prEN ISO 21813
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of high purity barium titanate powders (ISO/DIS 21813:2026)
- Abstract
ISO 21813 specifies methods for the chemical analysis of fine high purity barium titanate powders used as the raw material for fine ceramics.
ISO 21813 stipulates the determination methods of the barium, titanium, aluminium, cadmium, calcium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, sodium, strontium, vanadium, zirconium, carbon, oxygen and nitrogen contents in high purity barium titanate powders. The barium and titanium contents, the major elements, are determined by using an acid decomposition-gravimetric method or an acid decomposition-inductively coupled plasma-optical emission spectrometry (ICP-OES) method. The aluminium, cadmium, calcium, chromium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, strontium, vanadium and zirconium contents are simultaneously determined via an acid digestion-ICP-OES method. The nitrogen content is determined by using an inert gas fusion-thermal conductivity method, while that of oxygen is determined via an inert gas fusion-IR absorption spectrometry method. Finally, the carbon content is determined using a combustion-IR absorption spectrometry method or a combustion-conductometry method.
- Status
- Not Published
- Publication Date
- 11-Jan-2028
- Technical Committee
- CEN/TC 184 - Advanced technical ceramics
- Drafting Committee
- CEN/TC 184 - Advanced technical ceramics
- Current Stage
- 4020 - Submission to enquiry - Enquiry
- Start Date
- 23-Jul-2026
- Completion Date
- 23-Jul-2026
prEN ISO 21813 is a draft standard for the chemical analysis of high purity barium titanate powders used as raw material for fine ceramics. It specifies how to determine barium, titanium, selected trace elements, oxygen and carbon, and it gives the sample preparation, calculation and reporting rules needed for laboratory analysis.
What does prEN ISO 21813 specify?
prEN ISO 21813 specifies methods for chemical analysis of fine, high purity barium titanate powders used for fine ceramics. In practice, it tells a laboratory which analytes to measure, which analytical route to use for each group of elements, and how to prepare and report results.
The document is organized into scope, normative references, sample preparation, reporting rules, determination of Ba and Ti, determination of trace elements, oxygen, carbon, the test report, and an informative annex with round-robin results. That structure matters because the user can move from sampling to measurement to reporting without needing another method document.
| Annex | What it covers |
|---|---|
| Annex A | Informative analytical results from a round-robin test |
What are the key requirements of prEN ISO 21813?
Sample preparation and reporting
prEN ISO 21813 requires the test sample to be prepared in accordance with ISO 8656-1 unless the analyser and customer agree otherwise. The sample is dried at the stated temperature and time, then weighed to the nearest 0,1 mg. That matters because moisture and poor sampling can shift the reported mass fractions.
Clause 6 requires duplicate analyses on different days and a blank value for each method. If the two results fall within the tolerance table, the average is reported; if not, two more analyses are made and the average or median rule is applied. In practice, the standard is controlling repeatability before a result is released.
Results are reported on a dry basis as mass fraction in percent. Ba, Ti and O are reported to two decimal places, while the other analytes are reported to three decimal places. That keeps the output format consistent for certificates and internal quality records.
Barium and titanium determination
Clause 7 gives two ways to determine the major elements barium and titanium: an acid decomposition-gravimetric method and an acid decomposition-ICP-OES method. The gravimetric route is the choice when four significant figures are needed; the ICP-OES route is used when two or three significant figures are sufficient. This lets a laboratory match the method to the required data quality.
In the gravimetric method, the sample is decomposed with hydrogen peroxide and hydrochloric acid, barium is precipitated and weighed as barium sulfate, and titanium is recovered and weighed as titanium oxide. The practical consequence is that the lab needs classical wet chemistry equipment and careful handling of precipitates and ignition steps.
In the ICP-OES method, the decomposed solution is measured by inductively coupled plasma-optical emission spectrometry at selected emission lines. The method includes calibration solutions, background correction, and blank correction. That matters because instrument calibration and matrix correction drive the reliability of the reported Ba and Ti values.
Trace element determination
Clause 8 uses ICP-OES for the trace elements after acid digestion with hydrochloric acid and hydrogen peroxide. The document gives a mixed standard solution, calibration steps, a blank measurement, and recommended emission lines. For routine work, this section is the main route for impurity control in the powder.
The trace-element section is intended to cover the listed minor constituents at low mass fractions, and the wavelength table helps the operator choose a line with fewer spectral interferences. In practice, the analyst must select emission lines that fit the instrument and the sample matrix, then confirm that the chosen line is clean enough for the result to be trusted.
