www bzfxw com BRITISH STANDARD BS EN 725 12 2001 Advanced technical ceramics — Methods of test for ceramic powders — Part 12 Chemical analysis of zirconia The European Standard EN 725 12 2001 has the[.]
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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 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 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 580 37668 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy B-1050 Brussels Ref No EN 725-12:2001 E Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 Contents Page Foreword Scope Normative references Concentration ranges Principle Reagents Apparatus Test sample Sample preparation Calibration 10 Adjustment of the apparatus 11 Measurements 12 Expression of results 13 Accuracy 14 Test report Bibliography 4 5 7 10 14 16 17 18 19 20 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 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 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 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 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 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 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 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 5 100 10 g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g; g/g to 000 g/g NOTE For concentrations above 000 g/g, the X-ray fluorescence (XRF) method, in prEN ISO 12677:1998, should be used ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 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 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 (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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 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 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 5.4.2.3 Titanium, Ti `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 5.4.2.12 Strontium, Sr NOTE Certificates for analysis should be obtained Apparatus 6.1 Ordinary laboratory apparatus and apparatus for fusion 6.1.2 Muffle furnace, suitable for operation up to 200 °C 50 °C 6.1.3 Magnetic stirrer 6.2 Apparatus for acid microwave dissolution and for FAAS analysis `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - 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 6.3 Apparatus for ICP-AES analysis ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 6.3.1 Inductively coupled plasma spectrometer Test sample Dry the sample at 110 °C 10 °C for at least h For the fusion method (see 8.1): Weigh approximately 0,08 g of sample to the nearest 0,000 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 g Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 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 200 °C 50 °C for at least 30 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 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 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 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 Automatic fusion apparatus should be used with care to ensure complete fusion the sample, followed by a suitable dissolution procedure `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - NOTE To prevent the melt sticking, the use of a new crucible is recommended 8.2 Acid microwave dissolution 8.2.1 Example Weigh approximately 0,3 g of the test sample (see clause 7) into the pressure vessel and add 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page EN 725-12:2001 NOTE Typical programme for microwave time and power settings: Time (min) 15 20 Power (%) 60 30 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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Weigh approximately 0,125 g of test sample (see clause 7) into the pressure vessel and add ml of hydrofluoric acid (see 5.3.3) and ml of hydrochloric acid (see 5.3.4) and 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 at 250 °C, followed by 10 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 10 EN 725-12:2001 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 and make up to the mark with distilled water `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 11 EN 725-12:2001 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Table — Volume of standard solutions (µl) to be added to the calibration solutions after fusion Calibration Standard solutions (µl) solution Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy S0 S1 S2 S3 S4 Si 50 100 150 200 Al 50 100 150 200 Ti 100 150 200 250 Fe 50 125 200 300 Ca 50 125 200 300 Mg 100 150 200 250 K 50 150 250 350 Na 50 125 200 300 Y 50 150 250 350 Hf 50 150 250 350 Ce 50 150 250 350 Sr 50 150 250 350 Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 12 EN 725-12:2001 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 and make up to the mark with distilled water NOTE For acid microwave dissolution, Example in 8.2.2, the volumes in Table should be adjusted for the sample mass Table — 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 150 300 500 750 Al 200 400 600 800 Ti 300 500 700 900 Fe 300 500 700 000 Ca 300 600 900 100 Mg 300 500 700 000 K 200 400 800 250 Na 200 400 800 200 Y 200 400 800 200 Hf 100 400 800 300 Ce 200 500 900 350 Sr 100 400 800 300 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 13 EN 725-12:2001 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 or Table Table — 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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Page 14 EN 725-12:2001 Table — 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 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 15 EN 725-12:2001 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 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 shall be used for the analysis Wait until a stable signal is obtained NOTE Depending on the analytical method used and concentration of elements, other wavelengths may be used NOTE If other lines are used, interferences may be encountered and should be corrected for `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 16 EN 725-12:2001 Table — 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 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - 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 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 Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 17 EN 725-12:2001 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 Ca I oCa (2) NOTE Equations (1) and (2) are only valid if background corrections are made `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 Page 18 EN 725-12:2001 13 Accuracy The reproducibility of the method, as determined by inter laboratory trial on reference material BCS 358, is given in Table Oxides Number of determinations Mean (g/g) Standard deviation (g/g) Certified value (g/g) SiO2 080 260 000 Al2O3 820 270 800 TiO2 910 190 000 Fe2O3 610 140 640 CaO 14 650 020 15 000 MgO 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 15 540 820 16 300 CeO 240 50 250 SrO 820 120 700 NOTE The reference material (BCS 358) was the only available certified material for this round robin test Copyright British Standards Institution Reproduced by IHS under license with BSI - Uncontrolled Copy Document provided by IHS Licensee=Bureau Veritas/5959906001, 11/08/2004 05:29:16 MST Questions or comments about this message: please call the Document Policy Group at 303-397-2295 `,,,,``,`,,,,`,,,`,,`,`,``,,-`-`,,`,,`,`,,` - Table — Reproducibility