ISO 5647:2019

INTERNATIONAL ISO
STANDARD 5647
Second edition
2019-05
Paper and board — Determination of
titanium dioxide content
Papier et carton — Détermination de la teneur en dioxyde de titane
Reference number
©
ISO 2019
© ISO 2019
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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Selection of the sample . 3
8 Preparation of ash solution . 3
9 Reagent blank solution . 3
10 Spectrophotometric procedure . 3
10.1 Preparation of the calibration graph . 3
10.2 Preparation of the test solutions . 4
10.3 Spectrophotometric determination . 4
11 Flame atomic absorption spectrophotometric procedure . 4
11.1 Preparation of the calibration graph . 4
11.1.1 Preparation of the calibration solution . 4
11.1.2 Adjustment of apparatus . 4
11.1.3 Reagent blank determination . 5
11.1.4 Spectrophotometric measurement . 5
11.1.5 Plotting the calibration graph . 5
11.2 Determination . 5
11.2.1 Preparation of test solution . 5
11.2.2 Spectrophotometric measurement . 5
12 Expression of results . 5
13 Test report . 6
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 6, Paper, Board and Pulps.
This second edition cancels and replaces the first edition (ISO 5647:1990), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— Clause 4: The option of using Inductively Coupled Plasma/Atomic Emission Spectrometry (ICP/AES)
has been added.
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.
iv © ISO 2019 – All rights reserved

INTERNATIONAL STANDARD ISO 5647:2019(E)
Paper and board — Determination of titanium dioxide
content
WARNING — The method specified in this document involves the use of some hazardous
chemicals and of gases that can form explosive mixtures with air. Care shall be taken to ensure
that the relevant safety precautions are observed.
1 Scope
This document specifies a method for determining titanium dioxide content in all kinds of paper and
board, in particular coated or filled products. It comprises two procedures for the final determination
of titanium, one of them relying on spectrophotometry and the other on flame atomic absorption
spectrophotometry. The limits of the determination depend on the amount of sample taken (8.1).
NOTE The method is designed for the determination of titanium dioxide. Titanium present in other forms,
for example as a constituent of clay, will not interfere in the determination.
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 186, Paper and board — Sampling to determine average quality
ISO 287, Paper and board — Determination of moisture content of a lot — Oven-drying method
ISO 2144, Paper, board, pulps and cellulose nanomaterials — Determination of residue (ash content) on
ignition at 900 °C
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
titanium dioxide content
titanium dioxide content of paper or board (expressed on an oven-dry basis), determined after ashing
the sample and dissolving the ash by the method specified in this document
4 Principle
Titanium dioxide is determined by ashing the sample and dissolution of the ash in sulphuric acid
and ammonium sulphate. Determination of the titanium by spectrophotometry, applying hydrogen
peroxide, or by flame atomic absorption spectrophotometry, adding potassium chloride.
The determination of titanium, after ashing the sample and dissolution of the ash, can also be done by
ICP/AES (Inductively Coupled Plasma/Atomic Emission Spectrometry) provided that the results have
been validated.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity (5.1).
5.1 Distilled water or deionized water, conductivity less than 1 mS/m.
5.2 Sulphuric acid (H S0 ), ρ density 1,84 g/ml.
2 4
5.3 Ammonium sulphate [(NH ) SO ].
4 2 4
5.4 Diluted sulphuric acid. ln a beaker with approximately 500 ml of water (5.1) carefully add 100 ml
of sulphuric acid (5.2) and 40 g of ammonium sulphate (5.3). Dilute to 1 l with water (5.1).
5.5 Standard titanium dioxide solution, 500 mg of TiO per litre.
Weigh 0,500 g of titanium dioxide (TiO ) in a 500 ml beaker, add 40,0 g of ammonium sulphate (5.3)
and 100 ml of sulphuric acid (5.2). In a fume hood, gradually heat the mixture to boiling and then boil
for 5 min to 10 min. Cover the beaker and allow the solution to cool to room temperature and, while
stirring, pour it carefully into a larger beaker containing about 300 ml of water (5.1). When the solution
has reached room temperature, decant it quantitatively into a 1 000 ml volumetric flask. Rinse both
beakers with water and add the rinsings to the volumetric flask. Make up to the mark with water (5.1).
5.6 Hydrogen peroxide, solution containing 30 g of H O per litre. This solution is only required for
2 2
the spectrophotometric procedure
5.7 Potassium chloride, solution containing 20 g of KCl per litre. This solution is only required for the
flame atomic absorption spectrophotometric procedure.
5.8 Hydrochloric acid (HCI), solution 6 mol/l.
6 Apparatus
In addition to the usual laboratory apparatus the following are required.
6.1 Dishes, of platinum or quartz.
Wash the platinum dishes thoroughly and remove any traces of impurities by cleaning with fine sand.
Soak and boil the dishes in the 6 mol/l hydrochloric acid solution (5.8). Avoid contact with metals other
than platinum.
Wash the quartz dishes thoroughly and soak and boil them in the 6 mol/l hydrochloric acid solution (5.8).
6.2 Spectrophotometer or filter photometer, for determining absorbance at 410 nm. It shall have
10 mm cells provided with lids. This apparatus is only required for the spectrophotometric procedure.
6.3 Atomic absorption spectrophotometer, fitted with an acetylene and dinitrogen monoxide burner
and a titanium hollow-cathode lamp. This apparatus is only required for the flame atomic absorption
spectrophotometric procedure.
2 © ISO 2019 – All rights reserved

