ISO/FDIS 12467-1

• Abstract:

  This International Standard specifies methods for the chemical analysis of lithium nickel manganese cobalt oxide (NMC) powders used as the raw material for cathode materials. This document stipulates the determination methods of nickel, manganese, cobalt, aluminium, barium, calcium, copper, iron, lead, magnesium, molybdenum, phosphorus, sodium, strontium, titanium, zinc, zirconium, lithium hydroxide (LiOH) and lithium carbonate (Li2CO3) contents in NMC powders. NMC powders are decomposed by an acid decomposition method. The nickel, manganese, cobalt, aluminium, barium, calcium, copper, iron, lead, magnesium, molybdenum, phosphorus, sodium, strontium, titanium, zinc and zirconium contents in the test solution are determined by an inductively coupled plasma—optical emission spectrometry (ICP-OES). Li2CO3 and LiOH are determined by using an acid-base titration.

• Status: Not Published
• ICS: 71.040.40 - Chemical analysis
• Technical Committee: ISO/TC 333 - Lithium
• Drafting Committee: ISO/TC 333 - Lithium
• Current Stage: 5020 - FDIS ballot initiated: 2 months. Proof sent to secretariat
• Start Date: 16-Sep-2026
• Completion Date: 16-Sep-2026

ISO/FDIS 12467-1 is an ISO International Standard for chemical analysis of lithium composite oxides, focused on NMC powders used as raw material for cathode materials. It specifies how to determine the main components by inductively coupled plasma optical emission spectrometry (ICP-OES), and how to determine Li2CO3 and LiOH by acid-base titration. It is written for laboratories and other users who need a controlled method for composition checking of lithium-ion battery materials.

What does ISO/FDIS 12467-1 specify?

ISO/FDIS 12467-1 specifies an analytical procedure for lithium nickel manganese cobalt oxide (NMC) powders, with a particular focus on the main elements used to define cathode composition. It also covers selected impurity or companion elements, plus Li2CO3 and LiOH in the powder.

The document is organized into clauses 1 to 12, followed by Annex A. Clause 7 gives example working ranges, Clause 9 sets out the preparation and measurement steps, Clause 10 covers calculation and expression of results, and Annex A reports interlaboratory test results.

Annex	What it covers
Annex A	Informative results of an interlaboratory test on two NMC samples

What are the key requirements of ISO/FDIS 12467-1?

Sample collection and preparation

ISO/FDIS 12467-1 relies on representative sampling and careful drying before analysis. Clause 8 says the sample collection and preparation should follow ISO 8656-1 unless the laboratory and customer agree otherwise, and the test sample should be homogenized until a representative amount is obtained.

This matters because NMC powders can vary within a batch. A poor sample split or uneven moisture content can change the measured composition even when the material itself is acceptable.

The clause also requires a weighed test portion of about 100 mg, taken to the nearest 0.1 mg. In practice, this means the balance, handling and sample containers all affect the final result.

Digestion and solution preparation

Clause 9 uses acid digestion as the core sample-preparation step. The powder is dissolved in a suitable acid mixture, and the resulting solution is combined with an internal standard solution before measurement.

This is important because the method measures elements in solution, not in the powder directly. If the sample does not dissolve fully, the result can be biased or incomplete.

If insoluble material remains, the document gives two practical paths: filter it out when only stoichiometric composition is needed, or redigest with a different acid mixture when exact content is required. That distinction helps the user decide whether the result is suitable for composition control or for full quantitative analysis.

ICP-OES measurement and calibration

Clause 9.3 and 9.10 require ICP-OES set-up, wavelength selection, calibration, and background correction. The method uses simultaneous measurement of analyte and internal standard lines, and the instrument should be thermally stable before calibration.

Clause 9.7 requires at least three calibration solutions and a linearity check, with a very high coefficient of determination. In practice, that means the calibration curve must be strong enough to support routine batch analysis.

The method also uses bracketing, where each sample is measured between low and high standards. This reduces drift effects and helps the result stay close to the standards used for calculation.

Internal standard and recovery control

Clause 9.4 requires an internal standard that is not analyzed and not present in the sample. Typical choices named in the document include Sc, Y, In, Ge and Lu.

This matters because the internal standard compensates for signal variation during nebulization, plasma behavior and instrument drift. For the analyst, it is a control on measurement stability, not a second target element.

Clause 9.5 and 9.10 use cadmium as a recovery check for sample preparation. If the recovery is outside the stated acceptance band, the sample preparation must be repeated. That gives a practical check that digestion and transfer were successful before reporting results.

