www bzfxw com BRITISH STANDARD BS EN 623 2 1993 Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2 Determination of density and porosity The European Standard[.]
BRITISH STANDARD Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2: Determination of density and porosity The European Standard EN 623-2:1993 has the status of a British Standard UDC 666.5/.6:620-1:531.75 BS EN 623-2:1993 BS EN 623-2:1993 Cooperating organizations The European Committee for Standardization (CEN), under whose supervision this European Standard was prepared, comprises the national standards organizations of the following countries: Austria Belgium Denmark Finland France Germany Greece Iceland Ireland Italy Luxembourg Netherlands Norway Portugal Spain Sweden Switzerland United Kingdom This British Standard, having been prepared under the direction of the Refractory Products Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 November 1993 © BSI 10-1999 The following BSI references relate to the work on this standard: Committee reference RPM/13 Draft for comment 92/36001 DC ISBN 580 21772 Oesterreichisches Normungsinstitut Institut belge de normalisation Dansk Standardiseringsraad Suomen Standardisoimisliito, r.y Association franỗaise de normalisation Deutsches Institut für Normung e.V Hellenic Organization for Standardization Technological Institute of Iceland National Standards Authority of Ireland Ente Nazionale Italiano di Unificazione Inspection du Travail et des Mines Nederlands Normalisatie-instituut Norges Standardiseringsforbund Instituto Portugs da Qualidade Asociación Espola de Normalización y Certificación Standardiseringskommissionen i Sverige Association suisse de normalisation British Standards Institution Amendments issued since publication Amd No Date Comments BS EN 623-2:1993 Contents Cooperating organizations National foreword Foreword Text of EN 623-2 National annex NA (informative) Committees responsible National annex NB (informative) Cross-references © BSI 10-1999 Page Inside front cover ii Inside back cover Inside back cover i BS EN 623-2:1993 National foreword This British Standard has been prepared under the direction of the Refractory Products Standards Policy Committee and is the English language version of EN 623-2 Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2: Determination of density and porosity published by the European Committee for Standardization (CEN) It supersedes BS 7134-1.2:1989 which is withdrawn EN 623-2 was produced as a result of international discussions in which the UK took an active part 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 Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages to 8, an inside back cover and a back cover This standard has been updated (see copyright date) and may have had amendments incorporated This will be indicated in the amendment table on the inside front cover ii © BSI 10-1999 EUROPEAN STANDARD EN 623-2 NORME EUROPÉENNE September 1993 EUROPÄISCHE NORM UDC 666.5/.6:620.1:531.75 Descriptors: Ceramics, characteristics, tests, determination, bulk density, porosity, quality English version Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 2: Determination of density and porosity Céramiques techniques avancées — Céramiques monolithiques — Propriétés générales et structurales — Partie 2: Détermination de la masse volumique et de la porosité Hochleistungskeramik — Monolithische Keramik — Allgemeine und strukturelle Eigenschaften — Teil 2: Bestimmung von Dichte und Porosität ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ This European Standard was approved by CEN on 1993-08-30 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 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 Secretariat 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 CEN European Committee for Standardization Comité Européen de Normalisation Europäisches Komitee für Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels © 1993 Copyright reserved to CEN members Ref No EN 623-2:1993 E EN 623-2:1993 Foreword This European Standard has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by BSI EN 623 Advanced technical ceramics — Monolithic ceramics — General and textural properties consists of four Parts: — Part 1: Determination of the presence of defects by dye penetration tests; — Part 2: Determination of density and porosity; — Part 3: Determination of grain size1); — Part 4: Determination of surface roughness1) The 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 1994, and conflicting national standards shall be withdrawn at the latest by March 1994 In accordance with the CEN/CENELEC Internal Regulations, the following countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom 1) Contents Foreword Scope Normative references Definitions Statement of accuracy and errors The evacuation method (Method 1) Method by measurement of dimensions and mass (geometric bulk density) (Method 2) Test report Table — Accuracy and errors of