《ISO-15901-1-2005.pdf》由会员分享，可在线阅读，更多相关《ISO-15901-1-2005.pdf（26页珍藏版）》请在三一文库上搜索。
1、 Reference number ISO 15901-1:2005(E) ISO 2005 INTERNATIONAL STANDARD ISO 15901-1 First edition 2005-12-15 Evaluation of pore size distribution and porosimetry of solid materials by mercury porosimetry and gas adsorption Part 1: Mercury porosimetry Distribution des dimensions des pores et porosimtri
2、e des matriaux solides par porosimtrie au mercure et par adsorption de gaz Partie 1: Porosimtrie au mercure ISO 15901-1:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless t
3、he typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of
4、Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the
5、 unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2005 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, includi
6、ng photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published
7、 in Switzerland ii ISO 2005 All rights reserved ISO 15901-1:2005(E) ISO 2005 All rights reserved iii Contents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 2 4 Symbols. 4 5 Principles. 4 6 Apparatus and material 5 7 Procedures for calibration and perf
8、ormance. 5 8 Procedures 6 9 Evaluation 9 10 Reporting. 10 Annex A (informative) Mercury porosimetry analysis results for alumina reference sample 12 Bibliography. 18 ISO 15901-1:2005(E) iv ISO 2005 All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide f
9、ederation of national standards 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 co
10、mmittee. International organizations, 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. International Standards are drafted in accor
11、dance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requir
12、es approval by at least 75 % of the member bodies casting a vote. 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. ISO 15901-1 was prepared by Technic
13、al Committee ISO/TC 24, Sieves, sieving and other sizing methods, Subcommittee SC 4, Sizing by methods other than sieving. ISO 15901 consists of the following parts, under the general title Evaluation of pore size distribution and porosimetry of solid materials by mercury porosimetry and gas adsorpt
14、ion: Part 1: Mercury porosimetry Part 2: Analysis of mesopores and macropores by gas adsorption Part 3: Analysis of micropores by gas adsorption ISO 15901-1:2005(E) ISO 2005 All rights reserved v Introduction In general, different pores (micro-, meso-, and macropores) can be pictured as either apert
15、ures, 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 which is often used to indicate the porous nature of solid material and is more precisely defined as the ratio of the volume of the access
16、ible pores and voids to the total volume occupied by a given amount of the solid. In addition to the accessible pores, a solid can contain 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
17、 this International Standard. Porous materials can take the form of fine or coarse powders, compacts, extrudates, sheets or monoliths. Their characterization usually involves the determination of the pore size distribution as well as the total pore volume or porosity. For some purposes, it is also n
18、ecessary to study the pore shape and interconnectivity and to determine the internal and external specific surface area. Porous materials have great technological importance, for example in the context of the following: controlled drug release; catalysis; gas separation; filtration including sterili
19、zation; materials technology; environmental protection and pollution control; natural reservoir rocks; building materials properties; polymers and ceramic. It is well established that the performance of a porous solid (e.g. its strength, reactivity, permeability of adsorbent power) is dependent on i
20、ts 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 not surprising that the results obtained are not always in agreement and that no single technique can be relied upon to provide a complete
21、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 range of pore size. The most commonly used methods are as follows: a) mercury porosimetry, where the pores are filled with mercury under p
22、ressure; this method is suitable for many materials with pores in the appropriate diameter of 0,003 m to 400 m; b) meso- and macropore analysis by gas adsorption, where the pores are characterized by adsorbing a gas, such as nitrogen, at liquid nitrogen temperature; the method is used for pores in t
23、he approximate diameter range of 0,002 m to 0,1 m (2,0 nm to 100 nm), and is an extension of the surface area estimation technique; c) micropore analysis by gas adsorption, where the pores are characterized by adsorbing a gas, such as nitrogen, at liquid nitrogen temperature; the method is used for
24、pores in the approximate diameter range of 0,4 nm to 2,0 nm, and is an extension of the surface area estimation technique. -,-,- -,-,- INTERNATIONAL STANDARD ISO 15901-1:2005(E) ISO 2005 All rights reserved 1 Evaluation of pore size distribution and porosimetry of solid materials by mercury porosime
25、try and gas adsorption Part 1: Mercury porosimetry WARNING 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 use
26、r of this International Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope This International Standard describes a method for the evaluation of the pore size distribution and the specific surface in pores of s
27、olids by mercury porosimetry according to the method of Ritter and Drake 1, 2. 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
28、 a pore diameter. Practical considerations presently limit the maximum applied absolute pressure to about 400 MPa (60 000 psia) corresponding to a minimum equivalent pore diameter of approximately 0,003 m. The maximum diameter will be limited for samples having a significant depth due to the differe
