ISO 15901-1:2016

DRAFT INTERNATIONAL STANDARD
ISO/DIS 15901-1
ISO/TC 24/SC 4 Secretariat: DIN
Voting begins on: Voting terminates on:
2013-12-16 2014-03-16
Evaluation of pore size distribution and porosity of solid
materials by mercury porosimetry and gas adsorption —
Part 1:
Mercury porosimetry
Distribution de taille des pores et la porosité des matériaux solides par porosimétrie à mercure et
l’adsorption des gaz —
Partie 1: Porosimétrie à mercure
[Revision of first edition (ISO 15901-1:2005) and ISO 15901-1:2005/Cor 1:2007]
ICS: 19.120
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 15901-1:2013(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2013

ISO/DIS 15901-1:2013(E)
Copyright notice
This ISO document is a Draft International Standard and is copyright-protected by ISO. Except as
permitted under the applicable laws of the user’s country, neither this ISO draft nor any extract
from it 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 being secured.
Requests for permission to reproduce should be addressed to either ISO at the address below or ISO’s
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 copyright@iso.org
Web www.iso.org
Reproduction may be subject to royalty payments or a licensing agreement.
Violators may be prosecuted.
ii © ISO 2013 – All rights reserved

ISO/DIS 15901-1
Contents Page
Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Symbols and abbreviated terms . 5
5 Principles. 6
6 Apparatus and material . 7
6.1 Sample holder . 7
6.2 Porosimeter . 7
6.3 Mercury . 7
7 Procedures for calibration and performance . 7
7.1 General . 7
7.2 Pressure signal calibration. 8
7.3 Volume signal calibration . 8
7.4 Vacuum transducer calibration . 8
7.5 Verification of porosimeter performance . 8
8 Procedures . 8
8.1 Sampling. 8
8.1.1 Obtaining a test sample . 8
8.1.2 Quantity of sample . 9
8.2 Method . 9
8.2.1 Sample pre-treatment . 9
8.2.2 Filling of the sample holder . 9
8.2.3 Evacuation . 10
8.2.4 Filling the sample holder with mercury . 10
8.2.5 Measurement . 10
8.2.6 Completion of test . 11
8.2.7 Blank and sample compression correction . 11
9 Evaluation. 11
9.1 Determination of the pore size distribution . 11
9.2 Determination of the specific pore volume . 12
9.3 Determination of the specific surface area . 12
9.4 Determination of the bulk and skeleton densities . 13
9.4.1 Bulk density . 13
9.4.2 Skeleton density . 13
9.5 Determination of the porosity . 13
10 Reporting . 14
Annex A (informative) Mercury porosimetry analysis results . 15
A.1 Presentation of pore size distributions (Example) . 15
A.2 Intrusion data summary (Example) . 15
Annex B (informative) Recommendations for the safe handling of mercury . 18
Bibliography . 19

ISO/DIS 15901-1
Foreword
ISO (the International Organization for Standardization) is a worldwide federation 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 committee. 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 accordance 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 requires 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 Technical Committee ISO/TC 24, Particle characterization including sieving,
Subcommittee SC 4, Particle characterization.
ISO 15901 consists of the following parts, under the general 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 macro-pores by gas adsorption
 Part 3: Analysis of micropores by gas adsorption
iv © ISO 2013 – All rights reserved

ISO/DIS 15901-1
Introduction
In 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 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 accessible pores and voids to the total volume occupied by
an amount of the solid. In addition to the accessible pores, a solid may 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 this standard.
Porous materials may 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 necessary 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 sterilization,
 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) 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 not 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 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 appropriate diameter range of 0,004 µm to 400 µm.
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 the approximate
diameter range of 0,002 µm to 0,1 µm (2 nm to 100 nm).
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 pores in the approximate diameter range
of 0,4 nm to 2 nm.
DRAFT INTERNATIONAL STANDARD ISO/DIS 15901-1

Evaluation of pore size distribution and porosity of solid
materials by mercury porosimetry 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 user 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 area of pores in solids 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 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 4 nm. The maximum
diameter will be limited for samples having a significant depth
...