Oxygen determination
Clause 9 determines total oxygen by inert gas fusion. The sample is fused in a graphite crucible under helium, oxygen from the sample is converted to carbon monoxide and then measured after conversion to carbon dioxide, or directly by IR spectrometry. This is important because oxygen content is a key parameter in high purity ceramic powders.
The oxygen method uses a calibration sample such as yttrium oxide or a nitride reference material, a blank value based on repeated blank runs, and a calibration coefficient calculated from the measured integral value. In practice, the laboratory needs a dedicated oxygen analyser and a stable calibration routine to keep the oxygen result traceable.
Carbon determination
Clause 10 gives three combustion methods for total carbon: resistance furnace-IR absorption spectrometry, radio frequency heating furnace-thermal conductometry, and radio frequency heating furnace-IR absorption spectrometry. All three use combustion under oxygen with accelerators, blank measurements, calibration with calcium carbonate or a nitride, and a calculated calibration coefficient. That makes the method suitable for laboratories with different analyser designs.
For routine use, the important point is that the standard allows either IR detection or thermal conductometry, depending on the instrument available. The sample mass, accelerator choice and measurement path must match the method variant, so the lab needs to follow the selected procedure consistently.
Test report
Clause 11 requires the report to identify the sample, laboratory and date, state the method used by reference to the standard, give the results and their expression, and record any deviations or unusual observations. This is what makes the measurement usable in quality control, supplier verification and dispute resolution.
What terms does prEN ISO 21813 define?
Inductively coupled plasma-optical emission spectrometry (ICP-OES) is the elemental analysis technique used here to measure emissions from a plasma after the sample has been digested.
Infrared (IR) absorption spectrometry measures a gas by its absorption of infrared light, and the document uses it for oxygen and some carbon measurement routes.
Blank value is the result obtained without a sample and is used to correct the analytical result for each method.
Calibration coefficient links the measured instrument signal to the amount of oxygen or carbon determined from the calibration sample.
Mass fraction is the concentration expression used throughout the document, reported as percent on a dry basis.
Round-robin test is the interlaboratory study mentioned in Annex A and used to show how the method performed across several laboratories.
Who uses prEN ISO 21813?
prEN ISO 21813 is used by analytical laboratories that test fine ceramics raw materials, especially high purity barium titanate powders. It is relevant to quality managers, process laboratories, and suppliers that need to verify composition before the powder is used in ceramic production.
It also serves buyers and specification writers who need a shared method for comparing supplier data. In practice, it helps teams decide whether a powder meets the required composition and impurity profile before release or acceptance.
Which standards are used with prEN ISO 21813?
prEN ISO 21813 refers to ISO 3696 for laboratory water quality. That supports the preparation of solutions and reduces contamination risk.
It refers to ISO 6353-1, ISO 6353-2 and ISO 6353-3 for reagents used in the chemical methods. These references matter because the analytical procedures depend on reagent grade and reagent specifications.
It refers to ISO 8656-1 for sampling raw materials and unshaped products. That provides the sampling basis for taking the test portion used in the analysis.
What does the prEN ISO 21813 document contain?
The document contains detailed analytical procedures rather than general guidance. It includes sample drying and weighing steps, blank determination, calibration procedures, calculation formulas, and reporting rules for each analytical route.
It also contains a tolerance table for deciding whether repeated results can be averaged, and a wavelength table for ICP-OES line selection. These tables are practical tools for the analyst because they control result acceptance and instrument setup.
For oxygen and carbon, the document describes the analyser blocks, gas flow and detection concepts, and the steps for calibration and measurement. Annex A then gives informative round-robin results that show how the methods performed in interlaboratory testing.
Relations
- Effective Date
- 05-Oct-2024
Frequently Asked Questions
prEN ISO 21813 is a draft published by the European Committee for Standardization (CEN). Its full title is "Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of high purity barium titanate powders (ISO/DIS 21813:2026)". This standard covers: ISO 21813 specifies methods for the chemical analysis of fine high purity barium titanate powders used as the raw material for fine ceramics. ISO 21813 stipulates the determination methods of the barium, titanium, aluminium, cadmium, calcium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, sodium, strontium, vanadium, zirconium, carbon, oxygen and nitrogen contents in high purity barium titanate powders. The barium and titanium contents, the major elements, are determined by using an acid decomposition-gravimetric method or an acid decomposition-inductively coupled plasma-optical emission spectrometry (ICP-OES) method. The aluminium, cadmium, calcium, chromium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, strontium, vanadium and zirconium contents are simultaneously determined via an acid digestion-ICP-OES method. The nitrogen content is determined by using an inert gas fusion-thermal conductivity method, while that of oxygen is determined via an inert gas fusion-IR absorption spectrometry method. Finally, the carbon content is determined using a combustion-IR absorption spectrometry method or a combustion-conductometry method.