density and porosity measurement Table — Density of distilled water as a function of temperature between 15 °C and 30 °C Page 3 3 ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ Parts and of this European Standard will be published as ENV © BSI 10-1999 EN 623-2:1993 Scope Definitions This Part of EN 623 describes methods for determination of the bulk density, apparent solid density, and apparent porosity of advanced technical ceramics Two methods are described and are designated as Methods and 2, as follows Method Determination of bulk density, apparent solid density and apparent porosity by the evacuation method For the purposes of this Part of EN 623 the following definitions apply NOTE This method is not suitable for the determination of apparent porosity of less than % A method for determining the presence of defects and surface porosity in this type of material is given in EN 623-1 NOTE The method is also not suitable for materials which are known to have an average pore size of greater than 200 Èm Method Determination of bulk density only, by measurement of dimensions and mass NOTE Neither of these test methods measures total porosity including open and closed pores This parameter may be calculated from the test results of Method if the true density of pore-free material is known Normative references pores that are penetrated by an immersion liquid in vacuum, or that are connected with the atmosphere, either directly or via one another 3.2 closed pores pores that are not penetrated by the immersion liquid, or that are not connected with the atmosphere 3.3 bulk volume Vb the sum of the volumes of the solid material, the open pores and the closed pores in a porous body 3.4 true volume the volume of a body occupied by solid material, excluding all forms of porosity ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 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 EN 623-1, Advanced technical ceramics — Monolithic ceramics — General and textural properties — Part 1: Determination of the presence of defects by dye penetration tests EN 45001, General criteria for the operation of testing laboratories EN 1006, Advanced technical ceramics — Methods of testing monolithic ceramics — Guidance on the sampling and selection of test pieces ISO 758:1976, Liquid chemical products for industrial use — Determination of density at 20 °C ISO 3611:1978, Micrometer callipers for external measurement ISO 4964:1984, Steel — Hardness conversions ISO 6906:1984, Vernier callipers reading to 0,02 mm © BSI 10-1999 3.1 open pores 3.5 apparent solid volume Vs the sum of the volume of the closed pores and true volume 3.6 bulk density Ôb the ratio of the mass of the dry material of a porous body to its bulk volume 3.7 geometric bulk density the mass per unit total volume of a material including all porosity accessible and in accessible from the surface, the volume being calculated from linear dimensions 3.8 apparent solid density Ôs the ratio of the mass of the dry material to its apparent solid volume 3.9 apparent porosity Ïa the ratio of the total volume of the open pores in a porous body to its bulk volume Statement of accuracy and errors The minimum accuracy of measurement of the parameters used in calculation of densities and porosities is given in Table EN 623-2:1993 Table — Accuracy and errors of density and porosity measurement Method 1: Evacuation method (see clause 5) Method 2: Geometric bulk density (see clause 6) Minimum test piece dimension in mm — 3,0 Accuracy of measurement of dimensiona — 0,01 mm or 0,05 % of smallest dimension Minimum test piece mass in g 30 2,0 Accuracy of weighing in g 0,0001 0,001 0,01 0,001 Accuracy of measurement of density of 0,0001 immersion liquid, (Mg/m3); see 5.5 and Table 0,001 0,001 — Accuracy of density measurement (%) 0,3 a 1,0 The maximum non-uniformity of any dimension should not exceed % of its average value The evacuation method (Method 1) 5.1 Principle The mass of dry test piece is determined by weighing, then its apparent mass when immersed in a liquid with which it has been impregnated under vacuum, and then its mass in air while still soaked with the liquid From these values its bulk density and apparent porosity are determined by calculation NOTE Some materials may chemically react with water, others such as boron nitride are not wetted by water Where test pieces of smaller volume (1 cm3 to 10 cm3) (see 5.3.1) are used, and the error caused by evaporation of liquids is comparatively high, dibutyl phthalate should be used 5.2.8 Thermometer, capable of measuring to ± 0,1 K 5.2.9 Glass beaker, of a size allowing adequate clearance of its walls by the test piece 5.2.10 Desiccator, for storage of test pieces ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ 5.2.11 Manometer 5.2 Apparatus 5.2.12 Absorbent cloth or tissue paper 5.2.1 Drying oven, capable of maintaining a temperature of 110 °C ± °C 5.2.2 Balance with accuracy in accordance with clause 