SIST EN ISO 21813:2023
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of high purity barium titanate powders (ISO 21813:2019)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of high purity barium titanate powders (ISO 21813:2019)
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.
Hochleistungskeramik - Verfahren zur chemischen Analyse von hochreinen Bariumtitanatpulvern (ISO 21813:2019)
Dieses Dokument legt Verfahren für die chemische Analyse von feinen, hochreinen Bariumtitanatpulvern fest, die als Rohmaterial für Hochleistungskeramiken verwendet werden.
Dieses Dokument legt die Verfahren zur Bestimmung des Barium-, Titan-, Aluminium-, Cadmium-, Calcium-, Cobalt-, Dysprosium-, Eisen-, Blei-, Magnesium-, Mangan-, Nickel-, Niob-, Kalium-, Silicium-, Natrium-, Strontium-, Vanadium-, Zirkonium-, Kohlenstoff-, Sauerstoff- und Stickstoffgehaltes in hochreinen Bariumtitanatpulvern fest. Der Barium und Titangehalt, die wesentlichen Elemente, werden mithilfe eines gravimetrischen Verfahrens mit Säureaufschluss oder eines Verfahrens mit Säureaufschluss kombiniert mit optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (en: inductively coupled plasma optical emission spectrometry, ICP-OES) bestimmt. Die Aluminium-, Cadmium-, Calcium-, Chrom-, Cobalt-, Dysprosium-, Eisen-, Blei-, Magnesium-, Mangan-, Nickel-, Niob-, Kalium-, Silicium-, Strontium-, Vanadium- und Zirkoniumgehalte werden simultan mithilfe einem Verfahren von Säureaufschluss mit ICP-OES bestimmt. Der Stickstoffgehalt wird mithilfe eines -Inertgasschmelzverfahrens mit Wärmeleitfähigkeitsdetektion bestimmt, während der Sauerstoffgehalt mithilfe eines Inertgasschmelzverfahrens mit IR-Absorptionsspektroskopie bestimmt wird. Der Kohlenstoffgehalt wird abschließend mithilfe eines Verbrennungs-IR-Absorptionsspektrometrieverfahrens oder eines Verbrennungs-Konduktometrie-Verfahrens bestimmt.
Céramiques techniques - Méthodes d’analyse chimique des poudres de titanate de baryum à haute pureté (ISO 21813:2019)
Le présent document spécifie des méthodes d'analyse chimique de poudres fines de titanate de baryum de haute pureté utilisées comme matière première pour les céramiques techniques.
Le présent document spécifie les méthodes de détermination des teneurs en baryum, titane, aluminium, cadmium, calcium, cobalt, dysprosium, fer, plomb, magnésium, manganèse, nickel, niobium, potassium, silicium, sodium, strontium, vanadium, zirconium, carbone, oxygène et azote dans les poudres de titane de baryum de haute pureté. Les teneurs en baryum et en titane (les éléments principaux) sont déterminées au moyen d’une méthode par gravimétrie après décomposition en milieu acide ou d’une méthode par spectrométrie d’émission optique à plasma induit (ICP-OES) après décomposition en milieu acide. Les teneurs en aluminium, cadmium, calcium, chrome, cobalt, dysprosium, fer, plomb, magnésium, manganèse, nickel, niobium, potassium, silicium, strontium, vanadium et zirconium sont déterminées simultanément au moyen d’une méthode par ICP-OES après minéralisation en milieu acide. La teneur en azote est déterminée à l’aide d’une méthode par conductivité thermique après fusion sous gaz inerte, tandis que celle de l’oxygène est déterminée en utilisant une méthode par spectrométrie d’absorption infrarouge après fusion sous gaz inerte. Enfin, la teneur en carbone est déterminée au moyen d'une méthode par spectrométrie d’absorption infrarouge après combustion ou d’une méthode par conductométrie après combustion.
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za kemijsko analizo praškov barijevega titanata visoke čistosti (ISO 21813:2019)
Standard ISO 21813 določa metode za kemijsko analizo finih praškov barijevega titanata visoke čistosti, ki se uporabljajo kot surovina za fino keramiko.