7 Selection of the sample
Select a representative sample in accordance with ISO 186. Tear the air-dry sample into pieces of
suitable size. Use protective cotton gloves. Do not use cut or punched edges or other parts where
metallic contamination may have occurred.
8 Preparation of ash solution
8.1 Carry out the determination in duplicate. Weigh, to the nearest 0,01 g, two test portions of about
10 g of paper or board and place each test portion in a clean dish (6.1). Determine the moisture content
of a separate test sample as prescribed in ISO 287.
NOTE Select the amount of sample to be ashed, taking into account the anticipated titanium dioxide
content. If a 10 g portion is ashed, the optimum range of the titanium dioxide content is from 1,5 g/kg to
8 g/kg (spectrophotometric procedure) or from 0,8 g/kg to 3,2 g/kg (flame atomic absorption spectrophotometric
procedure).
8.2 Ash the test portion as described in ISO 2144. Allow the dish to
...

SLOVENSKI STANDARD
01-november-2020
Papir, karton in lepenka - Določanje vsebnosti titanovega dioksida
Paper and board -- Determination of titanium dioxide content
Papier et carton -- Détermination de la teneur en dioxyde de titane
Ta slovenski standard je istoveten z: ISO 5647:2019
ICS:
85.060 Papir, karton in lepenka Paper and board
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 5647
Second edition
2019-05
Paper and board — Determination of
titanium dioxide content
Papier et carton — Détermination de la teneur en dioxyde de titane
Reference number
©
ISO 2019
© ISO 2019
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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 2
7 Selection of the sample . 3
8 Preparation of ash solution . 3
9 Reagent blank solution . 3
10 Spectrophotometric procedure . 3
10.1 Preparation of the calibration graph . 3
10.2 Preparation of the test solutions . 4
10.3 Spectrophotometric determination . 4
11 Flame atomic absorption spectrophotometric procedure . 4
11.1 Preparation of the calibration graph . 4
11.1.1 Preparation of the calibration solution . 4
11.1.2 Adjustment of apparatus . 4
11.1.3 Reagent blank determination . 5
11.1.4 Spectrophotometric measurement . 5
11.1.5 Plotting the calibration graph . 5
11.2 Determination . 5
11.2.1 Preparation of test solution . 5
11.2.2 Spectrophotometric measurement . 5
12 Expression of results . 5
13 Test report . 6
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 6, Paper, Board and Pulps.
This second edition cancels and replaces the first edition (ISO 5647:1990), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— Clause 4: The option of using Inductively Coupled Plasma/Atomic Emission Spectrometry (ICP/AES)
has been added.
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.
iv © ISO 2019 – All rights reserved