ISO 21813 specifies methods for the chemical analysis of fine high purity barium titanate powders used as the raw material for fine ceramics. ISO 21813 stipulates the determination methods of the barium, titanium, aluminium, cadmium, calcium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, sodium, strontium, vanadium, zirconium, carbon, oxygen and nitrogen contents in high purity barium titanate powders. The barium and titanium contents, the major elements, are determined by using an acid decomposition-gravimetric method or an acid decomposition-inductively coupled plasma-optical emission spectrometry (ICP-OES) method. The aluminium, cadmium, calcium, chromium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, strontium, vanadium and zirconium contents are simultaneously determined via an acid digestion-ICP-OES method. The nitrogen content is determined by using an inert gas fusion-thermal conductivity method, while that of oxygen is determined via an inert gas fusion-IR absorption spectrometry method. Finally, the carbon content is determined using a combustion-IR absorption spectrometry method or a combustion-conductometry method.
prEN ISO 21813 is classified under the following ICS (International Classification for Standards) categories: 81.060.30 - Advanced ceramics. The ICS classification helps identify the subject area and facilitates finding related standards.
prEN ISO 21813 has the following relationships with other standards: It is inter standard links to EN ISO 21813:2022. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
prEN ISO 21813 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
SLOVENSKI STANDARD
01-oktober-2026
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za
kemijsko analizo praškov barijevega titanata visoke čistosti (ISO/DIS 21813:2026)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for
chemical analysis of high purity barium titanate powders (ISO/DIS 21813:2026)
Hochleistungskeramik - Verfahren zur chemischen Analyse von hochreinen
Bariumtitanatpulvern (ISO/DIS 21813:2026)
Céramiques techniques (céramiques techniques avancées) - Méthodes d’analyse
chimique des poudres de titanate de baryum de haute pureté (ISO/DIS 21813:2026)
Ta slovenski standard je istoveten z: prEN ISO 21813
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
DRAFT
International
Standard
ISO/DIS 21813
ISO/TC 206
Fine ceramics (advanced ceramics,
Secretariat: JISC
advanced technical ceramics) —
Voting begins on:
Methods for chemical analysis
2026-07-20
of high purity barium titanate
Voting terminates on:
powders
2026-10-12
Céramiques techniques (céramiques techniques avancées) —
Méthodes d’analyse chimique des poudres de titanate de baryum
de haute pureté
ICS: 81.060.30
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document has not been edited by the ISO Central Secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
ISO/CEN PARALLEL PROCESSING
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS.
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 SUPPORTING DOCUMENTATION.
Reference number
ISO/DIS 21813:2026(en)
DRAFT
ISO/DIS 21813:2026(en)
International
Standard
ISO/DIS 21813
ISO/TC 206
Fine ceramics (advanced ceramics,
Secretariat: JISC
advanced technical ceramics) —
Voting begins on:
Methods for chemical analysis
of high purity barium titanate
Voting terminates on:
powders
Céramiques techniques (céramiques techniques avancées) —
Méthodes d’analyse chimique des poudres de titanate de baryum
de haute pureté
ICS: 81.060.30
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENTS AND APPROVAL. IT
IS THEREFORE SUBJECT TO CHANGE
AND MAY NOT BE REFERRED TO AS AN
INTERNATIONAL STANDARD UNTIL
PUBLISHED AS SUCH.