5.2.3 A bridge, to be placed over the load-bearing scale pan of the balance (see 5.2.2), if the balance is not equipped for suspension loading 5.2.4 Evacuating equipment, capable of reducing the pressure to a value less than 500 Pa (25 mbar), and a means of measuring the pressure used 5.3 Test pieces NOTE If a rotary vacuum pump is used, it should be fitted with a moisture trap, to minimize the mixing of water and the pump lubrication system 5.2.5 Degreased metal wire, of diameter not more than 0,15 mm 5.2.6 Cradle to contain test piece(s) (optional) 5.2.7 Immersion liquid, which may be either: a) cold distilled water, containing a dilute solution of a surface active agent (concentration not more than 0,01 %), the addition of which does not change the densities given in Table 2; or b) an organic liquid, which shall be used for materials that are sensitive to contact with water or that cannot be fully wetted by water 5.3.1 Materials for testing shall be sampled in accordance with the guidance given in ENV 1006 Test pieces shall be either whole or broken ceramic products, or shall be cut from blocks or rods of the same material The bulk volume of a test piece shall be not less than cm3, and its mass shall be greater than g (see Table and note 2) NOTE When the apparent porosity is greater than 10 %, the ratio of the longest to the shortest dimension of a test piece should not exceed : NOTE For test pieces of mass g to g, significant sources of error include temperature, air content of liquid and the consistency of the liquid level position on the suspension wire These factors should be kept constant 5.3.2 If any surface treatment such as the removal of “skin” is carried out this shall be reported in the test report (see clause 7) NOTE Since it is necessary to sponge the surface of the test piece to remove surface moisture, the test pieces should not have inaccessible external surfaces or very rough surfaces 5.4 Procedure 5.4.1 Determination of the mass of the dry test piece Dry the test piece in the oven (see 5.2.1) at 110 °C ± °C to constant mass, i.e until two successive weighings made before and after at least h in the drying oven not differ by more than 0,03 % © BSI 10-1999 EN 623-2:1993 Before each weighing, place the test piece in the desiccator (see 5.2.10), until it has cooled to room temperature, and weigh it as quickly as possible after removal from the desiccator The mass thus determined is the mass of the dry test piece (m1), weighed in accordance with Table 5.4.2 Soaking of test piece Place the cooled and dried test piece in an airtight vessel Seal the vessel and evacuate it until a pressure of less than 500 Pa is attained; maintain this vacuum for at least 15 In order to ensure that all the air has been removed from the test piece, isolate or disconnect the vessel from the vacuum pump and use the manometer (see 5.2.11) to check that the pressure does not rise through any degassing of the test piece Progressively introduce the immersion liquid in such a way that, after min, the test piece is covered by about 20 mm of liquid Reconnect the vessel to the vacuum pump and maintain this reduced pressure for 30 min, then switch off the pump and open the vessel to ambient air pressure Wait for at least a further 30 to ensure complete penetration of the test piece by the liquid NOTE If such loss occurs, the test should be repeated using a different immersion liquid (see note to 5.2.7) Record the mass thus determined as the mass of the soaked test piece (m3), weighed in accordance with Table Repeat the immersion, drying and weighing If the results for each test piece differ by more than the relevant accuracy figures given in Table 1, repeat the test until two sets of figures meet these criteria 5.5 Determination of the density of the immersion liquid Determine the density of the liquid used in the operation at the temperature of the test, using the method given in ISO 758:1976, to the accuracy given in Table NOTE For distilled water, the density at various temperatures is given in Table NOTE As many organic solvents have high coefficients of volume thermal expansion, the determination of density of the liquid should be carried out at the same temperature as that of the measurement of the apparent mass of the immersed test piece (see 5.4.3) Table — Density of distilled water as a function of temperature between 15 °C and 30 °C ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ NOTE If there is any doubt about the completion of penetration within 30 min, this period may be extended by agreement between parties as required 5.4.3 Determination of the apparent mass of the immersed test piece Suspend the test piece by the thin wire (see 5.2.5) from the load-pan suspension point of the balance, perpendicular to the liquid, and weigh it while completely immersed in a quantity of the immersion liquid, contained in the beaker (see 5.2.9), standing on the bridge (see 5.2.3) if used Remove bubbles