Calculation, repeatability and stoichiometric content

Clause 10 explains how to convert the measured intensity ratios into concentrations and then into sample content. The calculation uses the internal-standard approach and the exact sample mass and final solution volume.

This matters because the laboratory does not report only an instrument reading. It must trace the result back to the weighed portion of powder and the prepared solution.

Clause 10.2 requires duplicate determinations to agree closely, and Clause 10.3 gives the conversion to stoichiometric content in mol/kg and percentage ratio terms. That is the part a battery-material user needs when checking whether the NMC composition matches the intended cathode design.

Quality assurance and reporting

Clause 11 links the work to ISO/IEC 17025 and sets acceptance criteria for the calibration curve and control checks. Clause 12 then lists the minimum test-report information, including sample identification, sampling procedure, method reference, results, deviations, anomalies, date, laboratory identification, and responsible personnel.

In practice, these clauses turn the chemistry into a defensible laboratory record. They support traceability, review of abnormal results, and later comparison between laboratories.

What terms does ISO/FDIS 12467-1 define?

• laboratory sample - the sample prepared for sending to the laboratory for inspection or testing.
• test sample - the sample prepared from the laboratory sample, from which test portions are taken.
• test portion - the amount of material actually used for the test.
• test sample solution - the solution prepared after extraction or digestion of the test sample.
• standard solution - a solution with accurately known concentration of an element, ion, compound or group.
• calibration solution - a solution used to calibrate the instrument, prepared from stock solution(s) or a certified standard.
• calibration blank solution - a calibration solution prepared without the analyte.
• bracketing - an analytical approach where the sample signal is measured between two nearby calibration solutions.

Who uses ISO/FDIS 12467-1?

ISO/FDIS 12467-1 is used by analytical laboratories, battery-material producers, and quality-control teams working with lithium-ion battery cathode materials. It is relevant where NMC powder composition must be checked against a target formulation or batch specification.

It is also useful for laboratory managers and buyers who need a repeatable method for comparing suppliers or verifying incoming raw materials. The document supports routine production control, release testing, and laboratory-to-laboratory comparison.

Which standards are used with ISO/FDIS 12467-1?

• ISO 1042 - provides the specification for one-mark volumetric flasks used when preparing calibration and test solutions.
• ISO 7819 - provides the lithium vocabulary that the document draws on for terms and definitions.
• ISO 8656-1 - gives the sampling scheme referenced for collecting raw material samples.
• ISO/IEC 17025 - sets the competence and quality framework for the laboratories that apply the method.

What does the ISO/FDIS 12467-1 document contain?

ISO/FDIS 12467-1 contains a full analytical workflow, from sampling through digestion, calibration, measurement, calculation and reporting. It includes reagent lists, apparatus requirements, and guidance on cleaning glassware and setting up the ICP-OES instrument.

The document also provides example analytical wavelengths for target elements and recommended wavelengths for internal standards. Clause 7 gives example working ranges for the main analytes, which helps a laboratory judge whether the method suits its sample.

It includes calibration solution preparation examples for NMC material and a recovery-check approach based on cadmium. The calculation section sets out the result conversion steps and the stoichiometric-content calculation used for cathode composition work.

Annex A presents interlaboratory test results for two NMC samples, giving users evidence of how the method performed across multiple laboratories.

FINAL DRAFT
International
Standard
ISO/TC 333
Chemical analysis of lithium
Secretariat: SAC
composite oxides —
Voting begins on:
2026-09-16
Part 1:
Determination of main components
Voting terminates on:
2026-11-11
by inductively coupled plasma
optical emission spectrometry
Analyse chimique des oxydes composites de lithium —
Partie 1: Détermination des principaux composants par
spectrométrie d'émission optique à plasma induit
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
FINAL DRAFT
International
Standard
ISO/TC 333
Chemical analysis of lithium
Secretariat: SAC
composite oxides —
Voting begins on:
Part 1:
Determination of main components
Voting terminates on:
by inductively coupled plasma
optical emission spectrometry
Analyse chimique des oxydes composites de lithium —
Partie 1: Détermination des principaux composants par
spectrométrie d'émission optique à plasma induit
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
© ISO 2026
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
5 Reagents and solutions . 3
6 Apparatus . 4
7 Determined elements and concentration ranges . 5
8 Sampling . 6
8.1 General .6
8.2 Test sample .6
8.3 Drying .6
8.4 Test portion .6
9 Procedure . 6
9.1 Cleaning of glassware.6
9.2 Instrument performance parameters .6
9.3 Instrument set-up .7
9.3.1 General requirements .7
9.3.2 Software method development, wavelength selection .7
9.3.3 Preliminary instrument check .7
9.4 Internal standard solution .8
9.5 Sample preparation recovery solution .8
9.6 Calibration blank solution .8
9.7 Calibration solutions .8
9.8 Sample preparation .9
9.9 Test sample solutions . .9
9.10 Measurements .9
10 Calculation and expression of results . 10
10.1 Calculation .10
10.2 Repeatability .11
10.3 Calculation to stochiometric content . 12
11 Quality assurance .12
11.1 General . 12
11.2 Calibration curve . 12
12 Test report .12
Annex A (informative) Results of interlaboratory test . 14
Bibliography .15

