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1、BRITISH STANDARD BS EN 725-1:2007 Advanced technical ceramics Methods of test for ceramic powders Part 1: Determination of impurities in alumina The European Standard EN 725-1:2007 has the status of a British Standard ICS 81.060.30 ? Licensed Copy: London South Bank University, London South Bank Uni
2、versity, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 725-1:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2007 BSI 2007 ISBN 978 0 580 54527 6 National foreword This British Standard is the UK impleme
3、ntation of EN 725-1:2007. It supersedes BS EN 725-1:1997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics. A list of organizations represented on this committee can be obtained on request to its secretary. This publi
4、cation does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Ba
5、nk University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 725-1 September 2007 ICS 81.060.30Supersedes EN 725-1:1997 English Version Advanced technical ceramics - Methods of test for ceramic powder
6、s - Part 1: Determination of impurities in alumina Cramiques techniques avances - Mthodes dessai des poudres cramiques - Partie 1 : Dosage des impurets dans lalumine Hochleistungskeramik - Prfverfahren fr keramische Pulver - Teil 1: Bestimmung von Verunreinigungen in Aluminiumoxidpulver This Europea
7、n Standard was approved by CEN on 11 August 2007. 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 conce
8、rning such national standards may be obtained on application to the CEN 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 ow
9、n language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithua
10、nia, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007
11、CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 725-1:2007: E Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 2 Contents Pag
12、e Foreword3 1 Scope 4 2 Normative references4 3 Principle4 4 Reagents.4 4.1 General4 4.2 Reagents for fusion.4 4.3 Sulphuric acid-phosphoric acid mixture for acid dissolution 5 4.4 Reagents for calibration5 5 Apparatus .5 6 Test sample5 7 Decomposition of the test sample.6 7.1 General6 7.2 Fusion .6
13、 7.3 Acid dissolution.6 8 Calibration graph.6 8.1 General6 8.2 Fusion .6 8.3 Acid dissolution.7 8.4 Drawing the calibration curve 7 9 Adjustment of the apparatus7 9.1 Atomic absorption spectrometer.7 9.2 Inductively coupled plasma spectrometer8 10 Measurements8 11 Expression of the results8 12 Test
14、report9 Annex A (informative) Repeatability and reproducibility 10 Bibliography11 Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 3 Foreword This document (EN 725-1:2007) has been prepared by
15、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 March 2008, and conflicting national standard
16、s shall be withdrawn at the latest by March 2008. This document supersedes EN 725-1:1997. EN 725 Advanced technical ceramics Methods of test for ceramic powders was prepared in parts as follows: Part 1: Determination of impurities in alumina Part 2: Determination of impurities in barium titanate Par
17、t 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 Part 5 Determination of particle size distribution Part 6: Determination of the specific surface area withdrawn Part 7: Determi
18、nation of the absolute density withdrawn Part 8: Determination of tapped bulk density Part 9: Determination of un-tapped bulk density Part 10: Determination of compaction properties Part 11: Determination of densification on natural sintering Part 12: Chemical analysis of zirconia Parts 6 and 7 of t
19、he series were superseded in 2005 by EN ISO 18757 and EN ISO 18753 respectively. 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, Cyprus, Czech Republic, Denma
20、rk, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: London South Bank University, London South Bank Uni
21、versity, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 4 1 Scope This Part of EN 725 specifies one fusion and one acid dissolution method for the determination of elements of sodium, potassium, iron, silicon, calcium and magnesium present as impurities in alumina u
22、sing atomic absorption spectroscopy (AAS) or inductively coupled plasma (ICP) spectroscopy. For each element present as impurities, the methods are applicable to the following ranges, calculated as oxides : Sodium oxide: 20 ppm to 6000 ppm Potassium oxide: 20 ppm to 100 ppm Ferric oxide: 20 ppm to 3
23、00 ppm Silica: 50 ppm to 2000 ppm Calcium oxide: 20 ppm to 700 ppm Magnesium oxide: 5 ppm to 1000 ppm 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the la
24、test edition of the referenced document (including any amendments) applies. EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Princ
25、iple A test sample is decomposed by using either a fusion method or an acid dissolution method. NOTE The acid dissolution method cannot be used for the determination of silicon. The solution is transferred to a volumetric flask and diluted to a known volume, and the elements are determined by AAS or
26、 ICP. 4 Reagents 4.1 General During the analysis, use only reagents and calibration solutions of at least 99,99 % purity and water conforming to EN ISO 3696, Grade 3, or better. 4.2 Reagents for fusion 4.2.1 Lithium metaborate - LiBO2 4.2.2 Nitric acid HNO3 - (20 = 1,33 g/ml) Licensed Copy: London S
27、outh Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 5 4.3 Sulphuric acid-phosphoric acid mixture for acid dissolution Pour 700 ml of phosphoric acid (20 = 1,78 g/ml) into 300 ml of sulphuric acid (20 = 1,84 g/ml). 4.4 R
28、eagents for calibration 4.4.1 Pure alumina, of very low and known impurity levels, 99,99% purity. 4.4.2 Sodium - commercial solution or solution obtained by dissolution of pure chemical compound, of concentration 1 g/l. 4.4.3 Potassium - commercial solution or solution obtained by dissolution of pur
29、e chemical compound, of concentration 1 g/l. 4.4.4 Iron (ferric) - commercial solution or solution obtained by dissolution of pure chemical compound, of concentration 1 g/l. 4.4.5 Silicon - commercial solution or solution obtained by dissolution of pure chemical compound, of concentration 1 g/l. 4.4
30、.6 Calcium - commercial solution or solution obtained by dissolution of pure chemical compound, of concentration 1 g/l. 4.4.7 Magnesium - commercial solution or solution obtained by dissolution of pure chemical compound, of concentration 1 g/l. 5 Apparatus 5.1 Platinum or platinum-gold crucible with
31、 a capacity of at least 50 ml 5.2 Muffle furnace, suitable for operation in the range of (1 000 50) C to (1 200 50) C 5.3 Hot plate with magnetic stirrer 5.4 Atomic absorption spectrometer and/or inductively coupled plasma spectrometer 5.5 Laboratory glassware 5.6 Platinum spatula 6 Test sample Use
32、samples of approximately: 1 g for decomposition by fusion; 1 g for decomposition by acid dissolution. Weigh them to 0,0001 g. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 6 7 Decomposition
33、of the test sample 7.1 General Dissolve either by a fusion method (see 7.2) or an acid dissolution method (see 7.3) 7.2 Fusion Weigh 4 g of LiBO2 (4.2.1) and 1 g of test sample into a platinum or platinum-gold crucible (5.1). Mix intimately using a platinum spatula, put on lid. Place the crucible an
34、d contents into the muffle furnace (5.2) maintained at 1150 C 50 C for 30 min (after the first 15 min, swirl the contents of the crucible for a few seconds and put back in the muffle). Remove the crucible from the furnace, remove lid and rinse with distilled water, pouring the residue into a 400 ml
35、beaker containing 80 ml of water and 20 ml of nitric acid (4.2.2). Dip its base in water at ambient temperature (this procedure allows easy removal of the bead from the crucible). To prevent sticking of melt in the crucible, either use a new crucible or, with an old one, immerse it in the solution.
