EN ISO 23739:2023
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of zirconium oxide powders (ISO 23739:2021)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of zirconium oxide powders (ISO 23739:2021)
This document specifies methods for the chemical analysis of zirconium oxide powders used as the raw material for fine ceramics.
It stipulates the determination methods of the zirconium, aluminium, barium, calcium, cerium, cobalt, gadolinium, hafnium, iron, magnesium, potassium, silicon, sodium, strontium, titanium and yttrium contents in zirconium oxide powders for fine ceramics. The test sample is decomposed by acid pressure decomposition or alkali fusion. Contents of zirconium and yttrium are determined by using either a precipitation and gravimetric method or an inductively coupled plasma–optical emission spectrometry (ICP–OES) method. Contents of aluminium, barium, calcium, cerium, cobalt, gadolinium, hafnium, iron, magnesium, potassium, silicon, sodium, strontium and titanium are determined by using an ICP–OES method.
Hochleistungskeramik - Verfahren zur chemischen Analyse von Zirconiumoxidpulvern (ISO 23739:2021)
Céramiques techniques - Méthodes pour l'analyse chimique des poudres d'oxyde de zirconium (ISO 23739:2021)
Le présent document spécifie des méthodes pour l’analyse chimique des poudres d’oxyde de zirconium utilisées comme matières premières pour les céramiques techniques.
Il stipule les méthodes de détermination des teneurs en zirconium, aluminium, baryum, calcium, cérium, cobalt, gadolinium, hafnium, fer, magnésium, potassium, silicium, sodium, strontium, titane et yttrium dans les poudres d’oxyde de zirconium pour les céramiques techniques. L’échantillon pour essai est décomposé par décomposition sous pression acide ou par fusion alcaline. Les teneurs en zirconium et en yttrium sont déterminées en utilisant soit une précipitation et une méthode gravimétrique, soit une méthode par spectrométrie d’émission optique avec plasma à couplage inductif (ICP–OES). Les teneurs en aluminium, baryum, calcium, cérium, cobalt, gadolinium, hafnium, fer, magnésium, potassium, silicium, sodium, strontium et titane sont déterminées par la méthode ICP–OES.
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Preskusne metode za kemične analize praškov cirkonijevega oksida (ISO 23739:2021)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN ISO 23739:2023
01-junij-2023
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Preskusne
metode za kemične analize praškov cirkonijevega oksida (ISO 23739:2021)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for
chemical analysis of zirconium oxide powders (ISO 23739:2021)
Hochleistungskeramik - Verfahren zur chemischen Analyse von Zirconiumoxidpulvern
(ISO 23739:2021)
Céramiques techniques - Méthodes pour l'analyse chimique des poudres d'oxyde de
zirconium (ISO 23739:2021)
Ta slovenski standard je istoveten z: prEN ISO 23739
ICS:
81.060.30 Sodobna keramika Advanced ceramics
oSIST prEN ISO 23739:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 23739:2023
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oSIST prEN ISO 23739:2023
INTERNATIONAL ISO
STANDARD 23739
First edition
2021-08
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of
zirconium oxide powders
Céramiques techniques — Méthodes pour l'analyse chimique des
poudres d'oxyde de zirconium
Reference number
ISO 23739:2021(E)
©
ISO 2021
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oSIST prEN ISO 23739:2023
ISO 23739:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
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
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Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
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oSIST prEN ISO 23739:2023
ISO 23739:2021(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 the test sample . 2
5.1 General . 2
5.2 Sampling . 2
5.3 Drying . 2
5.4 Weighing . 2
6 Reporting the analytical values . 2
6.1 Number of analyses. 2
6.2 Blank test . 2
6.3 E valuation of the analytical values. 2
6.4 Expression of analytical values . 3