from the surface of the test piece and weigh Remove the test piece from the suspension wire, replace the wire in the liquid to the same suspension level and weigh The difference between the two weighings is the apparent mass of the immersed test piece (m2), weighed in accordance with Table Determine the temperature of the immersion liquid, using the thermometer (see 5.2.8) 5.4.4 Determination of the mass of the soaked test piece Remove the test piece from the liquid and, without waiting, sponge it quickly and carefully with a damp, lint-free absorbent cloth or tissue (see 5.2.12) to remove droplets and the surface film of liquid, but avoid drawing out liquid from the pores of the test piece Immediately weigh the test piece in air Take care to ensure that evaporation of the immersion liquid does not lead to any appreciable loss in mass during the weighing operation © BSI 10-1999 Temperature, °C 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 Density, Ô Mg/m3 0,99910 0,99894 0,99877 0,99860 0,99841 0,99820 0,99799 0,99777 0,99754 0,99730 0,99704 0,99678 0,99651 0,99623 0,99594 0,99565 Kg/m3 999,10 998,94 998,77 998,60 998,41 998,20 997,99 997,77 997,54 997,30 997,04 996,78 996,51 996,23 995,94 995,65 5.6 Calculation of results 5.6.1 Calculate the bulk density Ôb, in either megagrams per cubic metre or kilograms per cubic metre from the following equation: (1) EN 623-2:1993 5.6.2 Calculate the apparent solid density Ôs, in either megagrams per cubic metre or kilograms per cubic metre (2) 5.6.3 Calculate the apparent porosity Ïa as a percentage, (V/V) from the following equation: (3) where: m1 is the mass of the dry test piece in grams (see 5.4.1); m2 is the apparent mass of the immersed test piece in grams (see 5.4.3); m3 is the mass of the soaked test piece in grams (see 5.4.4); ÔL is the density of the immersion liquid (see 5.5) in megagrams per cubic metre or kilograms per cubic metre, as appropriate to the units chosen for the calculation Express the values of density in megagrams per cubic metre or kilograms per cubic metre to three significant digits Express the values of porosity to the nearest 0,1 % Method by measurement of dimensions and mass (geometric bulk density) (Method 2) 6.1 Principle A test piece of uniform geometry within specified tolerances is dried and weighed Its volume is determined by measurement of the appropriate dimensions The geometric bulk density (see 3.7) is calculated as mass per unit volume 6.2 Apparatus 6.2.1 Balance, with accuracy in accordance with Table 6.2.2 Calibrated measuring device capable of repeatable and accurate measurement in accordance with Table 1, e.g vernier callipers in accordance with ISO 6906:1984, or a micrometer in accordance with ISO 3611:1978 NOTE For flat test piece surfaces, spherical measuring anvils with radii of curvature between mm and 10 mm should be used For cylindrical test piece surfaces, cylindrical measuring anvils should be used These anvils should be constructed of material with hardness of at least 500 HV30 (see ISO 4964:1984) 6.2.3 Drying oven, capable of maintaining a temperature of 110 °C ± °C 6.2.4 Desiccator, for storage of test pieces 6.3 Test pieces Materials for testing shall be sampled in accordance with the guidance given in ENV 1006 The shape of test pieces shall be such that the volume can be calculated from the external dimensions NOTE Ideal shapes are rectangular parallelepipeds and right cylinders, discs or rods NOTE Test pieces which not have uniform dimensions and principal axes orthogonal to within 1° should be ground to achieve such conditions The mass of the test piece shall be greater than g and each dimension shall be greater than mm (see Table 1) Where “as-fired” test pieces are used, press flashing shall be removed NOTE The total volume of edge chips and surface pits or protrusions should not exceed approximately 0,1 % of the nominal total volume NOTE Some types of material possess surface skins which are rough or soft in the “as-fired” state These materials are unsuited to this method of measurement of bulk density unless the skin is flattened or removed by machining or other suitable method Reaction-bonded silicon nitride is an example where such a surface deposit may be present 6.4 Procedure Dry the test pieces in the oven (see 6.2.3) at 110 °C ± °C to constant mass, i.e until two successive weighings made before and after at least h in the drying oven not differ by more than 0,03 % Transfer them to a desiccator and allow to cool to room temperature Record the mass of each test piece in ambient air, as soon as possible after removal from the desiccator Using the selected measuring device (see 6.2.2), measure the dimensions of each test piece at at least three positions for each direction, to an accuracy better than 0,01 mm or 0,05 % of the smallest dimension Measure the directions parallel to the principal geometric axes, e.g the length, breadth and depth of a parallelepiped, the length and diameter for a disc or a rod ｗｗｗ．