Bsi bs en 00725 12 2001
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BS EN
725-12:2001
BRITISH STANDARD
Advanced technical
ceramics — Methods of
test for ceramic
powders —
Part 12: Chemical analysis of zirconia
The European Standard EN 725-12:2001 has the status of a
British Standard
ICS 81.060.30
NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW
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BS EN 725-12:2001
National foreword
This British Standard is the official English language version of
EN 725-12:2001.
The UK participation in its preparation was entrusted to Technical Committee
RPI/13, Advanced technical ceramics, which has the responsibility to:
—
aid enquirers to understand the text;
—
present to the responsible European committee any enquiries on the
interpretation, or proposals for change, and keep the UK interests
informed;
—
monitor related international and European developments and
promulgate them in the UK.
A list of organizations represented on this committee can be obtained on
request to its secretary.
Cross-references
The British Standards which implement international or European
publications referred to in this document may be found in the BSI Standards
Catalogue under the section entitled “International Standards Correspondence
Index”, or by using the “Find” facility of the BSI Standards Electronic
Catalogue.
A British Standard does not purport to include all the necessary provisions of
a contract. Users of British Standards are responsible for their correct
application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.
This British Standard, having
been prepared under the
direction of the Sector
Committee for Materials and
Chemicals, was published
under the authority of the
Standards Committee and
comes into effect on
15 June 2001
Summary of pages
This document comprises a front cover, an inside front cover, the EN title page,
pages 2 to 20, an inside back cover and a back cover.
The BSI copyright date displayed in this document indicates when the
document was last issued.
Amendments issued since publication
Amd. No.
Date
Comments
© BSI 06-2001
ISBN 0 580 37668 0
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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
poudres céramiques - Partie 12: Analyse chimique de
zircone
Hochleistungskeramik - Prüfverfahren für keramische
Pulver - Teil 12: Chemische Analyse von Zirconiumoxid
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.
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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
© 2001 CEN
All rights of exploitation in any form and by any means reserved
worldwide for CEN national Members.
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EN 725-12:2001
Contents
Page
Foreword
1 Scope
2 Normative references
3 Concentration ranges
4 Principle
5 Reagents
6 Apparatus
7 Test sample
8 Sample preparation
9 Calibration
10 Adjustment of the apparatus
11 Measurements
12 Expression of results
13 Accuracy
14 Test report
Bibliography
3
4
4
5
5
5
7
7
8
10
14
16
17
18
19
20
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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:
Part 2:
Part 3:
Part 4:
Part 5:
Part 6:
Part 7:
Part 8:
Part 9:
Part 10:
Part 11:
Part 12:
Determination of impurities in alumina
Determination of impurities in barium titanate (ENV)
Determination of the oxygen content of non-oxides by thermal extraction with a carrier gas
Determination of oxygen content in aluminium nitride by XRF analysis (ENV)
Determination of the particle size distribution
Determination of the specific surface area
Determination of the absolute density
Determination of tapped bulk density
Determination of untamped bulk density
Determination of compaction properties
Determination of densification on natural sintering (ENV)
Chemical analysis of zirconia
This standard includes a bibliography.
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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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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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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
Aluminium oxide
Titanium oxide
Iron oxide
Calcium oxide
Magnesium oxide
Potassium oxide
Sodium oxide
Yttrium oxide
Hafnium oxide
Cerium oxide
Strontium oxide
10
10
5
5
5
5
5
5
5
100
5
10
g/g to 5 000 g/g;
g/g to 5 000 g/g;
g/g to 2 000 g/g;
g/g to 2 000 g/g;
g/g to 5 000 g/g;
g/g to 5 000 g/g;
g/g to 2 000 g/g;
g/g to 2 000 g/g;
g/g to 5 000 g/g;
g/g to 5 000 g/g;
g/g to 5 000 g/g;
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.
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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, Li2B4O7
-1
5.2.2 Nitric acid, density at 20 oC approximately 1,33 gml , HNO3
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EN 725-12:2001
5.3 Reagents for acid microwave dissolution
5.3.1 Sulfuric acid (96 %), H2SO4
5.3.2 Ammonium fluoride, NH4F
5.3.3 Hydrofluoric acid (40 %), HF
5.3.4 Hydrochloric acid (30 %), HCl
5.3.5 Nitric acid (65 %), HNO3
5.4 Reagents for calibration
5.4.1 Pure zirconia of very low and known impurity levels 1)
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
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5.4.2.3 Titanium, Ti
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5.4.2.4 Iron, Fe
5.4.2.5 Calcium, Ca
5.4.2.6 Magnesium, Mg
5.4.2.7 Potassium, 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
) 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.
1
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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.
6.1.2 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.
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6.1.1 Platinum gold alloy crucible and lid, with a capacity of 35 ml.
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
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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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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.
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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.
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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 hand tighten. Place the vessel into the microwave unit. Set the
microwave programme and start.
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NOTE Typical programme for microwave time and power settings:
Time (min)
2
15
5
20
Power (%)
60
30
0
20
At the end of the programme allow to cool, remove the vessel and open carefully.
