1、BSI Standards PublicationBS ISO 15901-1:2016Evaluation of pore sizedistribution and porosity ofsolid materials by mercuryporosimetry and gasadsorptionPart 1: Mercury porosimetryBS ISO 15901-1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 15901-1:2016. It
2、 supersedes BS ISO 15901-1:2005 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee LBI/37, Particle characterization including sieving.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does
3、not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 81558 4 ICS 19.120 Compliance with a British Standard cannot confer immunity from legal o
4、bligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 15901-1:2016 ISO 2016Evaluation of pore size distribution and porosity of solid material
5、s by mercury porosimetry and gas adsorption Part 1: Mercury porosimetryEvaluation de la distribution de taille des pores et la porosit des matriaux solides par porosimtrie mercure et ladsorption des gaz Partie 1: Porosimtrie mercureINTERNATIONAL STANDARDISO15901-1Second edition2016-04-01Reference nu
6、mberISO 15901-1:2016(E)BS ISO 15901-1:2016ISO 15901-1:2016(E)ii ISO 2016 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2016, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means,
7、 electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 V
8、ernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 15901-1:2016ISO 15901-1:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms . 45 Principles . 56 Apparatus and material 66.1
9、 Sample holder 66.2 Porosimeter . 76.3 Mercury . 77 Procedures for calibration and performance 77.1 General . 77.2 Pressure signal calibration . 77.3 Volume signal calibration 77.4 Vacuum transducer calibration 77.5 Verification of porosimeter performance 88 Procedures 88.1 Sampling . 88.1.1 Obtaini
10、ng a test sample 88.1.2 Quantity of sample . 88.2 Method . 98.2.1 Sample pre-treatment . 98.2.2 Filling of the sample holder and evacuation 98.2.3 Filling the sample holder with mercury 98.2.4 Measurement . 108.2.5 Completion of test 108.2.6 Blank and sample compression correction 109 Evaluation .11
11、9.1 Determination of the pore size distribution . 119.2 Determination of the specific pore volume . 119.3 Determination of the specific surface area 129.4 Determination of the bulk and skeleton densities 129.5 Determination of the porosity 1310 Reporting .13Annex A (informative) Mercury porosimetry
12、analysis results .14Annex B (informative) Recommendations for the safe handling of mercury .17Bibliography .19 ISO 2016 All rights reserved iiiContents PageBS ISO 15901-1:2016ISO 15901-1:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national sta
13、ndards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International or
14、ganizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for it
15、s further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/di
16、rectives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in t
17、he Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions relat
18、ed to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.The committee responsible for this document is ISO/TC 24, Particle characterization
19、including sieving, Subcommittee SC 4, Particle characterization.This second edition cancels and replaces the first edition (ISO 15901-1:2005), which has been technically revised. It also incorporates the Corrigendum ISO 15901-1:2005/Cor 1:2007.ISO 15901 consists of the following parts, under the gen
20、eral title Evaluation of pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption: Part 1: Mercury porosimetry Part 2: Analysis of mesopores and macropores by gas adsorption Part 3: Analysis of micropores by gas adsorptioniv ISO 2016 All rights reservedBS ISO
21、15901-1:2016ISO 15901-1:2016(E)IntroductionIn general, different pores (micro-, meso-, and macropores) may be pictured as either apertures, channels or cavities within a solid body or as space (i.e. interstices or voids) between solid particles in a bed, compact or aggregate. Porosity is a term whic
22、h is often used to indicate the porous nature of solid material and in this International Standard is more precisely defined as the ratio of the total pore volume of the accessible pores and voids to the volume of the particulate agglomerate. In addition to the accessible pores, a solid may contain
23、closed pores which are isolated from the external surface and into which fluids are not able to penetrate. The characterization of closed pores is not covered in this International Standard.Porous materials may take the form of fine or coarse powders, compacts, extrudates, sheets or monoliths. Their
24、 characterization usually involves the determination of the pore size distribution as well as the total accessible pore volume or porosity. For some purposes it is also necessary to study the pore shape and interconnectivity and to determine the internal and external specific surface area.Porous mat
25、erials have great technological importance, for example in the context of the following: controlled drug release; catalysis; gas separation; filtration including sterilization; materials technology; environmental protection and pollution control; natural reservoir rocks; building materials; polymers
26、 and ceramic.It is well established that the performance of a porous solid (e.g. its strength, reactivity, permeability) is dependent on its pore structure. Many different methods have been developed for the characterization of pore structure. In view of the complexity of most porous solids, it is n
27、ot surprising that the results obtained are not always in agreement and that no single technique can be relied upon to provide a complete picture of the pore structure. The choice of the most appropriate method depends on the application of the porous solid, its chemical and physical nature and the
28、range of pore size.The most commonly used methods are as follows:a) Mercury porosimetry, where the pores are filled with mercury under pressure. This method is suitable for many materials with pores in the approximate diameter range of 0,004 m to 400 m.b) Meso- and macropore analysis by gas adsorpti