29、nce in hydrostatic head 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 interparticle and intraparticle porosity. In general, it cannot distinguish between these porosities where they co-exist. The method is suit
30、able for the study of most non-wettable, by mercury, porous materials. Samples that amalgamate with mercury, such as certain metals, e.g. gold, aluminium, reduced copper, reduced nickel and silver, can be unsuitable for this technique or can require a preliminary passivation. Under the applied press
31、ure, some materials are deformed, compacted or destroyed, whereby open pores can be collapsed and closed pores opened. In some cases, it is possible to apply sample compressibility corrections and useful comparative data can still be obtained. For these reasons, the mercury porosimetry technique is
32、considered to be comparative. 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 latest edition of the referenced document (including any amendments) appli
33、es. ISO 3165, Sampling of chemical products for industrial use Safety in sampling ISO 8213, Chemical products for industrial use Sampling techniques Solid chemical products in the form of particles varying from powders to coarse lumps M 024 4/85, Quecksilber und seine Verbindungen. Merkblatt der Ber
34、ufsgenossenschaft der chemischen Industrie, Postfach 101480, D-69004 Heidelberg, Germany ISO 15901-1:2005(E) 2 ISO 2005 All rights reserved 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 bulk density powder density under defined conditions 3
35、.2 blind pore dead-end-pore open pore having a single connection with an external surface 3.3 closed pore cavity not connected to the external surface NOTE Closed pores are not covered in this International standard. 3.4 contact angle angle that a non-wetting liquid makes with a solid material 3.5 e
36、xternal surface area area of external surface including roughness but outside pores 3.6 ink bottle pore narrow necked open pore 3.7 interconnected pore pore which communicates with one or more other pores 3.8 internal surface area area of internal pore walls 3.9 intraparticle porosity ratio of the v
37、olume of open pores internal to the particle to the total volume occupied by the solid 3.10 interparticle porosity ratio of the volume of space between particles in a powder to the apparent volume of the particles or powder 3.11 macropore pore of internal width greater than 50 nm 3.12 mesopore pore
38、of internal width between 2 nm and 50 nm 3.13 micropore pore of internal width less than 2 nm which is accessible for a molecule to be adsorbed ISO 15901-1:2005(E) ISO 2005 All rights reserved 3 3.14 open pore cavity or channel with access to an external surface 3.15 open porosity ratio of the volum
39、e of open pores and voids to the total volume occupied by the solid 3.16 pore size pore width (for example, the diameter of a cylindrical pore or the distance between the opposite walls of a slit) that is a representative value of various sizes of the vacant space inside a porous material NOTE One o
40、f the methods to determine pore sizes is by mercury porosimetry. 3.17 pore volume volume of pores determined by stated method 3.18 porosimeter instrument for measuring porosity and pore size distribution 3.19 porosimetry methods for the estimation of porosity and pore size distribution 3.20 porosity
41、 ratio of total pore volume to apparent volume of particle or powder 3.21 porous solid solid with cavities or channels which are deeper than they are wide 3.22 skeletal density mass of a powder divided by the total volume of the sample, including closed pores but excluding open pores 3.23 apparent d
42、ensity mass of a powder divided by the total volume of the sample, including closed and inaccessible pores, as determined by the stated method 3.24 powder density mass of a powder divided by its apparent volume, which is taken to be the total volume of the solid material, open and closed pores and i
43、nterstices 3.25 surface area extent of available surface area as determined by given method under stated conditions 3.26 surface tension force required to separate a film of liquid from either a solid material or a film of the same liquid -,-,- ISO 15901-1:2005(E) 4 ISO 2005 All rights reserved 3.27
44、 through pore pore which passes all the way through the sample 3.28 total porosity ratio of the volume of voids plus the volume of open and closed pores to the total volume occupied by the solid 3.29 true density true particle density mass of the particle divided by its volume, excluding open and cl
45、osed pores 3.30 void space between particles, i.e. an interparticle pore 4 Symbols For the purposes of this document, the following symbols apply. Symbol Term SI unit Derived unit Conversion factors for obsolete units p pressure Pa MPa, psia, Torr, mm Hg 1 psia = 1 lbin-2 = 6 894 Pa 1 Torr = 1 mm Hg
46、 = 133,32 Pa dp pore diameter m nm, m, 1 nm = 109 m, 1 m = 106 m, 1 = 1010 m t time s h 1 h = 3 600 s S specific surface area m2 kg1 m2 g1 VHg intruded volume (of mercury) m3 cm3, 103 mm3 103 mm3 = 1 cm3 = 106 m3 VHg,0 initial intruded volume of mercury m3 cm3, 103 mm3 VHg,max final intruded volume
47、of mercury m3 cm3, 103 mm3 Vp specific pore volume m3kg1 103 mm3 g1 surface tension of mercury Nm1 dynecm1, Nm1 dynecm1 = Nm1 density of mercury = 13,534 at 25,0 C kgm3 gcm3, 103 kgm3103kgm3 = 1 gcm3 contact angle of mercury at the sample, measured through the liquid phase rad 1= (/180) rad 5 Princi
48、ples A non-wettable liquid can enter a porous system only when forced by pressure. The pore size distribution of a porous solid can be determined by forcing mercury into an evacuated sample under increasing pressure and measuring the volume of mercury intruded as a function of pressure. The determination may proceed either with the pressure being raised in a step-wise manner and the volume of mercury intruded measured after an interval of time when equilibrium has been achieved, or by raising the pressure in a continuous (progressive) manner. -,-,- ISO 15901-1:2005(E)