This document has not been edited by the ISO Central Secretariat.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
© ISO 2026
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
STANDARDS MAY ON OCCASION HAVE TO
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BE CONSIDERED IN THE LIGHT OF THEIR
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TO SUBMIT, WITH THEIR COMMENTS,
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NOTIFICATION OF ANY RELEVANT PATENT
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Website: www.iso.org
Published in Switzerland Reference number
ISO/DIS 21813:2026(en)
ii
ISO/DIS 21813:2026(en)
Contents Page
Foreword .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Analytes and ranges . 1
5 Preparation of test sample . 2
5.1 General .2
5.2 Sampling .2
5.3 Drying .2
5.4 Weighing .2
6 Reporting the analytical values . . 3
6.1 Number of analyses .3
6.2 Blank value .3
6.3 Evaluation of the analytical values .3
6.4 Expression of the analytical values .3
7 Determination of the barium and titanium contents . 3
7.1 Classification of the determination methods .3
7.2 Acid decomposition-gravimetric method .4
7.2.1 Principle .4
7.2.2 Reagents .4
7.2.3 Apparatus .4
7.2.4 Procedure .5
7.2.5 Blank solution .5
7.2.6 Calculation .6
7.3 Acid decomposition-ICP-OES method .6
7.3.1 Principle .6
7.3.2 Reagents .6
7.3.3 Apparatus .6
7.3.4 Procedure .7
7.3.5 Blank solution .7
7.3.6 Calibration . . .7
7.3.7 Calculation .7
8 Determination of the trace element contents . 8
8.1 Principle .8
8.2 Reagents .8
8.3 Apparatus .8
8.4 Procedure .8
8.5 Blank solution .9
8.6 Calibration .9
8.7 Calculation .10
9 Determination of the total oxygen content. 10
9.1 Principle .10
9.2 Reagents .10
9.3 Apparatus .10
9.4 Instrument .10
9.5 Procedure .11
9.6 Blank value .11
9.7 Calculation of the calibration coefficient . 12
9.8 Calculation . 12
10 Determination of the total carbon content .12
10.1 Classification of the determination methods . 12
iii
ISO/DIS 21813:2026(en)
10.2 Combustion (resistance furnace)-IR absorption spectrometry . 12
10.2.1 Principle . 12
10.2.2 Reagents . 13
10.2.3 Apparatus . 13
10.2.4 Instrument . 13
10.2.5 Procedure .14
10.2.6 Blank value .14
10.2.7 Calculation of the calibration coefficient .14
10.2.8 Calculation . 15
10.3 Combustion (radio frequency heating furnace)-thermal conductometry . 15
10.3.1 Principle . 15
10.3.2 Reagents . 15
10.3.3 Apparatus . 15
10.3.4 Instrument .16
10.3.5 Procedure .16
10.3.6 Blank value .17
10.3.7 Calculation of the calibration coefficient .17
10.3.8 Calculation .17
10.4 Combustion (radio frequency heating furnace)-IR absorption spectrometry .17
10.4.1 Principle .17
10.4.2 Reagents .17
10.4.3 Apparatus .17
10.4.4 Instrument .17
10.4.5 Procedure .18
10.4.6 Blank value .19
10.4.7 Calculation of the calibration coefficient .19
10.4.8 Calculation .19
11 Test report . 19
Annex A (informative) Analytical results obtained from the round-robin test.20
Bibliography .22
iv
ISO/DIS 21813:2026(en)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
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[1]
This document, which is based on, was prepared by Technical Committee ISO/TC 206, Fine ceramics.
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.
v
DRAFT International Standard ISO/DIS 21813:2026(en)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of high purity
barium titanate powders
1 Scope
This document specifies methods for the chemical analysis of fine high purity barium titanate powders used
as the raw material for fine ceramics.
This document stipulates the determination methods of the barium, titanium, aluminium, cadmium,
calcium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel, niobium, potassium, silicon, sodium,
strontium, vanadium, zirconium, carbon and oxygen contents in high purity barium titanate powders.
The barium and titanium contents, the major elements, are determined by using an acid decomposition-
gravimetric method or an acid decomposition-inductively coupled plasma-optical emission spectrometry
(ICP-OES) method. The aluminium, cadmium, calcium, chromium, cobalt, dysprosium, iron, lead, magnesium,
manganese, nickel, potassium, silicon, strontium, vanadium and zinc contents are simultaneously
determined via an acid digestion-ICP-OES method. The oxygen content is determined via an inert gas fusion-
IR absorption spectrometry method. Finally, the carbon content is determined using a combustion-IR
absorption spectrometry method or a combustion-thermal conductometry method.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 6353-1, Reagents for chemical analysis — Part 1: General test methods
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
ISO 6353-3, Reagents for chemical analysis — Part 3: Specifications — Second series
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme
3 Terms and definitions
No terms and definitions are listed in this document.
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 https:// www .electropedia .org/
4 Analytes and ranges
a) Barium (Ba), range of 40 % to 60 % (mass fraction).
b) Titanium (Ti), range of 10 % to 30 % (mass fraction).
