of permanganate.
5 Reagents and materials
Use only chemicals of recognized analytical grade and only distilled water or water of equivalent purity.
5.1 Sulfuric acid, c(H SO ) = 2,0 mol/l.
2 4
Add with caution 112 ml of sulfuric acid, H SO , of density 1,84 g/ml, to about 600 ml of water. Allow to cool
2 4
and dilute to 1 litre with water.
5.2 Potassium iodide, c(KI) = 1 mol/l.
Dissolve 166 g of potassium iodide, KI, in a 1 000 ml volumetric flask and fill up to the mark with water.
5.3 Potassium permanganate, c(KMnO ) = (0,020 ± 0,001) mol/l.
4
Dissolve 3,161 g of potassium permanganate, KMnO , in a 1 000 ml volumetric flask and fill up to the mark
4
with water.
NOTE Fresh solution is stable for at least 6 months if stored in a dark bottle.
5.4 Sodium thiosulfate, c(Na S O ) = (0,200 0 ± 0,000 5 ) mol/l.
2 2 3
Dissolve 49,65 g of sodium thiosulfate, Na S O · 5H O, in a 1 000 ml volumetric flask and fill up to the mark
2 2 3 2
with water.
5.5 Starch indicator, 2 g/l solution.
NOTE Commercially available standard solutions may be used.
2 © ISO 2004 – All rights reserved

---------------------- Page: 6 ----------------------
ISO 302:2004(E)
6 Apparatus and equipment
Ordinary laboratory equipment and the following.
6.1 Agitator, of the propeller type, made of glass or other noncorrosive material (a plastic- or glass-covered
magnetic stirrer may be used instead).
6.2 Wet-disintegration apparatus or blender, high-speed mixer, capable of disintegrating the pulp
completely with minimum damage to the fibres.
6.3 Water bath, capable of maintaining a temperature of (25,0 ± 0,2) °C in the reaction vessel (see 8.3
regarding temperature correction).
6.4 Timing device, capable of measuring 10 min to the nearest 1 s.
NOTE Automatic Kappa number analysers can be used if they follow this International Standard and give the same
results.
7 Sampling and preparation of sample
7.1 Sampling
If the test is being made to evaluate a pulp lot, the sample shall be selected in accordance with ISO 7213. If
the test is made on another type of sample, report the source of the sample and if possible the sampling
procedure used.
Make sure that the test portions taken are representative of the pulp.
As the presence of small amounts of spent cooking liquor affects the Kappa number, ensure that the sample
is well washed.
7.2 Sample preparation
Prepare the test material according to one of the following procedures.
7.2.1 Air-dry pulp. Tear or cut the pulp into small pieces.
7.2.2 Screened slush pulp. Dewater the pulp sample by filtering on a Büchner funnel or by centrifuging,
avoiding any loss of fibres or fines. Air-dry the pulp sample, or dry it at a temperature not exceeding 105 °C,
and tear it into small pieces.
7.2.3 Unscreened pulp. If the sample is taken from unscreened pulp, which is normally screened before
bleaching or other processing, remove the shives and knots from the sample by screening. Choose a
procedure that gives results similar to those obtained by industrial screening. State the method of screening in
the test report. Continue the sample preparation as described in 7.2.2.
NOTE If the pulp sample contains a considerable amount of shives, the screening procedure may give rise to
incorrect results. A more reliable value may be obtained by defibrating the pulp sample before the determination. State the
method of defibration in the test report.
8 Procedure
8.1 General
This International Standard includes two different procedures. One is used in the Kappa number range
5 to 100 and the other in the Kappa number range 1 to 5.
© ISO 2004 – All rights reserved 3

---------------------- Page: 7 --------------
...

SLOVENSKI STANDARD
SIST ISO 302:2011
01-maj-2011
9ODNQLQH'RORþDQMHãWHYLOD.DSSD
Pulps -- Determination of Kappa number
Pâtes -- Détermination de l'indice Kappa
Ta slovenski standard je istoveten z: ISO 302:2004
ICS:
85.040 Vlaknine Pulps
SIST ISO 302:2011 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST ISO 302:2011

---------------------- Page: 2 ----------------------

SIST ISO 302:2011


INTERNATIONAL ISO
STANDARD 302
Second edition
2004-07-01


Pulps — Determination of Kappa number
Pâtes — Détermination de l'indice Kappa




Reference number
ISO 302:2004(E)
©
ISO 2004

---------------------- Page: 3 ----------------------

SIST ISO 302:2011
ISO 302:2004(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.


