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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 725-1 : 1997 The Eu
2、ropean Standard EN 725-1 : 1997 has the status of a British Standard ICS 81.060.99 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Advanced technical ceramics Methods of test for ceramic powders Part 1. Determination of impurities in alumina BS EN 725-1 : 1997 This British Sta
3、ndard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 July 1997 BSI 1997 The following BSI references relate to the work on this standard: Committee reference RPI/13 Draft
4、for comment 93/311578 DC ISBN 0 580 27918 9 Amendments issued since publication Amd. No.DateText affected Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee RPI/13, Advanced technical ceramics, upon which the following bodie
5、s were represented: AEATechnology Aluminium Federation British Ceramic Research Ltd. British Industrial Ceramic Manufacturers Association Department of Trade and Industry (National Physical Laboratory) Flat Glass Manufacturers Association GAMBICA (BEAMA Ltd.) Institute of Refractories Engineers Mini
6、stry of Defence Refractories Association of Great Britain Society of British Aerospace Companies Ltd. University of Manchester BS EN 725-1 : 1997 BSI 1997i Contents Page Committees responsibleInside front cover National forewordii Foreword2 Text of EN 725-13 ii BSI 1997 BS EN 725-1 : 1997 National f
7、oreword This British Standard has been prepared by Technical Committee RPI/13 and is the English language version of EN 725-1 : 1997 Advanced technical ceramics Methods of test for ceramic powders Part 1: Determination of impurities in alumina, published by the European Committee for Standardization
8、 (CEN). EN 725-1 : 1997 was produced as a result of international discussions in which the United Kingdom took an active part. EN 725-1 : 1997 has been approved by CEN member bodies under the weighted voting procedures introduced in 1988 to coincide with the introduction of New Approach Directives f
9、rom the Commisssion of the European Community. Cross-references Publication referred toCorresponding British Standard ISO 3696BS 3978 : 1995 Water for analytical laboratory use Specification and test methods ISO 5725BS 5497 Precision of test methods Part 1 : 1987 Guide for the determination of repea
10、tability and reproducibility for a standard test method by inter-laboratory tests NOTE. International and European Standards as well as overseas standards, are available from Customer Services, BSI, 389 Chiswick High Road, London, W4 4AL. Compliance with a British Standard does not of itself confer
11、immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 6, an inside back cover and a back cover. CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee f
12、u r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 Copyright reserved to CEN members Ref. No. EN 725-1 : 1997 E EUROPEAN STANDARDEN 725-1 NORME EUROPE ENNE EUROPA ISCHE NORM March 1997 ICS 81.060.99 Descriptors: Ceramics, powdery materials, impurities, aluminium oxide, chemica
13、l analysis, determination of content, sodium oxides, potassium oxides, iron oxides, magnesium oxides, calcium oxides, silicon oxides, atomic absorption spectrophotometry English version Advanced technical ceramics Methods of test for ceramic powders Part1: Determination of impurities in alumina Ce r
14、amiques techniques avance es Me thodes dessai pour poudres ce ramiques Partie 1: De termination des impurete s dans lalumine Hochleistungskeramik Pru fverfahren fu r keramische Pulver Teil 1: Bestimmung von Verunreinigungen in Aluminiumoxidpulver This European Standard was approved by CEN on 1997-02
15、-24. 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
16、 on application to the Central Secretariat 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 Central Secretar
17、iat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. Page 2 EN 725-1 : 1997 BS
18、I 1997 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
19、the latest by September 1997, and conflicting national standards shall be withdrawn at the latest by September 1997. EN 725 consists of 11 parts: Part 1 : Determination of impurities in alumina Part 2 : Determination of impurities in barium titanate (ENV) Part 3 : Determination of oxygen content of