iii
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 333, Lithium.
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
Introduction
Lithium, its alloys and compounds are technologically important and highly versatile materials, and are
used in various industries, such as electronics, ceramics, glasses, medicine, etc.
Lithium is the lightest solid element, and due to the high electrochemical potential of the redox couple Li/
Li+, its main use is as cathode material in lithium ion batteries (LiBs) in electric vehicles, laptops, mobile
phones and digital cameras. Examples of commonly used lithium composite oxide cathode materials and
their principal constituents are shown in Table 1. Lithium materials are classified into different grades,
according to their chemical and physical characteristics, including purity, impurities, and particle size.
Therefore, the content of lithium materials are an important index to monitor product quality. The
determination of content by inductively coupled plasma optical emission spectrometry (ICP-OES) have
numerous advantages, such as simple sample-pre-treatment, high accuracy and low detection limit.
Table 1 — Types of Li composite oxides for LiBs
Acronym Chemical formula
LCO Li-xCoO
LMO Li-xMn O
2 4
NCA Li-xNiCoAlO
NMC Li-x(Ni Mn Co )O
x y z 2
LFP Li-xFePO
LNO Li-xNiO
LMP Li-xMnPO
LMFP Li-xMnFePO
LTO Li-xTi O
5 12
OLO -
NOTE 1 For the purposes of this document, the term 'lithium composite oxides' includes lithium-containing cathode
materials such as layered oxides, spinel oxides and phosphate-based materials.
NOTE 2 New types of LiB can also be analysed by this method.
NOTE 3 The method is applicable for the other elements listed above, provided the user has verified the applicability.
This document specifies an analytical procedure for the determination of main components in Li composite
oxides for Li-ion batteries (LiB). The determination is applicable to all types of LiBs (see Table 1). The
determination is performed by optical emission spectrometry with inductively coupled plasma (ICP OES)
using an internal standard. The method of atomic emission spectrometry with inductively coupled plasma
(ICP AES) is interchangeable with ICP OES.
This test is recommended as the preferred method for determining the stoichiometric composition of several
elements in LiBs.
v
FINAL DRAFT International Standard ISO/FDIS 12467-1:2026(en)
Chemical analysis of lithium composite oxides —
Part 1:
Determination of main components by inductively coupled
plasma optical emission spectrometry
WARNING — The use of this document can involve hazardous materials, operations, and equipment.
This document does not purport to address any safety problems associated with its use. It is the
responsibility of the user of this document to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies an analytical procedure for the determination of main components in Li composite
oxides for Li-ion batteries (LiB), in particular the elements: lithium, cobalt, iron, manganese, nickel,
phosphorus, titanium and aluminium, depending on the composite oxide of interest.
This document establishes a test procedure for a high precision determination of stoichiometric composition
of the elements in LiBs.
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 1042, Laboratory glassware — One-mark volumetric flasks
ISO 7819, Lithium — Vocabulary
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 7819 and the following apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
laboratory sample
sample as prepared for sending to the laboratory and intended for inspection or testing
[SOURCE: ISO 78-2:1999, 3.1]
3.2
test sample
sample prepared from the laboratory sample (3.1) and from which test portions (3.3) will be taken
[SOURCE: ISO 78-2:1999, 3.2]
3.3
test portion
quantity of material drawn from the test sample (3.2) (or from the laboratory sample if both are the same)
and on which the test or observation is actually carried out
[SOURCE: ISO 78-2:1999, 3.3]
3.4
test sample solution
solution prepared after extraction or digestion of the test sample according to appropriate specifications
Note 1 to entry: A sample solution can be subjected to further operations, e.g., dilution and/or addition of an internal
standard, in order to produce a test solution that is ready for analysis.
[SOURCE: ISO 22036:2024, 3.10]
3.5
standard solution
solution of accurately known concentration of an element, an ion, a compound or a group derived from the
substance used for its preparation
[SOURCE: ISO 78-2:1999, 3.6]
3.6
stock solution
solution of accurately known analyte concentration(s), prepared from pure chemicals
3.7
calibration solution
solution used to calibrate the instrument, prepared from (a) stock solution(s) or from a certified standard
[SOURCE: ISO 17294-1:2024, 3.4]
3.8
calibration blank solution
solution prepared in the same way as the calibration solution (3.7) but leaving out the analyte
[SOURCE: ISO 17294-1:2024, 3.3]
3.9
blank test solution
solution prepared by adding to the solvent the same amounts of reagents as those added to the test sample
solution and with the same final volume
[SOURCE: ISO 17294-1:2024, 3.19]
3.10
bracketing
analytical method consisting of bracketing the measured emission line intensity of the sample between two
measurements made on calibration solutions of neighbouring concentrations within the optimum working
range
Note 1 to entry: Running of standards and samples in the following sequence: low standard – sample – high standard –
sample – low standard – sample – high standard.
[SOURCE: ISO 19919:2025, 3.2]
3.11
calibration curve
expression of the relation between indication and corresponding measured quantity value
[SOURCE: ISO/IEC Guide 99:2007, 4.31]
3.12
calibration curve control
standard prepared independently of the calibration curve, the concentration of which is near the midpoint
of the calibration range
3.13
linearity
straight-line relationship between the mean result of measurement and the quantity (concentration) of the
analyte
4 Principle
The determination is carried out by means of the analytical technique of optical emission spectroscopy with
inductively coupled plasma (ICP-OES), which allows the detection and quantitative determination of most of
the elements from the periodic table from samples in solution.
In the ICP-OES technique, the continuous introduction of the liquid sample and a nebulization system forms
an aerosol that is transported by Argon to the plasma torch, inductively coupled by radio frequency. In the
plasma, due to the high temperatures generated, the analytes are atomized and ionized, generating the
atomic emission spectra of characteristic lines. The spectra are scattered by the diffraction grating and the
light-sensitive detector measures the spectral line intensities. The information is processed by the computer
software system of the ICP-OES equipment.
At least two accurately weighed samples are dissolved in a suitable acid mixture. After dissolution, this
sample solution is mixed with an exact mass of an internal standard solution and made up to the measurement
final volume. Using ICP-OES, the main contents of the sample solution are measured by comparing the
intensities of the spectral emissions of the main components and (a) suitable internal standard line(s) with
the intensities of a solution where the contained mass of these elements and internal standard is precisely
known. The bracketing method is used for this purpose.
5 Reagents and solutions
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade.
WARNING — Concentrated mineral acids (5.2, 5.3, 5.4, 5.5, 5.6, 5.7) are corrosive and acid vapour
is an irritant. Avoid contact with the skin or eyes, or inhalation of the vapour. Use suitable personal
protective equipment (e.g., gloves, face shield or safety goggles, etc.) when working with concentrated
or dilute acid. Handle open vessels containing concentrated acid in a fume hood. Do not add water to
acid, as the reaction is violent. Small aliquots of acid shall be added slowly to larger volumes of water.
The vapour pressure of acid is high; therefore beware of pressure build-up in stoppered flasks when
preparing acid/water mixtures.
5.1 Water (H O), (see ISO 3696), grade 1.
®1)
5.2 Hydrochloric acid (HCl), (CAS RN 7647-01-0), 30 % to 37 % HCl (mass fraction).
5.3 Nitric acid (HNO ), (CAS RN 7697-37-2), 65 % minimum HNO (mass fraction).
3 3
1) CAS Registry Number® is a trademark of the American Chemical Society (ACS). This information is given for the
convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent
products may be used if they can be shown to lead to the same results.