Transfer the solution into a 100 ml volumetric flask. Rinse the vessel with distilled water and transfer
to the flask. Mix and make up to the mark with distilled water.
8.2.2 Example 2
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Weigh approximately 0,125 g of test sample (see clause 7) into the pressure vessel and add 7 ml of
hydrofluoric acid (see 5.3.3) and 7 ml of hydrochloric acid (see 5.3.4) and 1 ml of nitric acid
(see 5.3.5).
Close the vessel with the valve and tighten by hand.
Place the vessel into the microwave unit. Set the programme for 5 min at 250 °C, followed by 10 min
at 260 °C, and start.
At the end of the programme, allow to cool, remove the vessel and open carefully.
Transfer the solution into a 100 ml polypropylene volumetric flask.
Rinse out the vessel with distilled water and transfer to the flask. Add 5,5 ml of hydrochloric acid
(see 5.3.4).
Mix and make up to the mark with distilled water.
8.3 Blank test
With each analysis, carry out a blank in parallel with the test sample using identical reagents,
conditions, and analytical procedures in accordance with the chosen dissolution method (see 8.1 or
8.2). This blank solution shall be named S0.
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EN 725-12:2001
9 Calibration
9.1 General
The optimum calibration graph is obtained using calibration solutions with concentrations that are
compatible both with FAAS or ICP - AES analytical methods, and with the impurity concentrations in
the sample.
WARNING Take care to store solutions in non glass vessels.
Example procedures are given in 9.2.1 and 9.2.2
9.2 Calibration solutions
9.2.1 Fusion method
Weigh five portions of 0,08 g pure zirconia (see 5.4.1) and dissolve according to the method of sample
preparation given in 8.1. Transfer the solution into a 100 ml graduated flask, with a minimum of
washing. Add the quantities of standard solutions 5.4.2.1 to 5.4.2.12 given in Table 1 and make up to
the mark with distilled water.
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Table 1 — Volume of standard solutions (µl) to be added to the calibration solutions after fusion
Calibration
Standard solutions
(µl)
solution
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S0
S1
S2
S3
S4
Si
0
50
100
150
200
Al
0
50
100
150
200
Ti
0
100
150
200
250
Fe
0
50
125
200
300
Ca
0
50
125
200
300
Mg
0
100
150
200
250
K
0
50
150
250
350
Na
0
50
125
200
300
Y
0
50
150
250
350
Hf
0
50
150
250
350
Ce
0
50
150
250
350
Sr
0
50
150
250
350
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9.2.2 Acid microwave method
Weigh five portions of 0,3 g pure zirconia (see 5.4.1) and dissolve according to the method of sample
preparation given in 8.2.
Add the quantities of standard solutions 5.4.2.1 to 5.4.2.12 given in Table 2 and make up to the mark
with distilled water.
NOTE For acid microwave dissolution, Example 2 in 8.2.2, the volumes in Table 2 should
be adjusted for the sample mass.
Table 2 — Volume of standard solutions (µl) to be added to the calibration solutions
after microwave dissolution
Calibration
Standard solutions
(µl)
solution
S0
S1
S2
S3
S4
Si
0
150
300
500
750
Al
0
200
400
600
800
Ti
0
300
500
700
900
Fe
0
300
500
700
1 000
Ca
0
300
600
900
1 100
Mg
0
300
500
700
1 000
K
0
200
400
800
1 250
Na
0
200
400
800
1 200
Y
0
200
400
800
1 200
Hf
0
100
400
800
1 300
Ce
0
200
500
900
1 350
Sr
0
100
400
800
1 300
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9.3 Drawing the calibration curve
With the calibration solution prepared according to 9.1 or 9.2, calibration curves can be drawn directly
in g/g of impurity oxides by using respectively Table 3 or Table 4.
Table 3 — Impurity contents in micrograms per gram (g/g) for test sample dissolved by fusion
Calibration
Standard solutions
(ppm)
solution
S0
S1
S2
S3
S4
SiO2
b1
134+b1
267+b1
401+b1
535+b1
Al2O3
b2
118+b2
236+b2
354+b2
473+b2
TiO2
b3
208+b3
313+b3
417+b3
521+b3
Fe2O3
b4
89+b4
223+b4
357+b4
536+b4
CaO
b5
87+b5
219+b5
350+b5
525+b5
MgO
b6
207+b6
311+b6
414+b6
518+b6
K2O
b7
75+b7
156+b7
376+b7
527+b7
Na2O
b8
84+b8
211+b8
337+b8
505+b8
Y2O3
b9
79+b9
238+b9
397+b9
555+b9
HfO2
b10
74+b10
221+b10
369+b10
516+b10
CeO2
b11
70+b11
209+b11
348+b11
487+b11
SrO
b12
74+b12
222+b12
370+b12
517+b12
With b1 to b12 : SiO2 to SrO contents in blank solution obtained according to
8.3.