ISO/DIS 21813:2026(en)
c) Aluminium (Al), range of 0,001 % to 0,03 % (mass fraction).
d) Cadmium (Cd), range of 0,001 % to 0,03 % (mass fraction).
e) Calcium (Ca), range of 0,001 % to 0,03 % (mass fraction).
f) Cobalt (Co), range of 0,001 % to 0,03 % (mass fraction).
g) Dysprosium (Dy), range of 0,001 % to 0,03 % (mass fraction).
h) Iron (Fe), range of 0,001 % to 0,03 % (mass fraction).
i) Lead (Pb), range of 0,001 % to 0,03 % (mass fraction).
j) Magnesium (Mg), range of 0,001 % to 0,03 % (mass fraction).
k) Manganese (Mn), range of 0,001 % to 0,03 % (mass fraction).
l) Nickel (Ni), range of 0,001 % to 0,03 % (mass fraction).
m) Potassium (K), range of 0,001 % to 0,03 % (mass fraction).
n) Silicon (Si), range of 0,001 % to 0,03 % (mass fraction).
o) Sodium (Na), range of 0,001 % to 0,03 % (mass fraction).
p) Strontium (Sr), range of 0,001 % to 0,03 % (mass fraction).
q) Vanadium (V), range of 0,001 % to 0,03 % (mass fraction).
r) Zinc (Zn), range of 0,001 % to 0,03 % (mass fraction).
s) Oxygen (O), range of 10 % to 30 % (mass fraction).
t) Carbon (C), range of 0,01 % to 5 % (mass fraction).
5 Preparation of test sample
5.1 General
The sample preparation method shall be in accordance with ISO 8656-1, unless otherwise mutually agreed
upon by the analyser and customer.
5.2 Sampling
The sample shall be collected in accordance with ISO 8656-1.
5.3 Drying
Place a 10 g sample into a flat-type weighing bottle (60 mm × 30 mm) and spread it uniformly over the
bottom of the bottle. Place the bottle in a drying oven at 110 °C ± 5 °C for 2 h, uncovered, and cool in a
desiccator (desiccant: dried silica gel), covered, for 1 h.
5.4 Weighing
Weigh the sample to the nearest 0,1 mg using a balance.
ISO/DIS 21813:2026(en)
6 Reporting the analytical values
6.1 Number of analyses
Analyse the sample twice on different days.
6.2 Blank value
Determine the blank value for each analysis method described in this standard in order to correct the values
measured for the samples.
6.3 Evaluation of the analytical values
When the difference between the two analytical values does not exceed the tolerance value (Table 1),
the average value shall be reported. When the difference between the two analytical values exceeds the
tolerance value, perform two additional analyses. When the difference in these further two analyses does
not exceed the tolerance value, the average value thereof shall be reported. If the difference also exceeds the
tolerance value, the median of four analytical values shall be reported.
6.4 Expression of the analytical values
The analytical values shall be given in % (mass fraction), on a dry basis.
a) Barium, titanium and oxygen: express the results to two decimal places.
b) Others: express the results to three decimal places.
Table 1 — Tolerances for the analytical values
Units: % (mass fraction)
Al, Cd, Ca, Co, Dy, Fe, Pb, Mg, Mn, Ni,
Element Ba Ti O C
K, Si, Na, Sr, V, Zn
a a c
0,30 0,20 0,001
Tolerance 0,50 0,005
b b d
0,40 0,30 0,005
a
Acid decomposition-gravimetric method.
b
Acid decomposition-ICP-OES method.
c
Applicable to content of less than 0,01 % (mass fraction).
d
Applicable to content of not less than 0,01 % (mass fraction).
7 Determination of the barium and titanium contents
7.1 Classification of the determination methods
The barium and titanium contents shall be determined by either of the following methods:
— Method A, acid decomposition-gravimetric method;
— Method B, acid decomposition-ICP-OES method.
If analytical results with four significant figures are required, use method A; if two or three significant
figures are required, method B can be used.
ISO/DIS 21813:2026(en)
7.2 Acid decomposition-gravimetric method
7.2.1 Principle
A portion of the sample is decomposed using hydrogen peroxide and hydrochloric acid. The barium present
in the test solution is analysed by gravimetric analysis using sulfuric acid. The titanium in the test solution
is analysed by gravimetric analysis using ammonia solution.
7.2.2 Reagents
During the analysis, unless otherwise stated, only reagents of recognized analytical grade and only distilled
water or water of equivalent purity shall be used.
Reagents shall conform to the requirements of ISO 6353-1, ISO 6353-2 and ISO 6353-3 as appropriate.
Specific requirements for the reagents are given in the appropriate clause.