5.4 Perchloric acid (HClO ), (CAS RN 7601-90-3), 70 % to 73 % HClO (mass fraction).
4 4
5.5 Sulfuric acid (H SO ), (CAS RN 7664-93-9), 95 % minimum H SO (mass fraction).
2 4 2 4
5.6 Hydrofluoric acid (HF), (CAS RN 7664-39-3), 40 % to 42 % HF (mass fraction).
WARNING — Concentrated hydrofluoric acid is very toxic in contact with the skin and if inhaled or
swallowed. It is corrosive and causes severe burns. Take extreme care when using hydrofluoric acid.
Avoid contact with the skin or eyes, or inhalation of the vapour. It is essential that suitable personal
protective equipment (including suitable gloves, face shield, etc.) is used when working with
concentrated or dilute hydrofluoric acid. Handle open vessels containing concentrated hydrofluoric
acid in a fume hood. Ensure that the nature and seriousness of hydrofluoric acid burns is understood
before commencing work with this substance. Carry hydrofluoric acid burn cream (containing
calcium gluconate) at all times whilst working with hydrofluoric acid and for 24 h afterwards. Apply
the cream to any contaminated skin, after washing the affected area with copious amounts of water.
Obtain medical advice immediately in case of an accident.
NOTE The burning sensation associated with many concentrated acid burns is not immediately apparent on
exposure to hydrofluoric acid and will possibly not be felt for several hours. Relatively dilute solutions of hydrofluoric
acid can also be absorbed through the skin, with serious effects similar to those resulting from exposure to the
concentrated acid.
When using hydrofluoric acid, it is recommended that a pair of disposable gloves be worn underneath
suitable acid-resistant gloves to provide added protection for the hands.
5.7 Aqua regia (should be prepared just before use).
Mix three volumes of hydrochloric acid (5.2) and one volume of nitric acid (5.3).
5.8 Single element standard stock solutions, 1 000 or 10 000 mg/L
where c(element) is the concentration of the element.
Al, Co, Fe, Li, Mn, Ni, P, Ti; c = 1 000 or 10 000 mg/L each.
(element)
For internal standard the following elements can be used :
Be, Cd, Ge, In, Ru, Sc, Y; c = 1 000 or 10 000 mg/L each.
(element)
Single element standard stock solutions with adequate specification stating the acid used and the
preparation technique are commercially available. Single-element standard stock solutions can be made
from high purity metals or salts or oxides.
For stability of the solutions, refer to the manufacturer guarantee statement.
5.9 Argon gas (CAS RN 7440-37-1), purity ≥ 99,995 % (mass fraction).
6 Apparatus
All apparatus shall be carefully cleaned prior to use.
6.1 Inductively coupled argon plasma optical emission spectrometer
The
...