©  ISO 2004
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland

ii © ISO 2004 – All rights reserved

---------------------- Page: 4 ----------------------

SIST ISO 302:2011
ISO 302:2004(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Terms and definitions. 1
4 Principle . 2
5 Reagents and materials. 2
6 Apparatus and equipment. 3
7 Sampling and preparation of sample. 3
7.1 Sampling . 3
7.2 Sample preparation. 3
8 Procedure. 3
8.1 General. 3
8.2 Blank. 4
8.3 Determination . 4
9 Calculations. 6
9.1 Kappa number 5 to 100. 6
9.2 Kappa number 1 to 5. 7
9.3 Expression of results. 8
9.4 Example of calculation . 8
10 Precision . 8
10.1 Reference pulp . 8
10.2 Repeatability. 8
10.3 Reproducibility . 9
11 Test report. 9
Bibliography . 10

© ISO 2004 – All rights reserved iii

---------------------- Page: 5 ----------------------

SIST ISO 302:2011
ISO 302:2004(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 302 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps, Subcommittee SC 5, Test
methods and quality specifications for pulps.
This second edition cancels and replaces the first edition (ISO 302:1981), which has been technically revised.
iv © ISO 2004 – All rights reserved

---------------------- Page: 6 ----------------------

SIST ISO 302:2011
INTERNATIONAL STANDARD ISO 302:2004(E)

Pulps — Determination of Kappa number
1 Scope
This International Standard specifies a method for the determination of the Kappa number of pulp. The Kappa
number is an indication of the lignin content or bleachability of pulp.
This International Standard is applicable to all kinds of chemical pulps and semi-chemical pulps within the
Kappa number range 1 to 100. For pulps with a Kappa number exceeding 100, use the chlorine-consumption
procedure (ISO 3260) to describe the degree of delignification.
To achieve the greatest precision and accuracy, the sample size should be adjusted so that the consumption
of permanganate falls between 20 % and 60 % of the amount added.
NOTE There is no general and unambiguous relationship between the Kappa number and the lignin content of pulp.
The relationship varies according to the wood species and delignification procedure. All compounds oxidized by KMnO ,
4
not only lignin, will increase the consumption of KMnO , and thereby increase the Kappa number (see [7]). If the Kappa
4
number is to be used to derive an index of pulp lignin content, specific relationships will have to be developed for each
pulp type.
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 638, Pulps — Determination of dry matter content
ISO 7213, Pulps — Sampling for testing
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
oxidation capacity
relative amount of permanganate oxidized (expressed as MnO ) of the total oxidation capacity
2
3.2
total oxidation capacity
2+
oxidation capacity (permanganate consumption) when all permanganate is oxidized into Mn
3.3.
Kappa number of pulp
number of millilitres of 0,02 mol/l potassium permanganate solution consumed under the specified conditions
by one gram of pulp (calculated on an oven-dry basis)
NOTE The results are corrected to a value corresponding to that obtained when 50 % of the total oxidation capacity
of the permanganate is consumed in the test at a temperature of 25 °C.
© ISO 2004 – All rights reserved 1