Standard ISO 21813 določa metode za določevanje vsebnosti barija, titana, aluminija, kadmija, kalcija, kobalta, disprozija, železa, svinca, magnezija, mangana, niklja, niobija, kalija, silicija, natrija, stroncija, vanadija, cirkonija, ogljika, kisika in dušika v praških barijevega titanata visoke čistosti. Vsebnost barija in titana – glavnih elementov – se določi z uporabo gravimetrične metode v kombinaciji s kislinsko razgradnjo ali metode optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP-OES) v kombinaciji s kislinsko razgradnjo. Vsebnost aluminija, kadmija, kalcija, kroma, kobalta, disprozija, železa, svinca, magnezija, mangana, niklja, niobija, kalija, silicija, stroncija, vanadija in cirkonija se hkrati določi z uporabo metode optične emisijske spektrometrije z induktivno sklopljeno plazmo v kombinaciji z razklopom v kislini. Vsebnost dušika se določi z uporabo metode toplotne prevodnosti v kombinaciji s fuzijo inertnega plina, vsebnost kisika pa z metodo IR-absorpcijske spektrometrije v kombinaciji s fuzijo inertnega plina. Vsebnost ogljika se določi z uporabo metode IR-absorpcijske spektrometrije v kombinaciji z zgorevanjem ali metode konduktometrije v kombinaciji z zgorevanjem.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2023
Nadomešča:
SIST EN 725-2:2009
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za
kemijsko analizo praškov barijevega titanata visoke čistosti (ISO 21813:2019)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for
chemical analysis of high purity barium titanate powders (ISO 21813:2019)
Hochleistungskeramik - Verfahren zur chemischen Analyse von hochreinen
Bariumtitanatpulvern (ISO 21813:2019)
Céramiques techniques - Méthodes d’analyse chimique des poudres de titanate de
baryum à haute pureté (ISO 21813:2019)
Ta slovenski standard je istoveten z: EN ISO 21813:2022
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 21813
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2022
EUROPÄISCHE NORM
ICS 81.060.30 Supersedes EN 725-2:2007
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Methods for chemical analysis of high purity
barium titanate powders (ISO 21813:2019)
Céramiques techniques - Méthodes d'analyse chimique Hochleistungskeramik - Verfahren zur chemischen
des poudres de titanate de baryum à haute pureté (ISO Analyse von hochreinen Bariumtitanatpulvern (ISO
21813:2019) 21813:2019)
This European Standard was approved by CEN on 30 October 2022.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
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United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21813:2022 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
The text of ISO 21813:2019 has been prepared by Technical Committee ISO/TC 206 "Fine ceramics” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 21813:2022
by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by
DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by May 2023, and conflicting national standards shall be
withdrawn at the latest by May 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 725-2:2007.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 21813:2019 has been approved by CEN as EN ISO 21813:2022 without any modification.