INTERNATIONAL STANDARD ISO 5647:2019(E)
Paper and board — Determination of titanium dioxide
content
WARNING — The method specified in this document involves the use of some hazardous
chemicals and of gases that can form explosive mixtures with air. Care shall be taken to ensure
that the relevant safety precautions are observed.
1 Scope
This document specifies a method for determining titanium dioxide content in all kinds of paper and
board, in particular coated or filled products. It comprises two procedures for the final determination
of titanium, one of them relying on spectrophotometry and the other on flame atomic absorption
spectrophotometry. The limits of the determination depend on the amount of sample taken (8.1).
NOTE The method is designed for the determination of titanium dioxide. Titanium present in other forms,
for example as a constituent of clay, will not interfere in the determination.
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 186, Paper and board — Sampling to determine average quality
ISO 287, Paper and board — Determination of moisture content of a lot — Oven-drying method
ISO 2144, Paper, board, pulps and cellulose nanomaterials — Determination of residue (ash content) on
ignition at 900 °C
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
titanium dioxide content
titanium dioxide content of paper or board (expressed on an oven-dry basis), determined after ashing
the sample and dissolving the ash by the method specified in this document
4 Principle
Titanium dioxide is determined by ashing the sample and dissolution of the ash in sulphuric acid
and ammonium sulphate. Determination of the titanium by spectrophotometry, applying hydrogen
peroxide, or by flame atomic absorption spectrophotometry, adding potassium chloride.
The determination of titanium, after ashing the sample and dissolution of the ash, can also be done by
ICP/AES (Inductively Coupled Plasma/Atomic Emission Spectrometry) provided that the results have
been validated.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity (5.1).
5.1 Distilled water or deionized water, conductivity less than 1 mS/m.
5.2 Sulphuric acid (H S0 ), ρ density 1,84 g/ml.
2 4
5.3 Ammonium sulphate [(NH ) SO ].
4 2 4
5.4 Diluted sulphuric acid. ln a beaker with approximately 500 ml of water (5.1) carefully add 100 ml
of sulphuric acid (5.2) and 40 g of ammonium sulphate (5.3). Dilute to 1 l with water (5.1).
5.5 Standard titanium dioxide solution, 500 mg of TiO per litre.
Weigh 0,500 g of titanium dioxide (TiO ) in a 500 ml beaker, add 40,0 g of ammonium sulphate (5.3)
and 100 ml of sulphuric acid (5.2). In a fume hood, gradually heat the mixture to boiling and then boil
for 5 min to 10 min. Cover the beaker and allow the solution to cool to room temperature and, while
stirring, pour it carefully into a larger beaker containing about 300 ml of water (5.1). When the solution
has reached room temperature, decant it quantitatively into a 1 000 ml volumetric flask. Rinse both
beakers with water and add the rinsings to the volumetric flask. Make up to the mark with water (5.1).
5.6 Hydrogen peroxide, solution containing 30 g of H O per litre. This solution is only required for
2 2
the spectrophotometric procedure
5.7 Potassium chloride, solution containing 20 g of KCl per litre. This solution is only required for the
flame atomic absorption spectrophotometric procedure.
5.8 Hydrochloric acid (HCI), solution 6 mol/l.
6 Apparatus
In addition to the usual laboratory apparatus the following are required.
6.1 Dishes, of platinum or quartz.
Wash the platinum dishes thoroughly and remove any traces of impurities by cleaning with fine sand.
Soak and boil the dishes in the 6 mol/l hydrochloric acid solution (5.8). Avoid contact with metals other
than platinum.
Wash the quartz dishes thoroughly and soak and boil them in the 6 mol/l hydrochloric acid solution (5.8).
6.2 Spectrophotometer or filter photometer, for determining absorbance at 410 nm. It shall have
10 mm cells provided with lids. This apparatus is only required for the spectrophotometric procedure.
6.3 Atomic absorption spectrophotometer, fitted with an acetylene and dinitrogen monoxide burner
and a titanium hollow-cathode lamp. This apparatus is only required for the flame atomic absorption
spectrophotometric procedure.
2 © ISO 2019 – All rights reserved

7 Selection of the sample
Select a representative sample in accordance with ISO 186. Tear the air-dry sample into pieces of
suitable size. Use protective cotton gloves. Do not use cut or punched ed
...