ISO/DISFDIS 12467-1:2025(en)
Date:2025-02-09
ISO /TC 333/SC /WG 6
Secretariat: SAC
Date: 2026-09-01
Chemical analysis of lithium composite oxides – —
Part 1:
Determination of main components by inductively coupled plasma
optical emission spectrometry
Analyse chimique des oxydes composites de lithium —
Partie 1: Détermination des principaux composants par spectrométrie d'émission optique à plasma induit
FDIS stage
ISO #####-#:####(X/FDIS 12467-1:2026(en)
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'sISO’s member body in the country of the requester.
ISO Copyright Officecopyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
Email:
E-mail: [e-mail]
Website: www.iso.org
Published in Switzerland.
© ISO #### 2026 – All rights reserved
ii
ISO/DISFDIS 12467-1:2026(en)
© ISO 2026 – All rights reserved
iii
ISO #####-#:####(X/FDIS 12467-1:2026(en)
Contents
Foreword . v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
5 Reagents and solutions . 4
6 Apparatus . 5
7 Determined elements and concentration ranges . 6
8 Sampling . 6
8.1 General . 6
8.2 Test sample . 6
8.3 Drying . 6
8.4 Test portion . 6
9 Procedure . 7
9.1 Cleaning of glassware . 7
9.2 Instrument performance parameters . 7
9.3 Instrument set-up . 7
9.4 Internal standard solution . 8
9.5 Sample preparation recovery solution . 8
9.6 Calibration blank solution . 8
9.7 Calibration solutions . 9
9.8 Sample preparation . 10
9.9 Test sample solutions . 11
9.10 Measurements . 11
10 Calculation and expression of results . 12
10.1 Calculation . 12
10.2 Repeatability . 13
10.3 Calculation to stochiometric content . 13
11 Quality assurance . 14
11.1 General . 14
11.2 Calibration curve. 14
12 Test report . 14
Annex A (informative) Results of interlaboratory test . 15
Bibliography . 17