ｂｚｆｘｗ．ｃｏｍ NOTE If the dimensions of the test piece are too small to make three separate measurements in any direction, e.g of the length of a rod of small diameter, a single measurement may be used, such a simplified procedure being reported [see clause 7j)] Calculate the differences between the lowest and highest figures measured for each direction Reject the test pieces if any difference exceeds % of the mean dimensions measured 6.5 Results Calculate the geometric volume of each test piece from its mean dimensions The geometric bulk density is given by the mass divided by the geometrical volume Express the values of density in megagrams per cubic metre or kilograms per cubic metre © BSI 10-1999 EN 623-2:1993 Test report The results shall be reported in accordance with EN 45001 and the test report shall include the following information: a) the name of the testing establishment; b) the date of the test; a unique identification of the report and of each page, and the name and address of the customer, and a signatory of the report; c) a reference to this European standard, i.e “Determined in accordance with EN 623-2 and the method used, i.e Method or Method (see clause 1); d) the identification of the test material or component type (manufacturer, type, batch number); e) the number of test pieces; © BSI 10-1999 f) the shape and surface condition of the test pieces, and whether surfaces are as-fired or machined (see 5.3.2 and 6.3); g) for Method 1, the pressure to which the vacuum chamber was reduced; h) for Method 1, the immersion liquid used, and the temperature of the test; i) for Method 1, the time taken to complete the soaking of the test piece (see 5.4.2); j) for Method 2, any use of the simplified measurement procedure (see 6.4); k) the individual values and the mean value (where required) of the bulk density and apparent solid density expressed in either megagrams per cubic metre or kilograms per cubic metre, and the apparent porosity expressed as a percentage; l) comments on the test or test results blank BS EN 623-2:1993 National annex NA (informative) Committees responsible The United Kingdom participation in the preparation of this European Standard was entrusted by the Refractory Products Standards Policy Committee (RPM/-) to Technical Committee RPM/13, upon which the following bodies were represented: AEA Technology 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 Ministry of Defence Refractories Association of Great Britain Society of British Aerospace Companies Limited University of Manchester National annex NB (informative) Cross-references Publication referred to Corresponding British Standard EN 45001:1989 BS 7501:1989 General criteria for the operation of testing laboratories ISO 758:1976 BS 4522:1988 Method for determination of absolute density at 20 °C of liquid chemical products for industrial use © BSI 10-1999 BS EN 623-2:1993 BSI — British Standards Institution BSI is the independent national body responsible for preparing British Standards It presents the UK view on standards in Europe and at the international level It is incorporated by Royal Charter Revisions British Standards are updated by amendment or revision Users of British Standards should make sure that they possess the latest amendments or editions It is the constant aim of BSI to improve the quality of our products and services We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover Tel: 020 8996 9000 Fax: 020 8996 7400 BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services Tel: 020 8996 9001 Fax: 020 8996 7001 In response to orders for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requested Information on standards BSI provides a wide range of information on national, European and international standards through its Library and its Technical Help to Exporters Service Various BSI electronic information services are also available which give details on all its products and services Contact the Information Centre Tel: 020 8996 7111 Fax: 020 8996 7048 Subscribing members of BSI are kept up to date with standards developments and receive substantial discounts on the purchase price of standards For details of these and other benefits contact Membership Administration Tel: 020 8996 7002 Fax: 020 8996 7001 Copyright Copyright subsists in all BSI publications BSI also holds the copyright, in the UK, of the publications of the international standardization bodies Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means – electronic, photocopying, recording or otherwise – without prior written permission from BSI This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations If these details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained BSI 389 Chiswick High Road London W4 4AL If permission is granted, the terms may include royalty payments or a licensing agreement Details and advice can be obtained from the Copyright Manager Tel: 020 8996 7070