INTERNATIONAL ISO
STANDARD 21813
First edition
2019-02
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of high
purity barium titanate powders
Céramiques techniques — Méthodes d’analyse chimique des poudres
de titanate de baryum à haute pureté
Reference number
ISO 21813:2019(E)
©
ISO 2019
ISO 21813:2019(E)
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
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Published in Switzerland
ii © ISO 2019 – All rights reserved
ISO 21813:2019(E)
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 . 3
6 Reporting the analytical values . 3
6.1 Number of analyses. 3
6.2 Blank test . 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 test . 5
7.2.6 Calculation . 5
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 . 6
7.3.5 Blank test . 7
7.3.6 Drawing of the calibration curve . 7
7.3.7 Calculation . 7
8 Determination of the trace element contents . 7
8.1 Principle . 7
8.2 Reagents. 7
8.3 Apparatus . 8
8.4 Procedure . 8
8.5 Blank test . 9
8.6 Drawing of the calibration curve . 9
8.7 Calculation . 9
9 Determination of the total nitrogen content . 9
9.1 Principle . 9
9.2 Reagents.10
9.3 Apparatus .10
9.4 Instrument .10
9.5 Procedure .11
9.5.1 Starting up of the instrument .11
9.5.2 Preliminary heating . .12
9.5.3 Degassing of the graphite crucible .12
9.5.4 Measuring .12
9.6 Blank test .12
ISO 21813:2019(E)
9.7 Calculation of the calibration coefficient .12
9.8 Calculation .13
10 Determination of the oxygen content .13
10.1 Principle .13
10.2 Reagents.13
10.3 Apparatus .13
10.4 Instrument .13
10.5 Procedure .13
10.6 Blank test .14
10.7 Calculation of the calibration coefficient .14
10.8 Calculation .14
11 Determination of the carbon content .14
11.1 Classification of the determination methods .14
11.2 Combustion (resistance furnace)-IR absorption spectrometry .15
11.2.1 Principle .15
11.2.2 Reagents .15
11.2.3 Apparatus .15
11.2.4 Instrument .15
11.2.5 Procedure .16
11.2.6 Blank test .17
11.2.7 Calculation of the calibration coefficient .17
11.2.8 Calculation .18
11.3 Combustion (radio frequency heating furnace)-thermal conductometry .18
11.3.1 Principle .18
11.3.2 Reagents .18
11.3.3 Apparatus .18
11.3.4 Instrument .18
11.3.5 Procedure .19
11.3.6 Blank test .20
11.3.7 Calculation of the calibration coefficient .20
11.3.8 Calculation .20
11.4 Combustion (radio frequency heating furnace)-IR absorption spectrometry .20
11.4.1 Principle .20
11.4.2 Reagents .20
11.4.3 Apparatus .20
11.4.4 Instrument .20
11.4.5 Procedure .21
11.4.6 Blank test .22
11.4.7 Calculation of the calibration coefficient .22
11.4.8 Calculation .22
12 Test report .22
Annex A (informative) Analytical results obtained from the round-robin test .23
Bibliography .25
iv © ISO 2019 – All rights reserved
ISO 21813:2019(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
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ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
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expressions related to conformity assessment, as well as information about ISO's adherence to the
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.org/iso/foreword .html.
This document 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.
INTERNATIONAL STANDARD ISO 21813:2019(E)
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, 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.
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 http: //www .electropedia .org/
4 Analytes and ranges
a) Barium (Ba), range of 40 % to 60 % (mass fraction).
ISO 21813:2019(E)
b) Titanium (Ti), range of 10 % to 30 % (mass fraction).
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) Niobium (Nb), range of 0,001 % to 0,03 % (mass fraction).
n) Potassium (K), range of 0,001 % to 0,03 % (mass fraction).
o) Silicon (Si), range of 0,001 % to 0,03 % (mass fraction).
p) Sodium (Na), range of 0,001 % to 0,03 % (mass fraction).
q) Strontium (Sr), range of 0,001 % to 0,03 % (mass fraction).
r) Vanadium (V), range of 0,001 % to 0,03 % (mass fraction).
s) Zirconium (Zr), range of 0,001 % to 0,03 % (mass fraction).
t) Total nitrogen (T.N), range of 0,01 % to 5 % (mass fraction).
u) Oxygen (O), range of 10 % to 30 % (mass fraction).
v) 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 an air bath at 110 °C ± 5 °C for 2 h, uncovered, and cool in a
desiccator (desiccant: magnesium perchlorate), covered, for 1 h.
2 © ISO 2019 – All rights reserved
ISO 21813:2019(E)
5.4 Weighing
Weigh the sample to the nearest 0,1 mg of the required quantity using a balance.
6 Reporting the analytical values
6.1 Number of analyses
Analyse the sample twice on different days.
6.2 Blank test
Upon analysis, perform a blank test to correct the measured values.