7.2.2.1 Ammonia water (NH ), (ISO 6353-2, R 3), 25 % (mass fraction).
7.2.2.2 Hydrogen peroxide (H O ), (ISO 6353-2, R 14), 30 % (mass fraction).
2 2
7.2.2.3 Hydrochloric acid (HCl), (ISO 6353-2, R 13), 35 % (mass fraction).
7.2.2.4 Sulfuric acid (H SO ), (ISO 6353-2, R 37), 95 % (mass fraction).
2 4
7.2.2.5 Hydrogen peroxide (1+10).
7.2.2.6 Hydrochloric acid (1+10).
7.2.2.7 Sulfuric acid (1+1).
7.2.2.8 Water, grade 1 or superior as specified in ISO 3696.
7.2.3 Apparatus
Ordinary laboratory apparatus together with the following:
7.2.3.1 PTFE beaker, 250 ml.
7.2.3.2 Burette, with a 0,1 ml scale and a maximum volume of 50 ml.
7.2.3.3 PTFE pipette, suitable for the transfer of each sample or standard solution.
7.2.3.4 Desiccator, containing dried silica gel as the drying agent.
7.2.3.5 Balance, capable of weighing to ±0,1 mg.
7.2.3.6 Electric furnace, for operation at (1 000 ± 50) °C.
7.2.3.7 Platinum crucible (30 ml).
7.2.3.8 PTFE beaker cover.
7.2.3.9 Volumetric flask (100 ml, 500 ml).
ISO/DIS 21813:2026(en)
7.2.3.10 Hot plate, with magnetic stirrer and magnetic bar.
7.2.4 Procedure
7.2.4.1 Weigh 0,30 g of the test sample and transfer it into a 250 ml PTFE beaker (7.2.3.1). Place the
magnetic bar in the PTFE beaker containing the test sample and carefully add 20 ml water, 10 ml hydrogen
peroxide (7.2.2.2) and 20 ml hydrochloric acid (7.2.2.3) to the beaker. Cover the beaker with a PTFE beaker
cover (7.2.3.8) and heat and stir the contents at (85 ± 5) °C using the hot plate (7.2.3.10) until the test sample
is completely dissolved. After cooling, transfer the solution to a 100 ml volumetric flask, dilute with water to
the mark and mix well.
The highly pure fine barium titanate powder sample completely decomposes in hydrochloric acid and
hydrogen peroxide. However, the presence of impurities or coarse grains in the sample may hinder the
decomposition process. If the sample is not completely decomposed by the acid decomposition method,
it is recommended that other decomposition methods are applied. These include the acid pressure
decomposition, fusion or acid microwave dissolution methods.
7.2.4.2 Transfer a 50 ml aliquot of the test solution (7.2.4.1) to a 250 ml PTFE beaker (7.2.3.1) and add
10 ml sulfuric acid (1+1) (7.2.2.7). After covering the beaker with a PTFE beaker cover (7.2.3.8), heat and stir
the contents at 200 °C for 1 h using the hot plate (7.2.3.10).
7.2.4.3 Filter the solution with ashless filter paper and wash the precipitate several times with hot water.
Keep the filtrate and washings in the beaker covered with the watch glass for the determination of the
titanium content.
7.2.4.4 Transfer the precipitate and the filter paper to a 30 ml platinum crucible. Heat the crucible in an
electric furnace at low temperature until the filter paper has been completely burned to ashes. Heat the
crucible and its contents in an electric furnace (1 000 ± 50) °C for 1 h. After cooling in a desiccator, weigh the
barium sulfate.
7.2.4.5 Add 50 ml ammonia water (7.2.2.1) to the filtrate (7.2.4.3). Filter the solution with ashless filter
paper and wash over the precipitate several times with hot water. Transfer the precipitate with filter paper
to a 30 ml platinum crucible. Heat the sample in an electric furnace at low temperature until ashing of the
filter paper is complete. Next, heat the crucible and its contents in an electric furnace at (1 000 ± 50) °C for
1 h. After cooling in a desiccator, weigh the titanium oxide.
7.2.5 Blank solution
Carry out the procedure described in 7.2.4 without the sample. Designate the final solution as the blank
solution.
ISO/DIS 21813:2026(en)
7.2.6 Calculation
Calculate the mass fractions of barium and titanium in the sample according to Formula (1).
100 mm VF
21 1
w (1)
mV
where
w is the mass fraction of barium or titanium in the sample, in percent;
m is the mass of the empty platinum crucible, in grams;
m is the mass of the platinum crucible after ignition (7.2.4.4 or 7.2.4.5), in grams;
m is the sample mass, in grams;
V is the volume of the sample solution (7.2.4.1), in millilitres;
V is the volume of the aliquot of the sample solution (7.2.4.2), in millilitres;
F is the element to compound mass ratio: 0,588 4 for barium in barium sulphate and 0,599 3 for
titanium in titanium dioxide.