---------------------- Page: 7 ----------------------

SIST ISO 302:2011
ISO 302:2004(E)
4 Principle
Disintegrated pulp is allowed to react with a specified amount of potassium permanganate solution for a given
time. The amount of pulp is chosen so that about 50 % of the total oxidation capacity of the permanganate is
left unconsumed at the end of the reaction time.
The main reactions are as follows:
− +
1) Residual lignin + other oxidable compounds + MnO + 4H → oxidized lignin + other oxidized
4
−
compounds + excess MnO + MnO + 2H O
4 2 2
− − +
2+
2) 2MnO + 10I + 16H → 2Mn + 5I + 8H O
4 2 2
+ −
2+
3) MnO + 4H + 2I → Mn + 2H O + I
2 2 2
2− 2− −
4) 2S O + I → S O + 2I
2 3 2 4 6
NOTE By theoretical calculation and experimental observation, a consumption of 60 % (mass/mass) is actually the
endpoint of the consumption for the permanganate ions, at which point the ions have been reduced to MnO . Further
2
oxidation, performed by means of MnO should be considered as “out of range”. By adding potassium iodide solution, the
2
reaction is terminated and the free iodine is titrated with sodium thiosulfate solution. The value so obtained is corrected to
50 % consumption of the total oxidation capacity of permanganate.
5 Reagents and materials
Use only chemicals of recognized analytical grade and only distilled water or water of equivalent purity.
5.1 Sulfuric acid, c(H SO ) = 2,0 mol/l.
2 4
Add with caution 112 ml of sulfuric acid, H SO , of density 1,84 g/ml, to about 600 ml of water. Allow to cool
2 4
and dilute to 1 litre with water.
5.2 Potassium iodide, c(KI) = 1 mol/l.
Dissolve 166 g of potassium iodide, KI, in a 1 000 ml volumetric flask and fill up to the mark with water.
5.3 Potassium permanganate, c(KMnO ) = (0,020 ± 0,001) mol/l.
4
Dissolve 3,161 g of potassium permanganate, KMnO , in a 1 000 ml volumetric flask and fill up to the mark
4
with water.
NOTE Fresh solution is stable for at least 6 months if stored in a dark bottle.
5.4 Sodium thiosulfate, c(Na S O ) = (0,200 0 ± 0,000 5 ) mol/l.
2 2 3
Dissolve 49,65 g of sodium thiosulfate, Na S O · 5H O, in a 1 000 ml volumetric flask and fill up to the mark
2 2 3 2
with water.
5.5 Starch indicator, 2 g/l solution.
NOTE Commercially available standard solutions may be used.
2 © ISO 2004 – All rights reserved

---------------------- Page: 8 ----------------------

SIST ISO 302:2011
ISO 302:2004(E)
6 Apparatus and equipment
Ordinary laboratory equipment and the following.
6.1 Agitator, of the propeller type, made of glass or other noncorrosive material (a plastic- or glass-covered
magnetic stirrer may be used instead).
6.2 Wet-disintegration apparatus or blender, high-speed mixer, capable of disintegrating the pulp
completely with minimum damage to the fibres.
6.3 Water bath, capable of maintaining a temperature of (25,0 ± 0,2) °C in the reaction vessel (see 8.3
regarding temperature correction).
6.4 Timing device, capable of measuring 10 min to the nearest 1 s.
NOTE Automatic Kappa number analysers can be used if they follow this International Standard and give the same
results.
7 Sampling and preparation of sample
7.1 Sampling
If the test is being made to evaluate a pulp lot, the sample shall be selected in accordance with ISO 7213. If
the test is made on another type of sample, report the source of the sample and if possible the sampling
procedure used.
Make sure that the test portions taken are representative of the pulp.
As the presence of small amounts of spent cooking liquor affects the Kappa number, ensure that the sample
is well washed.
7.2 Sample preparation
Prepare the test material according to one of the following procedures.
7.2.1 Air-dry pulp. Tear or cut the pulp into small pieces.
7.2.2 Screened slush pulp. Dewater the pulp sample by filtering on a Büchner funnel or by centrifuging,
avoiding any loss of fibres or fines. Air-dry the pulp sample, or dry it at a temperature not exceeding 105 °C,
and tear it into small pieces.
7.2.3 Unscreened pulp. If the sample is taken from unscreened pulp, which is normally screened before
bleaching or other processing, remove the shives and knots from the sample by screening. Choose a
procedure that gives results similar to those obtained by industrial screening. State the method of screening in
the test report. Continue the sample preparation as described in 7.2.2.
NOTE If the pulp sample contains a considerable amount of shives, the screening procedure may give rise to
incorrect results. A more reliable value may be obtained by defibrating the pulp sample before the determina
...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Pâtes -- Détermination de l'indice KappaPulps -- Determination of Kappa number85.040VlakninePulpsICS:Ta slovenski standard je istoveten z:ISO 302:2004oSIST ISO 302:2011en01-marec-2011oSIST ISO 302:2011SLOVENSKI
STANDARD



oSIST ISO 302:2011



Reference numberISO 302:2004(E)© ISO 2004
INTERNATIONAL STANDARD ISO302Second edition2004-07-01Pulps — Determination of Kappa numberPâtes — Détermination de l'indice Kappa
oSIST ISO 302:2011



