Advanced technical ceramics - Methods of test for ceramic powders - Part 12: Chemical analysis of zirconia

This part of EN 725 specifies methods for the determination of the levels of silicon, aluminium, titanium, iron, calcium, magnesium, potassium, sodium, yttrium, hafnium, cerium and strontium using flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP - AES).  These methods are applicable to the concentration ranges given in clause 3, expressed as oxides.

Hochleistungskeramik - Prüfverfahren für keramische Pulver - Teil 12: Chemische Analyse von Zirconiumoxid

1 Anwendungsbereich
Dieser Teil von EN 725 legt Verfahren für die Bestimmung der Gehalte von Silicium, Aluminium, Titan, Eisen, Calcium, Magnesium, Kalium, Natrium, Yttrium, Hafnium, Cerium und Strontium mit Hilfe der Flammen-Atom-absorptionsspektrometrie (FAAS) und der Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) fest. Diese Verfahren sind auf die in Abschnitt 3 angegebenen Konzentrationsbereiche der oxidischen Verunreinigun-gen anwendbar.

Céramiques techniques avancées - Méthodes d'essai pour poudres céramiques - Partie 12: Analyse chimique de la zircone

La présente partie de l'EN 725 spécifie des méthodes permettant le dosage de silicium, d'aluminium, de titane, de fer, de calcium, de magnésium, de potassium, de sodium, d'yttrium, d'hafnium, de cérium et de strontium, par spectrométrie d'absorption atomique dans la flamme (FAAS) ou par spectrométrie d'émission atomique avec plasma à couplage inductif (ICP - AES). Ces méthodes s'appliquent aux gammes de concentration indiquées dans l'article 3, exprimées sous forme d'oxydes.

Advanced technical ceramics - Methods of test for ceramic powders - Part 12: Chemical analysis of zirconia

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Publication Date
10-Apr-2001
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SLOVENSKI STANDARD
SIST EN 725-12:2002
01-januar-2002
Advanced technical ceramics - Methods of test for ceramic powders - Part 12:
Chemical analysis of zirconia
Advanced technical ceramics - Methods of test for ceramic powders - Part 12: Chemical
analysis of zirconia
Hochleistungskeramik - Prüfverfahren für keramische Pulver - Teil 12: Chemische
Analyse von Zirconiumoxid
Céramiques techniques avancées - Méthodes d'essai pour poudres céramiques - Partie
12: Analyse chimique de la zircone
Ta slovenski standard je istoveten z: EN 725-12:2001
ICS:
81.060.30 Sodobna keramika Advanced ceramics
SIST EN 725-12:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 725-12:2002

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SIST EN 725-12:2002
EUROPEAN STANDARD
EN 725-12
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2001
ICS 81.060.30
English version
Advanced technical ceramics - Methods of test for ceramic
powders - Part 12: Chemical analysis of zirconia
Céramiques techniques avancées - Méthodes d'essai pour Hochleistungskeramik - Prüfverfahren für keramische
poudres céramiques - Partie 12: Analyse chimique de Pulver - Teil 12: Chemische Analyse von Zirconiumoxid
zircone
This European Standard was approved by CEN on 19 February 2001.
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 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 725-12:2001 E
worldwide for CEN national Members.

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SIST EN 725-12:2002
Page 2
EN 725-12:2001
Contents
Page
Foreword 3
1 Scope 4
2 Normative references 4
3 Concentration ranges 5
4 Principle 5
5 Reagents 5
6 Apparatus 7
7 Test sample 7
8 Sample preparation 8
9 Calibration 10
10 Adjustment of the apparatus 14
11 Measurements 16
12 Expression of results 17
13 Accuracy 18
14 Test report 19
Bibliography 20

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SIST EN 725-12:2002
Page 3
EN 725-12:2001
Foreword
This European Standard has been prepared by Technical Committee CEN/TC 184 "Advanced technical
ceramics", the secretariat of which is held by BSI.
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 October 2001, and conflicting national standards shall
be withdrawn at the latest by October 2001.
EN 725 ‘Methods of test for ceramic powders’ consists of 12 Parts:
Part 1: Determination of impurities in alumina
Part 2: Determination of impurities in barium titanate (ENV)
Part 3: Determination of the oxygen content of non-oxides by thermal extraction with a carrier gas
Part 4: Determination of oxygen content in aluminium nitride by XRF analysis (ENV)
Part 5: Determination of the particle size distribution
Part 6: Determination of the specific surface area
Part 7: Determination of the absolute density
Part 8: Determination of tapped bulk density
Part 9: Determination of untamped bulk density
Part 10: Determination of compaction properties
Part 11: Determination of densification on natural sintering (ENV)
Part 12: Chemical analysis of zirconia
This standard includes a bibliography.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg,
Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.

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SIST EN 725-12:2002
Page 4
EN 725-12:2001
1 Scope
This part of EN 725 specifies methods for the determination of the levels of silicon, aluminium,
titanium, iron, calcium, magnesium, potassium, sodium, yttrium, hafnium, cerium and strontium using
flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission
spectrometry (ICP - AES). These methods are applicable to the concentration ranges given in clause 3,
expressed as oxides.
2 Normative references
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of
these publications apply to this European Standard only when incorporated in it by amendment or
revision. For undated references the latest edition of the publication referred to applies (including
amendments).
ISO 3696 Water for analytical laboratory use - Specification and test methods
ECSC/CI 9 Chemical analysis of ferrous materials – Operational guidelines for the
application of flame atomic absorption spectrometry in standard methods
for the chemical analysis of iron and steel

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SIST EN 725-12:2002
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EN 725-12:2001
3 Concentration ranges
The FAAS and ICP-AES methods shall be applicable to the concentration ranges for each oxide as
follows:
Silicon oxide
10 g/g to 5 000 g/g;
Aluminium oxide
10 g/g to 5 000 g/g;
Titanium oxide
5 g/g to 2 000 g/g;
Iron oxide
5 g/g to 2 000 g/g;
Calcium oxide
5 g/g to 5 000 g/g;
Magnesium oxide
5 g/g to 5 000 g/g;
Potassium oxide
5 g/g to 2 000 g/g;
Sodium oxide
5 g/g to 2 000 g/g;
Yttrium oxide
5 g/g to 5 000 g/g;
Hafnium oxide
100 g/g to 5 000 g/g;
Cerium oxide 5 g/g to 5 000 g/g;
 
Strontium oxide 10 g/g to 5 000 g/g.
 