7.3 Acid decomposition-ICP-OES method
7.3.1 Principle
A portion of the sample is decomposed in concentrated hydrogen peroxide and hydrochloric acid. The
barium and titanium present in the test solution are analysed by ICP-OES at selected emission lines.
7.3.2 Reagents
Use the reagents described in 7.2.2 together with the following:
7.3.2.1 Barium standard solution (Ba 10 mg/ml).
The SI traceable commercial standard solution is available.
7.3.2.2 Barium standard solution (Ba 1 mg/ml).
Transfer 10 ml barium standard solution (7.3.2.1) to a 100 ml volumetric flask, dilute with water to the mark
and mix well.
7.3.2.3 Titanium standard solution (Ti 10 mg/ml).
The SI traceable commercial standard solution is available.
7.3.2.4 Titanium standard solution (Ti 1 mg/ml).
Transfer 10 ml titanium standard solution (7.3.2.3) to a 100 ml volumetric flask, dilute with water to the
mark and mix well.
7.3.3 Apparatus
Use the apparatus described in 7.2.3 together with the following:
7.3.3.1 ICP-OES, consisting of a sample introduction system (pump, nebulizer, spray chamber), inductively
coupled plasma as excitation source, optical system, detector and computer with software for device control,
data acquisition and data evaluation.
ISO/DIS 21813:2026(en)
7.3.4 Procedure
7.3.4.1 Carry out the procedures described in 7.2.4.1.
7.3.4.2 After cooling, transfer a 10 ml aliquot of the solution into a 500 ml volumetric flask, dilute with
water to the mark and mix well. This solution is used as the test solution.
7.3.4.3 Spray a portion of the test solution into the argon plasma flame of the ICP-OES, then measure the
emission intensity for barium at 455,40 nm, 493,40 nm and 233,52 nm, and that for titanium at 334,94 nm,
336,12 nm and 337,27 nm. The measurements should be carried out using background correction.
NOTE To improve trueness and precision of the measurements the method of internal standard can be applied.
For this purpose, the ratio of intensities of the emission lines of analyte elements to the intensity of the emission line
of a reference element added to the test solutions is used to compensate for matrix effects and changed excitation
conditions in the plasma. The method of internal standard was not used by any of the laboratories participating in the
round-robin test (see Annex A).
7.3.5 Blank solution
Perform the operation described in 7.3.4 without using a sample. Designate the final solution as the blank
solution.
7.3.6 Calibration
Transfer 0 ml, 1 ml, 2 ml, 3 ml, 4 ml and 5 ml aliquots of the barium standard solution (7.3.2.2) and 0 ml,
0,5 ml, 1 ml, 1,5 ml, 2 ml and 2,5 ml of the titanium standard solution (7.3.2.4) to six separate 100 ml
volumetric flasks. To each flask, add 5 ml hydrochloric acid (1+10). Dilute with water to the mark and mix
well. The calibration functions are created by measurement of these six calibration solutions as described in
7.3.4.3. The measurements should be carried out using background correction.
NOTE 1 Based on practical experience, using less than six points for the calibration function usually has no impact
on the precision of the determination. It is recommended to use at least three points for the calibration function
including the zero point, for example, calibration solutions with a concentration of 0 mg/L, 25 mg/L and 50 mg/L for
barium and 0 mg/L, 12 mg/L and 25 mg/L for titanium.
NOTE 2 The calculation of the calibration functions is usually carried out as linear regression.
7.3.7 Calculation
Determine the barium and titanium concentrations in the test solution and blank solution from the
calibration function. Calculate the mass fraction of barium or titanium in the sample, w, according to
Formula (2).
CC VV
TB TS
w (2)
10000Vm
A
where
w is the mass fraction of barium or titanium in the sample, in percent;
C is the measured barium or titanium concentration in the test solution (7.3.4.2), in milligrams
T
per litre;
C is the measured barium or titanium concentration in the blank test solution (7.3.5), in milligrams
B
per litre;
V is the volume of the test solution (7.3.4.2), in millilitres;
T
V is the volume of the sample solution (7.2.4.1), in millilitres;
S
V is the volume of the aliquot of the sample solution (7.2.4.1) used for preparation of the test
A
solution (7.3.4.2), in millilitres;
m is the mass of the test portion, in grams.
ISO/DIS 21813:2026(en)
8 Determination of the trace element contents
8.1 Principle
To prepare the test solution, the sample is decomposed in hydrochloric acid and hydrogen peroxide.