ISO 302:2004(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
©
ISO 2004 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.
+ 41 22 749 01 11 Fax
+ 41 22 749 09 47 E-mail
[e-mail] Web
www.iso.org Published in Switzerland
ii © ISO 2004 – All rights reserved
oSIST ISO 302:2011



ISO 302:2004(E) © ISO 2004 – All rights reserved iii Contents Page Foreword.iv 1 Scope.1 2 Normative references.1 3 Terms and definitions.1 4 Principle.2 5 Reagents and materials.2 6 Apparatus and equipment.3 7 Sampling and preparation of sample.3 7.1 Sampling.3 7.2 Sample preparation.3 8 Procedure.3 8.1 General.3 8.2 Blank.4 8.3 Determination.4 9 Calculations.6 9.1 Kappa number 5 to 100.6 9.2 Kappa number 1 to 5.7 9.3 Expression of results.8 9.4 Example of calculation.8 10 Precision.8 10.1 Reference pulp.8 10.2 Repeatability.8 10.3 Reproducibility.9 11 Test report.9 Bibliography.10
oSIST ISO 302:2011



ISO 302:2004(E) iv © ISO 2004 – All rights reserved 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 302 was prepared by Technical Committee ISO/TC 6, Paper, board and pulps, Subcommittee SC 5, Test methods and quality specifications for pulps. This second edition cancels and replaces the first edition (ISO 302:1981), which has been technically revised. oSIST ISO 302:2011



INTERNATIONAL STANDARD ISO 302:2004(E) © ISO 2004 – All rights reserved 1 Pulps — Determination of Kappa number 1 Scope This International Standard specifies a method for the determination of the Kappa number of pulp. The Kappa number is an indication of the lignin content or bleachability of pulp. This International Standard is applicable to all kinds of chemical pulps and semi-chemical pulps within the Kappa number range 1 to 100. For pulps with a Kappa number exceeding 100, use the chlorine-consumption procedure (ISO 3260) to describe the degree of delignification. To achieve the greatest precision and accuracy, the sample size should be adjusted so that the consumption of permanganate falls between 20 % and 60 % of the amount added. NOTE There is no general and unambiguous relationship between the Kappa number and the lignin content of pulp. The relationship varies according to the wood species and delignification procedure. All compounds oxidized by KMnO4, not only lignin, will increase the consumption of KMnO4, and thereby increase the Kappa number (see [7]). If the Kappa number is to be used to derive an index of pulp lignin content, specific relationships will have to be developed for each pulp type.
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 638, Pulps — Determination of dry matter content ISO 7213, Pulps — Sampling for testing 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 oxidation capacity relative amount of permanganate oxidized (expressed as MnO2) of the total oxidation capacity 3.2 total oxidation capacity oxidation capacity (permanganate consumption) when all permanganate is oxidized into Mn2+ 3.3. Kappa number of pulp number of millilitres of 0,02 mol/l potassium permanganate solution consumed under the specified conditions by one gram of pulp (calculated on an oven-dry basis) NOTE The results are corrected to a value corresponding to that obtained when 50 % of the total oxidation capacity of the permanganate is consumed in the test at a temperature of 25 °C. oSIST ISO 302:2011