20、non-oxides by thermal extraction Part 4 : Determination of oxygen content of non-oxides by XRF analysis (ENV) Part 5 : Determination of particle size distribution Part 6 : Determination of specific area Part 7 : Determination of absolute density Part 8 : Determination of tapped bulk density Part 9 :
21、 Determination of untamped bulk density Part 10 :Determination of compaction properties Part 11 :Determination of reactivity on sintering (ENV) According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Stan
22、dard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword2 1Scope3 2Normative references3 3Principle3 4Reagents3 5Apparatus4 6Test sample4 7Decomposi
23、tion of the test sample4 8Calibration graph5 9Adjustment of the apparatus5 10Measurements6 11Expression of the results6 12Accuracy6 13Test report6 Page 3 EN 725-1 : 1997 BSI 1997 1 Scope This part of EN 725 specifies methods for the determination of elements of sodium, potassium, iron, silicon, calc
24、ium and magnesium present as impurities in alumina using atomic absorption (AAS) or inductively coupled plasma (ICP) instruments. For each element present as impurities, the methods are applicable to the following ranges, calculated as oxides: Sodium oxide20 ppm to 6000 ppm Potassium oxide20 ppm to
25、100 ppm Ferric oxide20 ppm to 300 ppm Silica50 ppm to 2000 ppm Calcium oxide20 ppm to 700 ppm Magnesium oxide5 ppm to 1000 ppm 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the app
26、ropriate places in the text and in the publications 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 publi
27、cation referred to applies. ECSC/CI 9Chemical 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 ISO 3696Water for analytical laboratory use Specification and test methods IS
28、O 5725Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests ISO/DIS 13527Chemical analysis of ferrous materials Guidelines on the use of inductively coupled plasma atomic emission spectroscopy 3 Principle The test sample is
29、decomposed by using either a fusion method or an acid dissolution method. 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 ICP (see clause 1). 4 Reag
30、ents 4.1 General During the analysis, use only reagents and calibration solutions of at least 99,99 % purity and only distilled water or water of equivalent purity (see ISO 3696). 4.2 Reagents for fusion 4.2.1 Lithium carbonate, Li2CO3 4.2.2 Potassium carbonate, K2CO3 4.2.3 Boric acid, H3BO3 4.2.4 S
31、ulfuric acid, H2SO4, (r20= 1,84 g/ml) 4.2.5 Lithium metaborate, LiBO2 4.2.6 Nitric acid, HNO3, (r20= 1,33 g/ml) 4.2.7 Phosphoric acid, H3PO4, (r20= 1,78 g/ml) 4.3 Reagents for acid dissolution 4.3.1 Sulfuric acid-phosphoric acid mixture (A) Pour 500 ml of phosphoric acid (r20= 1,78 g/ml) into 500 ml
32、 of sulfuric acid (r20= 1,84 g/ml) 4.3.2 Sulfuric acid-phosphoric acid mixture (B) Pour 700 ml of phosphoric acid (r20= 1,78 g/ml) into 300 ml of sulfuric acid (r20= 1,84 g/ml). 4.4 Reagents for calibration 4.4.1 Pure alumina, of very low and known impurity levels. 4.4.2 Sodium, commercial solution
33、or solution obtained by dissolution of pure chemical compound, concentration 1 g/l. 4.4.3 Potassium, commercial solution or solution obtained by dissolution of pure chemical compound, concentration 1 g/l. 4.4.4 Iron (ferric), commercial solution or solution obtained by dissolution of pure chemical c
34、ompound, concentration 1 g/l. 4.4.5 Silicon, commercial solution or solution obtained by dissolution of pure chemical compound, concentration 1 g/l. 4.4.6 Calcium, commercial solution or solution obtained by dissolution of pure chemical compound, concentration 1 g/l. 4.4.7 Magnesium, commercial solu
35、tion or solution obtained by dissolution of pure chemical compound, concentration 1 g/l. Page 4 EN 725-1 : 1997 BSI 1997 5 Apparatus 5.1 Platinum crucible, with a capacity of at least 50 ml. 5.2 Gold-platinum crucible, with a capacity of at least 50 ml. 5.3 Vitreous carbon crucible, with a capacity