36、Pour the bead, carefully, into the 400 ml beaker that contains 80 ml of water and 20 ml of nitric acid (4.2.2). Place the beaker, covered with a watch glass on a hot plate (5.3) with magnetic stirring and maintain the agitation at approximately 80 C 10 C until complete dissolution. Remove the beaker
37、 from the stirrer and allow it to cool down. Transfer the solution quantitatively into a 200 ml volumetric flask. Allow it to cool down to room temperature and make up to the mark. 7.3 Acid dissolution Weigh the test sample (see Clause 6) into a platinum or gold-platinum crucible (5.1). Add carefull
38、y 12 ml of sulphuric acid-phosphoric acid mixture (4.3) and cover with a lid. Put the crucible with the lid on to the hot plate (5.3) and maintain it at boiling for 12 min. Remove the crucible from the heating device and allow it to cool down. Transfer the content quantitatively into a 100 ml volume
39、tric flask which contains 30 ml of water. Rinse the crucible and the lid with distilled water into the flask and after cooling, make up to the mark with water. 8 Calibration graph 8.1 General The optimum calibration graph is obtained using calibration solutions whose concentrations are compatible bo
40、th with the analytical method (AAS or ICP) and with the impurity concentrations in the sample, and matrix matched. The following procedure is given as an example. 8.2 Fusion Prepare five decompositions of pure alumina (4.4.1) in accordance with 7.2. Transfer into five 200 ml volumetric flasks and di
41、lute to 150 ml with water. Add the quantities of solutions indicated in Table 1. Make up to the mark with water. Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 7 Table 1 Quantities of solutio
42、ns for fusion Elements 1 2 3 4 5 Na 0 l 1 l 2 l 4 l 6 l K 0 l 100 l 200 l 300 l 400 l Ca 0 l 250 l 500 l 750 l 1000 l Fe 0 l 100 l 200 l 300 l 400 l Si 0 l 200 l 400 l 800 l 1600 l Mg 0 l 250 l 500 l 750 l 1000 l 8.3 Acid dissolution Prepare 5 dissolutions of pure alumina (4.4.1) in accordance with
43、7.3. Transfer into five 100 ml volumetric flasks and dilute to 50 ml with water. Add the quantities indicated in Table 2. Make up to the mark with water. Table 2 Quantities of solutions for acid dissolution Elements 1 2 3 4 5 Na 0 l 500 l 1000 l 2000 l 3000 l K 0 l 50 l 100 l 150 l 200 l Ca 0 l 125
44、l 250 l 375 l 500 l Fe 0 l 50 l 100 l 150 l 200 l Mg 0 l 125 l 250 l 375 l 1000 l 8.4 Drawing the calibration curve 8.4.1 Blank test Prepare a blank test in accordance with 8.2 or 8.3 using the same quantities of all reagents as for dissolution of the test sample, but using pure alumina (4.4.1) in p
45、lace of the test sample. 8.4.2 Drawing the calibration curve Draw a graph of the AAS or ICP intensities recorded using the calibration solutions prepared against the impurity concentrations. 9 Adjustment of the apparatus 9.1 Atomic absorption spectrometer Follow the manufacturers instructions for ig
46、niting and extinguishing the nitrous oxide-acetylene flame to avoid explosion, and ensure the safety screen is in place. Set the wavelengths for the elements to be analysed (see Table 3) and adjust the apparatus so as to obtain maximum absorbance. Fit the correct burner and, in accordance with the m
47、anufacturers instructions, light the Licensed Copy: London South Bank University, London South Bank University, Wed Oct 17 01:21:56 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-1:2007 (E) 8 flame. After 10 min preheating of the burner, adjust fuel and burner to obtain maximum absorbance while a
48、spirating the highest calibration solution. Aspirate water and set to give the zero absorbance. Aspirate the blank solution and then, alternately aspirate the calibration solutions and water to establish that the absorbance reading is not drifting and draw the calibration graph. 9.2 Inductively coup
49、led plasma spectrometer Follow the manufacturers instructions for igniting the plasma. Ensure the safety screen is in place. NOTE 1 The wavelengths in Table 3 can be used for the analysis. Depending on the analytical method and element concentration, other wavelengths can also be used. NOTE 2 It should be ensured that there is no spectral interference if other lines are used. Wait until a st