7 Decomposition of the test sample . 3
7.1 Classification of the sample decomposition methods . 3
7.2 Acid pressure decomposition . 3
7.2.1 Reagents . 3
7.2.2 Apparatus and instruments. 3
7.2.3 Procedure . 4
7.2.4 Blank test . 4
7.3 Alkali fusion . 5
7.3.1 Reagents . 5
7.3.2 Apparatus and instruments. 5
7.3.3 Procedure . 5
7.3.4 Blank test . 5
8 Determination of the zirconium content . 6
8.1 Precipitation and gravimetric method . 6
8.1.1 Principle . 6
8.1.2 Reagents . 6
8.1.3 Apparatus and instruments. 6
8.1.4 Procedure . 6
8.1.5 Blank test . 7
8.1.6 Calculation . 7
8.2 ICP–OES method . 7
8.2.1 Principle . 7
8.2.2 Reagents . 7
8.2.3 Apparatus and instruments. 7
8.2.4 Procedure . 7
8.2.5 Blank test . 8
8.2.6 Drawing of calibration curve . 8
8.2.7 Calculation . 8
9 Determination of the major elements contents . 8
9.1 Precipitation and gravimetric method (for yttrium) . 8
9.1.1 Principle . 8
9.1.2 Reagents . 8
9.1.3 Apparatus and instruments. 8
9.1.4 Procedure . 9
9.1.5 Blank test . 9
9.1.6 Calculation . 9
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9.2 ICP–OES method (for calcium, hafnium, magnesium and yttrium) . 9
9.2.1 Principle . 9
9.2.2 Reagents . 9
9.2.3 Apparatus and instruments.10
9.2.4 Procedure .10
9.2.5 Blank test .10
9.2.6 Drawing of calibration curve .10
9.2.7 Calculation .11
10 Determination of the trace elements contents .11
10.1 Principle .11
10.2 Reagents.11
10.2.1 Elemental standard solution .11
10.2.2 Mixed standard solution (each element 50 mg/l) .12
10.3 Apparatus and instruments .12
10.4 Procedure .12
10.5 Blank test .13
10.6 Drawing of the calibration curve .13
10.7 Calculation .13
11 Test report .14
Annex A (informative) Analytical results obtained from the interlaboratory test .15
Bibliography .16
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oSIST prEN ISO 23739:2023
ISO 23739:2021(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
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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
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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.
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oSIST prEN ISO 23739:2023
INTERNATIONAL STANDARD ISO 23739:2021(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of zirconium
oxide powders
1 Scope
This document specifies methods for the chemical analysis of zirconium oxide powders used as the raw
material for fine ceramics.
It stipulates the determination methods of the zirconium, aluminium, barium, calcium, cerium, cobalt,
gadolinium, hafnium, iron, magnesium, potassium, silicon, sodium, strontium, titanium and yttrium
contents in zirconium oxide powders for fine ceramics. The test sample is decomposed by acid pressure
decomposition or alkali fusion. Contents of zirconium and yttrium are determined by using either a
precipitation and gravimetric method or an inductively coupled plasma–optical emission spectrometry
(ICP–OES) method. Contents of aluminium, barium, calcium, cerium, cobalt, gadolinium, hafnium, iron,
magnesium, potassium, silicon, sodium, strontium and titanium are determined by using an ICP–OES
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 835, Laboratory glassware — Graduated pipettes
ISO 3696, Water for analytical laboratory use — Specification and test methods
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 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 http:// www .electropedia .org/
4 Analytes and ranges
— Zirconium (Zr), range of 60 % to 74 % (mass fraction).
— Aluminium (Al), range of 0,01 % to 0,5 % (mass fraction).
— Barium (Ba), range of 0,01 % to 0,5 % (mass fraction).
— Calcium (Ca), range of 0,01 % to 6 % (mass fraction).
— Cerium (Ce), range of 0,01 % to 0,5 % (mass fraction).
— Cobalt (Co), range of 0,01 % to 0,5 % (mass fraction).
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ISO 23739:2021(E)
— Gadolinium (Gd), range of 0,01 % to 0,5 % (mass fraction).
— Hafnium (Hf), range of 0,01 % to 2 % (mass fraction).
— Iron (Fe), range of 0,01 % to 0,5 % (mass fraction).