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), in dryness.
a) Barium, titanium, oxygen, and nitrogen: 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 Total N O C
Nb, K, Si, Na, Sr, V, Zr,
a a c e
0,30 0,20 0,001 0,01
Tolerance 0,50 0,005
b b d f
0,40 0,30 0,005 0,05
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).
e
Applicable to content of less than 1,0 % (mass fraction).
f
Applicable to content of not less than 1,0 % (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.
ISO 21813:2019(E)
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.
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, with a range of the appropriate volume (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).
4 © ISO 2019 – All rights reserved
ISO 21813:2019(E)
7.2.3.8 PTFE beaker cover.
7.2.3.9 Volumetric flask (100 ml, 500 ml).
7.2.3.10 Hot plate, with magnetic stirrer.
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 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 the contents at (85 ± 5) °C 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 grain 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 the
contents at 200 °C for 1 h.
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 test
Carry out the procedure described in 7.2.4 without the sample. Designate the final solution as the blank
solution.
7.2.6 Calculation
Calculate the barium and titanium contents according to Formula (1).
WW=− Wm//××Va FFor ×100 (1)
()
21 12
ISO 21813:2019(E)
where
W is the barium or titanium content, in % (mass fraction);
W is the blank platinum crucible weight, in g;
W is the platinum crucible weight after ignition, in g;
m is the mass of the sample, in g;
V is the test solution volume, in ml;
a is the aliquot solution volume, in ml;
F is the mass ratio of barium in barium sulfate (0,588 4);
F is the mass ratio of titanium in titanium oxide (0,599 3).
7.3 Acid decomposition-ICP-OES method
7.3.1 Principle
Barium and titanium are decomposed in concentrated hydrogen peroxide and hydrochloric acid. The
barium and titanium present in the test solution are analysed by ICP-OES at a selected wavelength.
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.
7.3.4 Procedure
7.3.4.1 Carry out the procedures described in 7.2.4.1.
6 © ISO 2019 – All rights reserved
ISO 21813:2019(E)
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.
7.3.5 Blank test
Perform the operation described in 7.3.4 without using a sample to obtain the blank test value.
7.3.6 Drawing of the calibration curve
Transfer 0 ml, 1 ml, 2 ml, 3 ml, 4 ml and 5 ml aliquots of the barium and titanium standard solutions
(7.3.2.2 and 7.3.2.4, respectively) to separate 100 ml volumetric flasks. To each flask, add 5 ml
hydrochloric acid (1+10) and 5 ml hydrogen peroxide (1+10). Dilute with water to the mark and mix well.
7.3.7 Calculation
Determine the barium and titanium concentrations in the test solution and blank from the calibration
curve. Calculate the barium and titanium contents, W, expressed in the percentage mass fraction, from
Formula (2).
Wm=−mm//××500 10 100 (2)
()
sb
where
W is the barium and titanium content, in % (mass fraction);
m is the mass of barium and titanium in the test solution, in g;
s
m is the mass of barium and titanium in the blank solution, in g;
b
m is the mass of the test portion, in g.
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
the selected wavelength.
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);
ISO 21813:2019(E)
— 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);
— zirconium standard solution (Zr, 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.
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 wavelength that is free from concomitants.
Table 2 — Examples of an analytical wavelength 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
Considering the spectral interferences and the sensitivities, choose the higher-order spectral lines, if available.
8 © ISO 2019 – All rights reserved
ISO 21813:2019(E)
Table 2 (continued)
Wavelength 1 Wavelength 2
Element
nm nm
Ni 231,60 221,64
Nb 309,41 313,07
K 766,49 —
Si 251,61 212,41
Na 589,59 —
Sr 407,77 421,55
V 290,88 292,46
Zr 343,82 339,19
Considering the spectral interferences and the sensitivities, choose the higher-order spectral lines, if available.
8.5 Blank test
Perform the operation described in 8.4 without taking a sample to obtain the blank test value.
8.6 Drawing of the calibration curve
Pour 16 ml barium solution (7.3.2.1) and 8 ml titanium solution (7.3.2.3) separately into five 100 ml
volumetric flasks. Add 0 ml
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