IEC TS 62607-4-8:2020

IEC TS 62607-4-8 ®
Edition 1.0 2020-02
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –
Part 4-8: Nano-enabled electrical energy storage – Determination of water
content in electrode nanomaterials, Karl Fischer method
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 IEC or IEC's member National Committee in the country of the requester. If you have any questions about IEC
copyright or have an enquiry about obtaining additional rights to this publication, please contact the address below or
your local IEC member National Committee for further information.

IEC Central Office Tel.: +41 22 919 02 11
3, rue de Varembé info@iec.ch
CH-1211 Geneva 20 www.iec.ch
Switzerland
About the IEC
The International Electrotechnical Commission (IEC) is the leading global organization that prepares and publishes
International Standards for all electrical, electronic and related technologies.

About IEC publications
The technical content of IEC publications is kept under constant review by the IEC. Please make sure that you have the
latest edition, a corrigendum or an amendment might have been published.

IEC publications search - webstore.iec.ch/advsearchform Electropedia - www.electropedia.org
The advanced search enables to find IEC publications by a The world's leading online dictionary on electrotechnology,
variety of criteria (reference number, text, technical containing more than 22 000 terminological entries in English
committee,…). It also gives information on projects, replaced and French, with equivalent terms in 16 additional languages.
and withdrawn publications. Also known as the International Electrotechnical Vocabulary

(IEV) online.
IEC Just Published - webstore.iec.ch/justpublished
Stay up to date on all new IEC publications. Just Published IEC Glossary - std.iec.ch/glossary
details all new publications released. Available online and 67 000 electrotechnical terminology entries in English and
once a month by email. French extracted from the Terms and Definitions clause of
IEC publications issued since 2002. Some entries have been
IEC Customer Service Centre - webstore.iec.ch/csc collected from earlier publications of IEC TC 37, 77, 86 and
If you wish to give us your feedback on this publication or CISPR.

need further assistance, please contact the Customer Service

Centre: sales@iec.ch.
IEC TS 62607-4-8 ®
Edition 1.0 2020-02
TECHNICAL
SPECIFICATION
colour
inside
Nanomanufacturing – Key control characteristics –

Part 4-8: Nano-enabled electrical energy storage – Determination of water

content in electrode nanomaterials, Karl Fischer method

INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
ICS 07.030; 07.120 ISBN 978-2-8322-7813-0

– 2 – IEC TS 62607-4-8:2020 © IEC 2020
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 7
4 Principle . 8
5 Reagents . 9
5.1 Coulometric Karl Fischer reagent . 9
5.2 Methanol (anhydrous) . 9
5.3 Carrier gas . 9
5.4 Water standard for Karl Fischer coulometric titration . 9
6 Apparatus . 9
6.1 Karl Fischer coulometric titration apparatus . 9
6.2 Evaporator . 9
6.3 Analytical balance . 10
6.4 Sample container . 10
6.5 Micro-syringe . 10
6.6 Dew-point hygrometer . 10
7 Sample handling and sampling . 10
7.1 Sample handling . 10
7.2 Sampling. 11
8 Procedure . 11
8.1 Maintenance . 11
8.1.1 Reagent change . 11
8.1.2 Cleaning . 11
8.1.3 Calibration . 11
8.2 Measurement steps . 11
8.3 Water content of the sample . 12
9 Precision . 13
9.1 General . 13
9.2 Repeatability . 13
9.3 Reproducibility . 13
10 Test report . 13
Annex A (informative) Case study . 14
A.1 General . 14
A.2 Reagents . 14
A.2.1 Coulometric Karl Fischer reagent . 14
A.2.2 Methanol (anhydrous) . 14
A.2.3 Carrier gas . 14
A.2.4 Water standard for Karl Fischer coulometric titration . 14
A.3 Apparatus . 14
A.3.1 Karl Fischer coulometric titration apparatus . 14
A.3.2 Evaporator . 14
A.3.3 Analytical balance . 14
A.3.4 Sample container . 14
A.3.5 Micro-syringe . 14

A.3.6 Dew-point hygrometer. 15
A.4 Sampling. 15
A.5 Measurement steps . 15
A.6 Test results . 15
Bibliography . 17

Figure 1 – Example of Karl Fischer coulometric titration apparatus and evaporator . 10
Figure A.1 – Sample container . 15

Table 1 – Sample mass against water to be determined . 11
Table A.1 – Test data of water content in sample A . 16

– 4 – IEC TS 62607-4-8:2020 © IEC 2020
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 4-8: Nano-enabled electrical energy storage – Determination of
water content in electrode nanomaterials, Karl Fischer method

FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote
international co-operation on all questions concerning standardization in the electrical and electronic fields. To
this end and in addition to other activities, IEC publishes International Standards, Technical Specifications,
Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC
Publication(s)”). Their preparation is entrusted to technical committees; any IEC National Committee interested
in the subject dealt with may participate in this preparatory work. International, governmental and non-
governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely
with the International Organization for Standardization (ISO) in accordance with conditions determined by
agreement between the two organizations.
2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
consensus of opinion on the relevant subjects since each technical committee has representation from all
interested IEC National Committees.
3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC
Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any
misinterpretation by any end user.
4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications
transparently to the maximum extent possible in their national and regional publications. Any divergence
between any IEC Publication and the corresponding national or regional publication shall be clearly indicated in
the latter.
5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity
assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any
services carried out by independent certification bodies.
6) All users should ensure that they have the latest edition of this publication.
7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and
members of its technical committees and IEC National Committees for any personal injury, property damage or
other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and
expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC
Publications.
8) Attention is drawn to the normative references cited in this publication. Use of the referenced publications is
indispensable for the correct application of this publication.
9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of
patent rights. IEC shall not be held responsible for identifying any or all such patent rights.
The main task of IEC technical committees is to prepare International Standards. In
exceptional circumstances, a technical committee may propose the publication of a Technical
Specification when
• the required support cannot be obtained for the publication of an International Standard,
despite repeated efforts, or
• the subject is still under technical development or where, for any other reason, there is the
future but no immediate possibility of an agreement on an International Standard.
Technical Specifications are subject to review within three years of publication to decide
whether they can be transformed into International Standards.
IEC TS 62607-4-8, which is a Technical Specification, has been prepared by IEC technical
committee 113: Nanotechnology for electrotechnical products and systems.

The text of this Technical Specification is based on the following documents:
DTS Report on voting
113/491/DTS 113/515/RVDTS
Full information on the voting for the approval of this Technical Specification can be found in
the report on voting indicated in the above table.
This document has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 62607 series, published under the general title
Nanomanufacturing – Key control characteristics, can be found on the IEC website.
The committee has decided that the contents of this publication will remain unchanged until
the stability date indicated on the IEC website under "http://webstore.iec.ch" in the data
related to the specific publication. At this date, the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates
that it contains colours which are considered to be useful for the correct
understanding of its contents. Users should therefore print this document using a
colour printer.
– 6 – IEC TS 62607-4-8:2020 © IEC 2020
INTRODUCTION
Nano-enabled electrical energy storage has been applied in many fields such as portable
electronics, electric vehicles and energy storage systems. With continuous rapid development
in these applications, nano-enabled electrical energy storage with high performance is in
demand. The main properties of the electrical energy storage device are determined by its
electrode nanomaterials.
The water content for electrode nanomaterials is one of the important characteristics to be
determined as a quality control test. Water can affect electrical performance, cycling
performance and safety performance of nano-enabled electrical energy storage devices
[1] , [2]. A high amount of water from electrode materials has a critical influence on both
active materials and battery cells [3], and might affect performance or safety characteristics.
Several methods are available for the determination of water content. Karl Fischer titration
method is a direct method that is suitable for testing water in gas, liquid and solid samples.
The method is useful for low water content levels (< 1 %). Especially, Karl Fischer coulometric
titration method is an absolute method which can determine the water content from the
quantity of electricity consumed during the test. It can detect trace levels of free water (ppm
level), which cannot be detected with normal drying or gravimetric methods. The Karl Fischer
coulometric titration method is capable of distinguishing water levels as low as 0,000 1 %.
At present, there are 21 International Standards and/or Technical Specifications mentioning
the Karl Fischer method to measure water content, of which 16 use the volumetric titration
method, and 5 use the coulometric titration method. The accuracy and resolution of the
volumetric method is not appropriate for electrode nanomaterials, whose water content is
lower than 1 %. The sampling and measurement controls of the current coulometric method
standards are not appropriate for electrode nanomaterials, which have highly hygroscopic
characteristics. Therefore, the present standards are not suitable for electrode nanomaterials.
This document, considering a sample’s characteristic, will help to determine the water content
of the electrode nanomaterials in a short time with high accuracy, and will be helpful for
quality control in laboratories and industrial manufacturers.
This standardized method is intended for use in comparing the characteristics of raw
materials [e.g. lithium cobalt oxide (LCO), lithium nickel cobalt aluminium oxide (NCA), lithium
nickel cobalt manganese oxide (NCM), and lithium iron phosphate (LFP)] without any
additives [e.g. carbon nanomaterials like carbon black (CB), carbon nanotubes or fibres] or
organic binder [e.g. polyvinylidene difluoride (PVDF) or styrene-butadiene rubber (SBR)], their
selection process and as a quality control method for the fully formulated electrode material,
not for evaluating the electrode in end products.

___________
Numbers in square brackets refer to the Bibliography.

NANOMANUFACTURING –
KEY CONTROL CHARACTERISTICS –
Part 4-8: Nano-enabled electrical energy storage – Determination of
water content in electrode nanomaterials, Karl Fischer method

1 Scope
This part of IE
...