— Magnesium (Mg), range of 0,01 % to 6 % (mass fraction).
— Potassium (K), range of 0,01 % to 0,5 % (mass fraction).
— Sodium (Na), range of 0,01 % to 0,5 % (mass fraction).
— Silicon (Si), range of 0,01 % to 0,5 % (mass fraction).
— Strontium (Sr), range of 0,01 % to 0,5 % (mass fraction).
— Titanium (Ti), range of 0,01 % to 0,5 % (mass fraction).
— Yttrium (Y), range of 0,01 % to 15 % (mass fraction).
5 Preparation of the 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 10 g of the 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, covered, for 1 h.
5.4 Weighing
Weigh the test 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 test sample twice on different days.
6.2 Blank test
Upon analysis, perform a blank test to correct the measured values.
6.3 E valuation 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 of 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.
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ISO 23739:2021(E)
Table 1 — Tolerances for the analytical values
Units: % (mass fraction)
Component Zr Ca, Hf, Mg, Y Al, Ba, Ce, Co, Gd, Fe, K, Na, Si, Sr, Ti
a
0,01
Tolerance 0,70 0,01
b
0,1
a
Applicable to content of less than 0,1 %.
b
Applicable to content of not less than 0,1 %.
6.4 Expression of analytical values
The analytical values shall be given in % (mass fraction) in dryness. The results shall be expressed to
two decimal places (see Annex A).
7 Decomposition of the test sample
7.1 Classification of the sample decomposition methods
a) Acid pressure decomposition.
b) Alkali fusion, for the determination of the contents of major elements such as zirconium, calcium,
hafnium, magnesium and yttrium, and also for the determination of silicon content.
7.2 Acid pressure decomposition
7.2.1 Reagents
It shall be ascertained that the reagents are of sufficiently high purity to permit their use without
compromising the accuracy of the determination.
7.2.1.1 Water, grade 1 or superior as specified in ISO 3696.
7.2.1.2 Sulfuric acid (1+1).
7.2.2 Apparatus and instruments
Use ordinary laboratory apparatus and instruments together with the following:
7.2.2.1 Pressure decomposition vessel. A pressure decomposition vessel is shown in Figure 1. Use
the vessel exclusively for this analysis to avoid cross-contamination.
7.2.2.2 Polytetrafluoroethylene (PTFE) bottle, with cap.
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ISO 23739:2021(E)
7.2.2.3 Air bath, capable of heating at 230 °C ± 5 °C.
Key
1 centre screw
2 screw cap
3 top plate
4 PTFE cap
5 cylinder
6 PTFE bottle
7 bottom plate
Figure 1 — Example of a pressure decomposition vessel
7.2.3 Procedure
Weigh 0,2 g of the test sample in a polytetrafluoroethylene bottle (7.2.2.2) and add 10 ml of sulfuric acid
(1+1). Put the PTFE bottle into a pressure decomposition vessel (7.2.2.1) and close the vessel according
to the manufacturer's instructions. Place the vessel in an air bath and heat it at 230 °C ± 5 °C for 16 h.
After cooling, disassemble the vessel and transfer the dissolved solution to a 150-ml beaker. Wash the
bottle six times with approximately 10 ml of warm water each time and collect the washings into the
beaker. Transfer the solution into a 200-ml volumetric flask, dilute it with water up to the mark and mix
well. This solution is designated as the sample solution.
7.2.4 Blank test
Perform the operation described in 7.2.3 without taking a sample to obtain the blank test value. The
resulting solution is designated as blank test solution.
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7.3 Alkali fusion
7.3.1 Reagents
It shall be ascertained that the reagents are of sufficiently high purity to permit their use without
compromising the accuracy of the determination.
7.3.1.1 Water, grade 1 or superior as specified in ISO 3696.
7.3.1.2 Lithium tetraborate (Li B O ), powdery, more than 99,995 % purity by trace metal basis.
2 4 7
Some commercial products of lithium tetraborate can contain certain impurities such as calcium,
potassium, silicon and sodium. Check their conformity with the test before use.