© ISO #### 2026 – All rights reserved
iv
ISO/DISFDIS 12467-1:2026(en)
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent rights
in respect thereof. As of the date of publication of this document, ISO had not received notice of (a) patent(s)
which may be required to implement this document. However, implementers are cautioned that this may not
represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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 333, Lithium.
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.
© ISO 2026 – All rights reserved
v
ISO #####-#:####(X/FDIS 12467-1:2026(en)
Introduction
Lithium, its alloys and compounds are technologically important and highly versatile materials, and are used
in various industries, such as electronics, ceramics, glasses, medicine, etc.
Lithium is the lightest solid element, and due to the high electrochemical potential of the redox couple Li/Li+,
its main use is as cathode material in lithium ion batteries (LiBs) in electric vehicles, laptops, mobile phones
and digital cameras. Examples of commonly used lithium composite oxide cathode materials and their
principal constituents are shown in Table 1Table 1. Lithium materials are classified into different grades,
according to their chemical and physical characteristics, including purity, impurities, and particle size.
Therefore, the content of lithium materials are an important index to monitor product quality. The
determination of content by inductively coupled plasma optical emission spectrometry (ICP-OES) have
numerous advantages, such as simple sample-pre-treatment, high accuracy and low detection limit.
Table 1 — Types of Li composite oxides for LiBs
Acronym Chemical formula
LCO Li-xCoO
LMO Li-xMn2O4
NCA Li-xNiCoAlO
NMC Li-x(NixMnyCoz)O2
LFP Li-xFePO
LNO Li-xNiO2
LMP Li-xMnPO
LMFP Li-xMnFePO4
LTO Li-xTi O
5 12
OLO -
NOTE 1 For the purposes of this document, the term 'lithium composite oxides' includes lithium-containing cathode
materials such as layered oxides, spinel oxides and phosphate-based materials.
NOTE 2 New types of LiB can also be analysed by this method.
NOTE 3 The method is applicable for the other elements listed above, provided the user has verified the applicability.
This document specifies an analytical procedure for the determination of main components in Li composite
oxides for Li-ion batteries (LiB). The determination is applicable to all types of LiBs (see Table 1). The
determination is performed by optical emission spectrometry with inductively coupled plasma (ICP OES)
using an internal standard. The method of atomic emission spectrometry with inductively coupled plasma
(ICP AES) is interchangeable with ICP OES.
This test is recommended as the preferred method for determining the stoichiometric composition of several
elements in LiBs.
© ISO #### 2026 – All rights reserved
vi
DRAFT International Standard ISO/DIS 12467-1:2025(en)