ISO 302:2004(E) 2 © ISO 2004 – All rights reserved 4 Principle Disintegrated pulp is allowed to react with a specified amount of potassium permanganate solution for a given time. The amount of pulp is chosen so that about 50 % of the total oxidation capacity of the permanganate is left unconsumed at the end of the reaction time.
The main reactions are as follows: 1) Residual lignin + other oxidable compounds + MnO4− + 4H+ → oxidized lignin + other oxidized compounds + excess MnO4− + MnO2 + 2H2O 2) 2MnO4− + 10I− + 16H+ → 2Mn2+ + 5I2 + 8H2O 3) MnO2 + 4H+ + 2I− → Mn2+ + 2H2O + I2 4) 2S2O32− + I2 → S4O62− + 2I− NOTE By theoretical calculation and experimental observation, a consumption of 60 % (mass/mass) is actually the endpoint of the consumption for the permanganate ions, at which point the ions have been reduced to MnO2. Further oxidation, performed by means of MnO2 should be considered as “out of range”. By adding potassium iodide solution, the reaction is terminated and the free iodine is titrated with sodium thiosulfate solution. The value so obtained is corrected to 50 % consumption of the total oxidation capacity of permanganate. 5 Reagents and materials Use only chemicals of recognized analytical grade and only distilled water or water of equivalent purity. 5.1 Sulfuric acid, c(H2SO4) = 2,0 mol/l. Add with caution 112 ml of sulfuric acid, H2SO4, of density 1,84 g/ml, to about 600 ml of water. Allow to cool and dilute to 1 litre with water. 5.2 Potassium iodide, c(KI) = 1 mol/l. Dissolve 166 g of potassium iodide, KI, in a 1 000 ml volumetric flask and fill up to the mark with water. 5.3 Potassium permanganate, c(KMnO4) = (0,020 ± 0,001) mol/l. Dissolve 3,161 g of potassium permanganate, KMnO4 , in a 1 000 ml volumetric flask and fill up to the mark with water.
NOTE Fresh solution is stable for at least 6 months if stored in a dark bottle.
5.4 Sodium thiosulfate, c(Na2S2O3) = (0,200 0 ± 0,000 5 ) mol/l. Dissolve 49,65 g of sodium thiosulfate, Na2S2O3 · 5H2O, in a 1 000 ml volumetric flask and fill up to the mark with water. 5.5 Starch indicator, 2 g/l solution. NOTE Commercially available standard solutions may be used. oSIST ISO 302:2011



ISO 302:2004(E) © ISO 2004 – All rights reserved 3 6 Apparatus and equipment Ordinary laboratory equipment and the following. 6.1 Agitator, of the propeller type, made of glass or other noncorrosive material (a plastic- or glass-covered magnetic stirrer may be used instead). 6.2 Wet-disintegration apparatus or blender, high-speed mixer, capable of disintegrating the pulp completely with minimum damage to the fibres. 6.3 Water bath, capable of maintaining a temperature of (25,0 ± 0,2) °C in the reaction vessel (see 8.3 regarding temperature correction). 6.4 Timing device, capable of measuring 10 min to the nearest 1 s. NOTE Automatic Kappa number analysers can be used if they follow this International Standard and give the same results. 7 Sampling and preparation of sample 7.1 Sampling If the test is being made to evaluate a pulp lot, the sample shall be selected in accordance with ISO 7213. If the test is made on another type of sample, report the source of the sample and if possible the sampling procedure used. Make sure that the test portions taken are representative of the pulp. As the presence of small amounts of spent cooking liquor affects the Kappa number, ensure that the sample is well washed.
7.2 Sample preparation Prepare the test material according to one of the following procedures. 7.2.1 Air-dry pulp. Tear or cut the pulp into small pieces.
7.2.2 Screened slush pulp. Dewater the pulp sample by filtering on a Büchner funnel or by centrifuging, avoiding any loss of fibres or fines. Air-dry the pulp sample, or dry it at a temperature not exceeding 105 °C, and tear it into small pieces.
7.2.3 Unscreened pulp. If the sample is taken from unscreened pulp, which is normally screened before bleaching or other processing, remove the shives and knots from the sample by screening. Choose a procedure that gives results similar to those obtained by industrial screening. State the method of screening in the test report. Continue the sample preparation as described in 7.2.2. NOTE If the pulp sample contains a considerable amount of shives, the screening procedure may give rise to incorrect results. A more reliable value may be obtained by defibrat
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