7.3.1.3 Hydrochloric acid (35 %, mass fraction).
7.3.2 Apparatus and instruments
Use ordinary laboratory apparatus and instruments together with the following:
7.3.2.1 Platinum crucible (30 ml), heated at 1 200 °C ± 50 °C for 15 min, and then cooled down to
room temperature in a desiccator.
7.3.2.2 Platinum lid.
7.3.2.3 Electric furnace, capable of being operated at 1 300 °C.
7.3.2.4 Ultrasonic bath.
7.3.3 Procedure
Mix 0,2 g of the test sample and 1,0 g of lithium tetraborate (7.3.1.2) in a platinum crucible (7.3.2.1).
Add 1,0 g of lithium tetraborate to the mixed sample. After covering the crucible with a platinum lid
(7.3.2.2), place the crucible in an electric furnace (7.3.2.3).
Raise the temperature of the furnace gradually and heat the crucible at 1 200 °C ± 50 °C until the
contents are completely decomposed.
Remove the crucible from the furnace and cool it to room temperature.
Put the crucible and the platinum lid into a 150-ml beaker containing 20 ml of hydrochloric acid (7.3.1.3)
and 100 ml of water (7.3.1.1). Covering the beaker with a watch glass, warm the beaker in an ultrasonic
bath (7.3.2.4) until the melt is completely dissolved into the solution.
Remove the beaker from the ultrasonic bath. Wash the watch glass, the crucible and the platinum lid
several times with approximately 50 ml of water and collect the washings into the beaker. After cooling,
transfer the solution into a 200-ml volumetric flask, dilute it with water up to the mark and mix well.
This is designated as the sample solution.
7.3.4 Blank test
Perform the operation described in 7.3.3 without taking a sample to obtain the blank test value. The
resulting solution is designated as blank test solution.
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ISO 23739:2021(E)
8 Determination of the zirconium content
8.1 Precipitation and gravimetric method
8.1.1 Principle
Zirconium with hafnium in the sample solution is precipitated by adding DL-mandelic acid solution.
After igniting the precipitate, the mass of the zirconium oxide (ZrO ) and hafnium oxide (HfO ) is
2 2
measured. The zirconium content is calculated from the mass of zirconium oxide as well as the hafnium
oxide content.
8.1.2 Reagents
It shall be ascertained that the reagents are of sufficiently high purity to permit their use without
compromising the accuracy of the determination.
8.1.2.1 Water, grade 1 or superior as specified in ISO 3696.
8.1.2.2 Hydrochloric acid (35 %, mass fraction).
8.1.2.3 DL-mandelic acid.
8.1.2.4 DL-mandelic acid solution (1 M), dissolve 152,15 g DL-mandelic acid (8.1.2.3) in 1 000 ml of
warm water.
8.1.2.5 Washing solution, dissolve 10 g DL-mandelic acid (8.1.2.3) in 200 ml of warm water and 4 ml
of hydrochloric acid (8.1.2.2).
8.1.3 Apparatus and instruments
Use the apparatus and instruments described in 7.3.2 together with the following:
8.1.3.1 Glass volumetric pipette, 50 ml, Class A, according to ISO 835.
8.1.3.2 Filter paper (ashless), diameter 110 mm, pore size index 8 µm.
8.1.3.3 Hot plate, with magnetic stirrer, capable of being operated at 450 °C.
8.1.4 Procedure
Transfer 50 ml of the sample solution (7.2.3 or 7.3.3) using a volumetric pipette (8.1.3.1) into a 500-ml
beaker. After adding 25 ml of hydrochloric acid (8.1.2.2) to the beaker, heat the solution to 90 °C on a hot
plate. While stirring the solution, add 50 ml of DL-mandelic acid solution (8.1.2.4). Covering the beaker
with a watch glass, heat the beaker at 90 °C for 1h. Wash the watch glass with approximately 30 ml of
warm water and add the washings into the beaker. Filter the solution using a filter paper (8.1.
...
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