Chemical analysis of lithium composite oxides – —
Part 1:
Determination of main components by inductively coupled plasma
optical emission spectrometry
WARNING — The use of this document can involve hazardous materials, operations, and equipment.
This document does not purport to address any safety problems associated with its use. It is the
responsibility of the user of this document to establish appropriate safety and health practices and
determine the applicability of regulatory limitations prior to use.
1 Scope
This document specifies an analytical procedure for the determination of main components in Li composite
oxides for Li-ion batteries (LiB), in particular the elements: lithium, cobalt, iron, manganese, nickel,
phosphorus, titanium and aluminium, depending on the composite oxide of interest.
The determination is applicable to all types of LiBs (Table 1).This document The determination is performed
by optical emission spectrometry with inductively coupled plasma (ICP OES) using an internal standard. The
method of atomic emission spectrometry with inductively coupled plasma (ICP AES) is interchangeable with
ICP OES.
This test is recommended as the preferred method for determining the stoichiometric composition of several
elements in LiBs. This standard establishes a test procedure for a high precision determination of
stoichiometric composition of the elements in LiBs.
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 1042, Laboratory glassware — One-mark volumetric flasks
ISO 7819, Lithium — Vocabulary
ISO 8656--1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme
ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 7819, Lithium — Vocabulary, and
the following apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
ISO #####-#:####(X/FDIS 12467-1:2026(en)
— — ISO Online browsing platform: available at https://www.iso.org/obp
— — IEC Electropedia: available at https://www.electropedia.org/
3.1 3.1
laboratory sample
sample as prepared for sending to the laboratory and intended for inspection or testing
[SOURCE: ISO 78-2:1999, 3.1]
3.2 3.2
test sample
sample prepared from the laboratory sample (3.1(3.1)) and from which test portions (3.3(3.3)) will be taken
[SOURCE: ISO 78-2:1999, 3.2]
3.3 3.3
test portion
quantity of material drawn from the test sample (3.2(3.2)) (or from the laboratory sample if both are the same)
and on which the test or observation is actually carried out
[SOURCE: ISO 78-2:1999, 3.3]
3.4 3.4
test sample solution
solution prepared after extraction or digestion of the test sample according to appropriate specifications
Note 1 to entry: A sample solution can be subjected to further operations, e.g., dilution and/or addition of an internal
standard, in order to produce a test solution that is ready for analysis.
[SOURCE: ISO 22036:2024, 3.10]
3.5 3.5
standard solution
solution of accurately known concentration of an element, an ion, a compound or a group derived from the
substance used for its preparation
[SOURCE: ISO 78-2:1999, 3.6]
3.6 3.6
stock solution
solution of accurately known analyte concentration(s), prepared from pure chemicals
3.7 3.7
calibration solution
solution used to calibrate the instrument, prepared from (a) stock solution(s) or from a certified standard
[SOURCE: ISO 17294-1:2024, 3.4]
3.8 3.8
calibration blank solution
solution prepared in the same way as the calibration solution (3.7(3.7)) but leaving out the analyte
[SOURCE: ISO 17294-1:2024, 3.3]
© ISO #### 2026 – All rights reserved
ISO/DISFDIS 12467-1:2026(en)
3.9 3.9
blank test solution
solution prepared by adding to the solvent the same amounts of reagents as those added to the test sample
solution and with the same final volume
[SOURCE: ISO 17294-1:2024, 3.19]
3.10 3.10
bracketing
analytical method consisting of bracketing the measured emission line intensity of the sample between two
measurements made on calibration solutions of neighbouring concentrations within the optimum working
range
Note 1 to entry: Running of standards and samples in the following sequence: low standard – sample – high standard –
sample – low standard – sample – high standard .
[SOURCE: ISO 19919:2025, 3.2]
3.11 3.11
calibration curve
expression of the relation between indication and corresponding measured quantity value
[SOURCE: ISO/IEC Guide 99:2007, 4.31]
3.12 3.12
calibration curve control
standard prepared independently of the calibration curve, the concentration of which is near the midpoint of
the calibration range
3.13 3.13
linearity
straight-line relationship between the mean result of measurement and the quantity (concentration) of the
analyte
4 Principle
The determination is carried out by means of the analytical technique of optical emission spectroscopy with
inductively coupled plasma (ICP-OES), which allows the detection and quantitative determination of most of
the elements from the periodic table from samples in solution.
In the ICP-OES technique, the continuous introduction of the liquid sample and a nebulization system forms
an aerosol that is transported by Argon to the plasma torch, inductively coupled by radio frequency. In the
plasma, due to the high temperatures generated, the analytes are atomized and ionized, generating the atomic
emission spectra of characteristic lines. The spectra are scattered by the diffraction grating and the light-
sensitive detector measures the spectral line intensities. The information is processed by the computer
software system of the ICP-OES equipment.
At least two accurately weighed samples are dissolved in a suitable acid mixture. After dissolution, this sample
solution is mixed with an exact mass of an internal standard solution and made up to the measurement final
volume. Using ICP-OES, the main contents of the sample solution are measured by comparing the intensities
of the spectral emissions of the main components and (a) suitable internal standard line(s) with the intensities
of a solution where the contained mass of these elements and internal standard is precisely known. The
bracketing method is used for this purpose.
© ISO 2026 – All rights reserved
ISO #####-#:####(X/FDIS 12467-1:2026(en)
5 Reagents and solutions
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade.
WARNING — Concentrated mineral acids (5.2, 5.3, 5.4, 5.5, 5.6, 5.7(5.2, 5.3, 5.4, 5.5, 5.6, 5.7)) are
corrosive and acid vapour is an irritant. Avoid contact with the skin or eyes, or inhalation of the
vapour. Use suitable personal protective equipment (e.g., gloves, face shield or safety goggles, etc.)
when working with concentrated or dilute acid. Handle open vessels containing concentrated acid in
a fume hood. Do not add water to acid, as the reaction is violent. Small aliquots of acid shall be added
slowly to larger volumes of water. The vapour pressure of acid is high; therefore beware of pressure
build-up in stoppered flasks when preparing acid/water mixtures.
5.1 5.1 Water (H O), (see ISO 3696), grade 1.
®11)
5.2 5.2 Hydrochloric acid (HCl), (CAS RN 7647-01-0), 30 % to 37 % HCl (mass fraction).
5.3 5.3 Nitric acid (HNO ), (CAS RN 7697-37-2), 65 % minimum HNO (mass fraction).
3 3
5.4 5.4 Perchloric acid (HClO ), (CAS RN 7601-90-3), 70 % to 73 % HClO (mass fraction).
4 4
5.5 5.5 Sulfuric acid (H SO ), (CAS RN 7664-93-9), 95 % minimum H SO (mass fraction).
2 4 2 4
5.6 5.6 Hydrofluoric acid (HF), (CAS RN 7664-39-3), 40 % to 42 % HF (mass fraction).
WARNING — Concentrated hydrofluoric acid is very toxic in contact with the skin and if inhaled or
swallowed. It is corrosive and causes severe burns. Take extreme care when using hydrofluoric acid.
Avoid contact with the skin or eyes, or inhalation of the vapour. It is essential that suitable personal
protective equipment (including suitable gloves, face shield, etc.) is used when working with
concentrated or dilute hydrofluoric acid. Handle open vessels containing concentrated hydrofluoric
acid in a fume hood. Ensure that the nature and seriousness of hydrofluoric acid burns is understood
before commencing work with this substance. Carry hydrofluoric acid burn cream (containing calcium
gluconate) at all times whilst working with hydrofluoric acid and for 24 h afterwards. Apply the cream
to any contaminated skin, after washing the affected area with copious amounts of water. Obtain
medical advice immediately in case of an accident.
NOTE The burning sensation associated with many concentrated acid burns is not immediately apparent on
exposure to hydrofluoric acid and will possibly not be felt for several hours. Relatively dilute solutions of hydrofluoric
acid can also be absorbed through the skin, with serious effects similar to those resulting from exposure to the
concentrated acid.
When using hydrofluoric acid, it is recommended that a pair of disposable gloves be worn underneath suitable
acid-resistant gloves to provide added protection for the hands.
5.7 5.7 Aqua regia (should be prepared just before use).
Mix three volumes of hydrochloric acid (5.2(5.2)) and one volume of nitric acid (5.3(5.3).).
5.8 5.8 Single element standard stock solutions, 1 000 or 10 000 mg/L