29、on, where the pores are characterized by adsorbing a gas, such as nitrogen at liquid nitrogen temperature. The method is used for pores in the approximate diameter range of 0,002 m to 0,1 m (2 nm to 100 nm).c) Micropore analysis by gas adsorption, where the pores are characterized by adsorbing a gas
30、, such as nitrogen at liquid nitrogen temperature. The method is used for pores in the approximate diameter range of 0,4 nm to 2 nm. ISO 2016 All rights reserved vBS ISO 15901-1:2016BS ISO 15901-1:2016Evaluation of pore size distribution and porosity of solid materials by mercury porosimetry and gas
31、 adsorption Part 1: Mercury porosimetryWARNING The use of this International Standard may involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this In
32、ternational Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.1 ScopeThis International Standard describes a method for the evaluation of the pore size distribution and the specific surface area of pores in solids by
33、mercury porosimetry according to the method of Ritter and Drake12. It is a comparative test, usually destructive due to mercury contamination, in which the volume of mercury penetrating a pore or void is determined as a function of an applied hydrostatic pressure, which can be related to a pore diam
34、eter.Practical considerations presently limit the maximum applied absolute pressure to about 400 MPa (60 000 psi) corresponding to a minimum equivalent pore diameter of approximately 4 nm. The maximum diameter is limited for samples having a significant depth due to the difference in hydrostatic hea
35、d of mercury from the top to the bottom of the sample. For the most purposes, this limit can be regarded as 400 m. The measurements cover inter-particle and intra-particle porosity. In general, without additional information from other methods it is difficult to distinguish between these porosities
36、where they co-exist. The method is suitable for the study of most porous materials non-wettable by mercury. Samples that amalgamate with mercury, such as certain metals, e.g. gold, aluminium, copper, nickel and silver, can be unsuitable with this technique or can require a preliminary passivation. U
37、nder the applied pressure some materials are deformed, compacted or destroyed, whereby open pores may be collapsed and closed pores opened. In some cases it may be possible to apply sample compressibility corrections and useful comparative data may still be obtainable. For these reasons, the mercury
38、 porosimetry technique is considered to be comparative.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest e
39、dition of the referenced document (including any amendments) applies.ISO 3165, Sampling of chemical products for industrial use Safety in samplingISO 14488, Particulate materials Sampling and sample splitting for the determination of particulate properties3 Terms and definitionsFor the purposes of t
40、his document, the following terms and definitions apply.3.1porosimeterinstrument for measuring pore volume and pore size distributionINTERNATIONAL STANDARD ISO 15901-1:2016(E) ISO 2016 All rights reserved 1BS ISO 15901-1:2016ISO 15901-1:2016(E)3.2porosimetrymethods for the estimation of pore volume,
41、 pore size distribution, and porosity3.3porous solidsolid with cavities or channels which are deeper than they are wide3.4powderporous or nonporous solid composed of discrete particles with maximum dimension less than about 1 mm, powders with a particle size below about 1 m are often referred to as
42、fine powders3.5porecavity or channel which is deeper than it is wide, otherwise it is part of the materials roughness3.6voidintersticespace between particles, i.e. interparticle pore3.7macroporepore of internal width greater than 50 nm3.8mesoporepore of internal width between 2 nm and 50 nm3.9microp
43、orepore of internal width less than 2 nm3.10closed porepore totally enclosed by its walls and hence not interconnecting with other pores and not accessible to fluids3.11open porepore not totally enclosed by its walls and open to the surface either directly or by interconnecting with other pores and
44、therefore accessible to fluid3.12ink bottle porenarrow necked open pore3.13pore sizeinternal pore width (for example, the diameter of a cylindrical pore or the distance between the opposite walls of a slit) which is a representative value of various sizes of vacant space inside a porous material3.14
45、pore volumevolume of open pores unless otherwise stated2 ISO 2016 All rights reservedBS ISO 15901-1:2016ISO 15901-1:2016(E)3.15pore diameterdiameter of a pore in a model in which the pores typically are assumed to be cylindrical in shape and which is calculated from data obtained by a specified proc
46、edure3.16median pore diameterdiameter that corresponds to the 50th percentile of pore volume, i.e. the diameter for which one half of the pore volume is found to be in larger pores and one half is found to be in smaller pores3.17modal pore diameter modepore diameter of the maximum in a differential
47、pore size distribution curve3.18hydraulic pore diameteraverage pore diameter, calculated as the ratio of pore volume multiplied by four to pore area.3.19bulk volumevolume of powder or solids, including all pores (open and closed) and interstitial spaces between particles.3.20bulk densityratio of sam
48、ple mass to bulk volume3.21skeleton volumevolume of the sample including the volume of closed pores (if present) but excluding the volumes of open pores as well as that of void spaces between particles within the bulk sampleSOURCE: ISO 121543.22skeleton densityratio of sample mass to skeleton volume
49、3.23apparent volumetotal volume of the solid constituents of the sample including closed pores and pores inaccessible or not detectable by the stated method;3.24apparent densityratio of sample mass to apparent volume3.25envelope volumetotal volume of the particle, including closed and open pores, but excluding void space between the individual particles3.26envelope densityratio of sample mass to envelope volume3.27porosityratio of the volume of the accessible pores and voids to the bulk volume occupied by an amount of the
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