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Table 4 — Impurity contents in g/g for test sample dissolved by acid microwave dissolution
Standard solutions
Calibration
(ppm)
solution
S0
S1
S2
S3
S4
SiO2
b1
107+b1
214+b1
357+b1
535+b1
Al2O3
b2
126+b2
252+b2
378+b2
504+b2
TiO2
b3
167+b3
278+b3
389+b3
500+b3
Fe2O3
b4
143+b4
238+b4
334+b4
477+b4
CaO
b5
140+b5
280+b5
420+b5
513+b5
MgO
b6
166+b6
276+b6
387+b6
553+b6
K2O
b7
80+b7
161+b7
321+b7
502+b7
Na2O
b8
90+b8
180+b8
359+b8
539+b8
Y2O3
b9
85+b9
169+b9
339+b9
508+b9
HfO2
b10
39+b10
157+b10
314+b10
511+b10
CeO2
b11
74+b11
186+b11
334+b11
501+b11
SrO
b12
39+b12
158+b12
315+b12
512+b12
With b1 to b12 : SiO2 to SrO contents in blank solution obtained according to 8.3.
NOTE For acid microwave dissolution, Example 2, impurity contents in Table 4 need
adjustment for sample mass.
10 Adjustment of the apparatus
10.1 Atomic absorption spectrometer
Follow the manufacturer's instructions for igniting and extinguishing the nitrous oxide-acetylene flame
to avoid explosion.
WARNING If necessary, wear tinted safety glasses whenever the flame is alight.
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Set the wavelengths for the elements to be analysed (see Table 5) to obtain maximum absorbance. Fit
the correct burner and, in accordance with the manufacturer's instructions, light the flame. After 10 min
preheating of the burner, adjust fuel and burner to obtain maximum absorbance while aspirating the
highest calibration solution.
Aspirate the water and the calibration solutions to establish that the absorbance reading is not drifting
and then set the initial reading for water to zero absorbance.
10.2 Inductively coupled plasma spectrometer
Follow the manufacturer's instructions for igniting the plasma.
WARNING If necessary, wear anti-UV safety glasses whenever the plasma is ignited.
The wavelengths in Table 5 shall be used for the analysis.
Wait until a stable signal is obtained.
NOTE 1 Depending on the analytical method used and concentration of elements, other
wavelengths may be used.
NOTE 2 If other lines are used, interferences may be encountered and should be corrected
for.
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Table 5 — Recommended wavelengths in nanometres
Test
sample
Wavelength
(nm)
FAAS
ICP - AES
Si
251,6
251,611
Al
309,3
308,215
Ti
364,3
336,121
Fe
248,3
259,940
Ca
422,7
396,847
Mg
285,2
279,553
K
766,5
766,490
Na
589,0
588,995
Y
410,2
371,030
Hf
Not applicable
277,336
Ce
Not applicable
413,765
Sr
460,7
407,771
11 Measurements
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Aspirate each calibration solution and the final test solution in order of increasing concentrations.
Aspirate distilled water between each solution and record the readings when stable responses are
obtained. Repeat the measurements at least twice and calculate the average of the readings for each
solution.
For each element, draw the calibration curve by plotting the net signal values of the calibration solution
against the concentration of the element in micrograms per gram (g/g) (see Table 3 or
Table 4, according to the chosen method of dissolution). Convert the signal value of the test solution to
micrograms per gram (g/g), by means of the calibration curves, to obtain raw result.
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12 Expression of results
Calculate the concentration of element i in micrograms per gram (g/g) by subtracting the raw result
obtained in 12, the blank value bi (this value bi is the concentration read at the intersection of the
calibration curve with the concentrations axis).
bi I o i
Cimax
I 4i I oi
(1)
with:
bi :
Impurity content in blank solution for element i
Ioi:
Cimax:
signal value measured on blank solution for element i
I4i:
signal value measured on S4 solution for element i
content of element i in solution S4
For example (Test sample dissolved by acid microwave dissolution) :
bCa I o Ca
513
I 4 Ca I oCa
(2)
NOTE Equations (1) and (2) are only valid if background corrections are
made.
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13 Accuracy
The reproducibility of the method, as determined by inter laboratory trial on reference material
BCS 358, is given in Table 6.
Oxides
Number of
determinations
Mean
(g/g)
Standard
deviation
(g/g)
Certified
value
(g/g)
SiO2
5
2 080
260
2 000
Al2O3
8
820
270
800
TiO2
8
1 910
190
2 000
Fe2O3
8
610
140
640
CaO
7
14 650
2 020
15 000
MgO
5
33 570
380
34 200
K 2O
no result
available
no result
available
no result
available
no result
available
Na2O
no result
available
no result
available
no result
available
no result
available
Y2O3
no result
available
no result
available
no result
available
no result
available
HfO2
5
15 540
820
16 300
CeO
5
240
50
250
SrO
7
820
120
700
NOTE The reference material (BCS 358) was the only available certified
material for this round robin test.
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Table 6 — Reproducibility