CAS Registry Number® is a trademark of the American Chemical Society (ACS). This information is given for the
convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent
products may be used if they can be shown to lead to the same results.
1)
CAS Registry Number® is a trademark of the American Chemical Society (ACS). This information is given for the
convenience of users of this document and does not constitute an endorsement by ISO of the product named. Equivalent
products may be used if they can be shown to lead to the same results.

© ISO #### 2026 – All rights reserved
ISO/DISFDIS 12467-1:2026(en)
where c(element) is the concentration of the element.
Al, Co, Fe, Li, Mn, Ni, P, Ti; c = 1 000 or 10 000 mg/L each.
(element)
For internal standard the following elements can be used :
Be, Cd, Ge, In, Ru, Sc, Y; c = 1 000 or 10 000 mg/L each.
(element)
Single element standard stock solutions with adequate specification stating the acid used and the preparation
technique are commercially available. Single-element standard stock solutions can be made from high purity
metals or salts or oxides.
For stability of the solutions, refer to the manufacturer guarantee statement.
5.9 5.9 Argon gas (CAS RN 7440-37-1), purity ≥ 99,995 % (mass fraction)).
6 Apparatus
All apparatus shall be carefully cleaned prior to use.
6.1 6.1 Inductively coupled argon plasma optical emission spectrometer
The ICP optical emission spectrometer consists of a sample introduction system, the plasma (an excitation or
emission source), a plasma torch, an optical system, a detector and a computer. The sample introduction
system usually consists of a peristaltic pump for sample transport to the nebulizer, the nebulizer and a spray
chamber. The most common nebulizers are the concentric nebulizer, the cross-flow nebulizer and the V-
groove nebulizer. They are made from glass, quartz, polytetrafluoroethylene (PTFE), fluorinated ethylene
propylene (FEP), perfluoroalkoxy (PFA), ceramic or other acid-resistant polymer materials. For higher salt
tolerance, it is recommended to use an argon humidifier.
In addition, many types of spray chambers are applied in commercial systems. The most common, beside the
cyclonic type with a baffle, is the Scott type where double concentric tubes separate larger droplets from the
fine aerosol which is introduced into the plasma torch.
The plasma torch consists of three concentric tubes (Fassel type). Quartz is the most commonly used material.
The injector tube can be made of HF-acid resistant material, e.g., aluminum oxide, sapphire or platinum. The
plasma gas flow and the auxiliary gas flow rates depend on the type of construction and are typically around
12 L/min to 20 L/min and 0 L/min to 3 L/min, respectively. All gas flows shall be controlled by a flow
controller.
A radio frequency (RF) oscillator is placed at the end of the torch, through which a high alternating current
flows to excite the plasma. The typical frequency used is 27 MHz to 40 MHz with a power of 600 W to 2 000 W.
The emission from the plasma can be observed either from the side (radial view), both sides (dual radial view),
or from the torch central symmetrical axis (axial view). For highest precision, the radial view is recommended.
The analyte and internal standard wavelength have to be measured and registered in a simultaneous manner
with a minimum optical resolution of 0,02 nm.
NOTE 1 The compu
...