NOTE For concentrations above 5 000 g/g, the X-ray fluorescence (XRF) method, in
prEN ISO 12677:1998, should be used.
4 Principle
The test sample is decomposed by using either a fusion method or an acid microwave dissolution
method. The solution is transferred to a volumetric flask and diluted to a known volume. The
determination is made using FAAS or ICP-AES
5 Reagents
5.1 General
Reagents of at least 99,99 % purity or better, calibration solutions of ultra high purity and distilled
water or water of purity 2 (according to ISO 3696) or equivalent, shall be used.
5.2 Reagents for fusion
5.2.1 Lithium tetraborate, Li B O
2 4 7
-1
o
,
5.2.2 Nitric acid, density at 20 C approximately 1,33 gml HNO
3

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SIST EN 725-12:2002
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EN 725-12:2001
5.3 Reagents for acid microwave dissolution
5.3.1 Sulfuric acid (96 %), H SO
2 4
5.3.2 Ammonium fluoride, NH F
4
5.3.3 Hydrofluoric acid (40 %), HF
5.3.4 Hydrochloric acid (30 %), HCl
5.3.5 Nitric acid (65 %), HNO
3
5.4 Reagents for calibration
)
1
5.4.1 Pure zirconia of very low and known impurity levels
5.4.2 General
Commercial solutions or solutions obtained by dissolution of pure chemical product at a concentration
level of 0,1 g/l of the following shall be used.
5.4.2.1 Silicon, Si
5.4.2.2 Aluminium, Al
5.4.2.3 Titanium, Ti
5.4.2.4 Iron, Fe
5.4.2.5 Calcium, Ca
5.4.2.6 Magnesium, Mg
Potassium,
5.4.2.7 K
5.4.2.8 Sodium, Na
5.4.2.9 Yttrium, Y
5.4.2.10 Hafnium, Hf
5.4.2.11 Cerium, Ce

1
) Johnson Matthey specpure, total impurities < 50 g/g for 30 impurities, is an example of a suitable product available commercially.
This information is given for the convenience of users of this standard and does not constitute an endorsement by CEN of this product.

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SIST EN 725-12:2002
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EN 725-12:2001
5.4.2.12 Strontium, Sr
NOTE Certificates for analysis should be obtained.
6 Apparatus
6.1 Ordinary laboratory apparatus and apparatus for fusion.
6.1.1 Platinum gold alloy crucible and lid, with a capacity of 35 ml.
6.1.2 Muffle furnace, suitable for operation up to 1 200 °C  50 °C.
6.1.3 Magnetic stirrer.
6.2 Apparatus for acid microwave dissolution and for FAAS analysis.
6.2.1 Microwave unit, including PTFE-lined pressure vessels.
6.2.2 Flame atomic absorption spectrometer, conforming to ECSC/CI 9.
6.3 Apparatus for ICP-AES analysis
6.3.1 Inductively coupled plasma spectrometer.
7 Test sample
Dry the sample at 110 °C  10 °C for at least 1 h.
For the fusion method (see 8.1):
Weigh approximately 0,08 g of sample to the nearest 0,000 5 g.
For the acid dissolution method (see 8.2):
Weigh approximately 0,3 g or 0,125 g of sample to the nearest 0,000 5 g.

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SIST EN 725-12:2002
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EN 725-12:2001
8 Sample preparation
8.1 Fusion
Weigh 1g of lithium tetraborate (see 5.2.1) into a platinum gold alloy crucible (see 6.1.1).
Add approximately 0,08 g of test sample (see clause 7) and mix.
Place the crucible and contents into the muffle furnace (see 6.1.2) maintained at 1 200 °C  50 °C for
at least 30 min.
After the first 15 min, swirl the contents of the crucible for a few seconds and replace in the furnace.
At the end of the 30 min remove the crucible from the furnace and dip its base in water at ambient
temperature to allows easy removal of the melt from the crucible.
Put the crucible and melt into a 250 ml beaker which contains 50 ml of water and 10 ml of nitric acid
(see 5.2.2).
Place the beaker, covered with a watch glass, on a magnetic stirrer (see 6.1.3) and maintain the
agitation until complete dissolution.
Remove the beaker from the stirrer. Remove the crucible and rinse with distilled water and transfer the
solution into a 100 ml volumetric flask. Mix and make up to the mark with distilled water.
NOTE 1 Automatic fusion apparatus should be used with care to ensure complete fusion
the sample, followed by a suitable dissolution procedure.
NOTE 2 To prevent the melt sticking, the use of a new crucible is recommended.
8.2 Acid microwave dissolution
8.2.1 Example 1
Weigh approximately 0,3 g of the test sample (see clause 7) into the pressure vessel and add 3 ml of
sulphuric acid (see 5.3.1) and 270 mg of ammonium fluoride (see 5.3.2).
Close the vessel with the valve and ha
...

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