Aluminium, cadmium, calcium, chromium, cobalt, dysprosium, iron, lead, magnesium, manganese, nickel,
niobium, potassium, silicon, strontium, vanadium and zirconium are determined by ICP-OES at selected
emission lines.
8.2 Reagents
Use the reagents described in 7.2.2 together with the following:
8.2.1 Element standard solutions.
The SI traceable commercial standard solution is available for each of the following elements.
— aluminium standard solution (Al, 1 mg/ml);
— cadmium standard solution (Cd, 1 mg/ml);
— calcium standard solution (Ca, 1 mg/ml);
— cobalt standard solution (Co, 1 mg/ml);
— dysprosium standard solution (Dy, 1 mg/ml);
— iron standard solution (Fe, 1 mg /ml);
— lead standard solution (Pb, 1 mg/ml);
— magnesium standard solution (Mg, 1 mg/ml);
— manganese standard solution (Mn, 1 mg /ml);
— nickel standard solution (Ni, 1 mg/ml);
— potassium standard solution (K, 1 mg/ml);
— silicon standard solution (Si, 1 mg/ml);
— sodium standard solution (Na, 1 mg/ml);
— strontium standard solution (Sr, 1 mg/ml);
— vanadium standard solution (V, 1 mg/ml);
— zinc standard solution (Zn, 1 mg/ml).
8.2.2 Mixed standard solution (each element 50 mg/l), place 5 ml each of the element standard
solutions (8.2.1) in a 100 ml volumetric flask. Dilute with water to the mark and mix well. Attention shall be
paid to ensure that no precipitation occurs during the mixing. Prepare a fresh solution before use.
8.3 Apparatus
Use the apparatus described in 7.2.3.
8.4 Procedure
8.4.1 Carry out the procedures described in 7.2.4.1. This solution is designated as the test solution.
ISO/DIS 21813:2026(en)
8.4.2 Spray a portion of the test solution into the argon plasma flame of an ICP-OES and measure the
emission intensity at the appropriate wavelength (Table 2). Interferences may be encountered. Carefully
choose the optimum emission lines that are free from interferences. The measurements should be carried
out using background correction.
Table 2 — Recommended emission lines for each element
Wavelength 1 Wavelength 2
Element
nm nm
Al 396,15 308,21
Cd 228,80 214,44
Ca 317,93 315,88
Co 228,61 238,89
Dy 353,17 394,46
Fe 238,20 239,56
Pb 220,35 217,00
Mg 285,21 279,07
Mn 257,61 259,37
Ni 231,60 221,64
K 766,49 —
Si 251,61 212,41
Na 589,59 —
Sr 407,77 421,55
V 290,88 292,46
Zn 206,20 213,86
NOTE For spectrometers with Echelle optics, to mitigate spectral interferences and sensitivities higher-order emission lines
should be selected, if available.
8.5 Blank solution
Perform the operation described in 8.4 without taking a sample. Designate the final solution as the blank
solution.
8.6 Calibration
Pour 15 ml barium solution (7.3.2.1) and 6 ml titanium solution (7.3.2.3) separately into six 100 ml
volumetric flasks. Add 0 ml, 0,5 ml, 1 ml, 1,5 ml, 2 ml and 2,5 ml of the mix standard solution (8.2.2) stepwise
and precisely. Add 20 ml hydrochloric acid (7.2.2.3), dilute with water to the mark and mix well. Spray a
portion of each solution into the argon plasma flame of the ICP-OES and measure the emission intensity at
the appropriate wavelength. The measurements should be carried out using background correction.
NOTE 1 Based on practical experience, using less than six points for the calibration function usually has no impact
on the precision of the determination. It is recommended to use at least three points for the calibration function
including the zero point, for example, calibration solutions with a concentration of 0 mg/L, 0,6 mg/L and 1,25 mg/L for
each trace element.
NOTE 2 The calculation of the calibration functions is usually carried out as linear regression.
ISO/DIS 21813:2026(en)
8.7 Calculation
Determine the concentration of each element in the test solution and in the blank solution from the
calibration function. Calculate the mass fraction of each element in the sample, w , according to Formula (3).
i
CC V
iB T
w (3)
i
10000m
where
w is the mass fraction of each element in the sample, in percent;
i
C is the measured concentration of each element in the test solution (7.2.4.1), in milligrams per
i
litre;
C is the measured concentration of each element in the blank test solution (8.5), in milligrams
B
per litre;
V is the volume of the test solution (7.2.4.1), in millilitres;
T
m is the mass of the test portion, in grams.
NOTE The analytical results obtained from the round-robin test are listed i
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