36、of at least 50 ml with lid and heating device. 5.4 Muffle furnace, suitable for operation in the range of 1000 C to 1200 C. 5.5 Magnetic stirrer, with heating. 5.6 Atomic absorption spectrometer and/or inductively coupled plasma spectrometer, in accordance with ECSC/CI 9 or ISO 13527 respectively. 5
37、.7 Laboratory glassware. 6 Test sample Use samples of approximately : 2 g for decomposition by fusion; 1 g for decomposition by acid dissolution. Weigh them to 0,0005 g. 7 Decomposition of the test sample 7.1 General Dissolve either by a fusion method (see 7.2 to 7.4) or an acid dissolution method (
38、see 7.5 and 7.6) 7.2 Fusion 1 In a platinum crucible (see 5.1) weigh 1,5 g Li2CO3 (see 4.2.1) 5 g K2CO3(see 4.2.2) and 2,5 g H3BO3 (see 4.3.3). Add the test sample of approximately 2 g (see clause 6) and mix intimately using a platinum spatula. Place the crucible and contents into the muffle furnace
39、 (see 5.4), maintained at 1050 C50 C, for 30 min. Remove the crucible from the furnace and swirl the contents on the sides of the crucible, then allow to cool to room temperature. Dissolve the fused product in a 400 ml beaker which contains 100 ml of water and 10 ml of sulfuric acid (see 4.2.4). Pla
40、ce the beaker, covered with a watch glass, on a hot plate and heat to boiling. Maintain at boiling point to obtain a complete dissolution. Remove the beaker from the hot plate. Allow to cool. Transfer quantitatively the solution into a 200 ml volumetric flask. This procedure allows for a concentrati
41、on of alumina up to 8 g/l but if needed, a dilution to a higher volume is possible. Allow to cool to room temperature and make up to the mark. 7.3 Fusion 2 In a platinum crucible (see 5.1) weigh 4 g of LiBO2 (see 4.2.5) and 1 g of test sample. Mix intimately using a platinum spatula. Place the cruci
42、ble and contents into the muffle furnace (see 5.4) maintained at 1150 C50 C for 30 min (after the first 15 min, swirl the contents of the crucible for a few seconds). Remove the crucible from the furnace and dip its base in water at ambient temperature (this procedure allows easy removal of the bead
43、 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. Place the bead into a 400 ml beaker which contains 80 ml of water and 20 ml of nitric acid (see 4.2.6). Place the beaker, covered with a watch glass on a magne
44、tic stirrer with heating stirrer and maintain the agitation at approximately 80 C10 C until complete dissolution. Remove the beaker from the stirrer and allow to cool. Transfer quantitatively the solution into a 200 ml volumetric flask. This procedure allows for a concentration of alumina up to 8 g/
45、l but if needed, a dilution to a higher volume is possible. Allow to cool to room temperature and make up to the mark. 7.4 Fusion 3 In a gold-platinum crucible (see 5.2), weigh 2,2 g Li2CO3(see 4.2.1) and 5,5 g H3BO3(see 4.2.3). Add the test sample (see clause 6). Mix intimately using a platinum spa
46、tula. Place the crucible and contents into the muffle furnace (see 5.4), maintained at 1100 C 50 C for 30 min. Remove the crucible from the furnace and swirl the contents on the sides of the crucible, then allow to cool to room temperature. Dissolve the fused product in a 400 ml beaker which contain
47、s 100 ml of water and 20 ml of sulfuric acid (see 4.2.4). Place the beaker, covered with a watch glass, on a hot plate and heat to boiling. Maintain at boiling point to obtain complete dissolution. Remove the beaker from the hot plate. Allow to cool. Transfer quantitatively the solution into a 200 m
48、l volumetric flask. This procedure allows for a concentration of alumina up to 8 g/l, but if needed a dilution to a higher volume is possible. Allow to cool to room temperature and make up to the mark. 7.5 Acid dissolution 1 Weigh the test sample (see clause 6) into a vitreous carbon crucible (see 5
49、.3). Add carefully 15 ml of sulfuric acid-phosphoric acid mixture (see 4.3.1). Cover with a lid. Put the crucible with the lid into the heating device and maintain at boiling for 20 min. Remove the crucible from the heating device and allow to cool to room temperature. Transfer quantitatively the contents into a 100 ml volumetric 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. 7.6 Acid dissolution 2 Weigh the
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