ISO/FDIS 20579-2
(Main)Surface chemical analysis — Sample handling, preparation and mounting — Part 2: Documenting and reporting the preparation and mounting of specimens for analysis
Surface chemical analysis — Sample handling, preparation and mounting — Part 2: Documenting and reporting the preparation and mounting of specimens for analysis
This document identifies information to be reported by an analyst in a datasheet, certificate of analysis, report or other publication regarding the preparation and mounting of specimens for surface analysis. This information is needed to ensure reliability and reproducibility of analyses. Such information is in addition to other details associated with specimen synthesis, processing history and characterization, and should become part of the data record (sometimes identified as provenance information) regarding the source of the material and changes that have taken place since it was originated. This document also includes informative annexes that summarize important processes and common approaches relevant to sample preparation and mounting for surface analysis. These are intended as an aid for the analyst in understanding the specialized sample-handling conditions required for analyses by techniques such as Auger electron spectroscopy, secondary-ion mass spectrometry, and X-ray photoelectron spectroscopy. The protocols described may also be applicable for other analytical techniques, such as TXRF, that are sensitive to surface composition. This document does not define the nature of instrumentation or operating procedures needed to ensure that the analytical measurements described have been appropriately conducted.
Analyse chimique des surfaces — Manipulation, préparation et montage des échantillons — Partie 2: Titre manque
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FINAL DRAFT
International
Standard
ISO/TC 201/SC 2
Surface chemical analysis —
Secretariat: ANSI
Sample handling, preparation and
Voting begins on:
mounting —
2024-11-21
Part 2:
Voting terminates on:
2025-01-16
Documenting and reporting the
preparation and mounting of
specimens for analysis
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 SUPPOR TING DOCUMENTATION.
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INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
FINAL DRAFT
International
Standard
ISO/TC 201/SC 2
Surface chemical analysis —
Secretariat: ANSI
Sample handling, preparation and
Voting begins on:
mounting —
Part 2:
Voting terminates on:
Documenting and reporting the
preparation and mounting of
specimens for analysis
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 SUPPOR TING DOCUMENTATION.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms. 2
5 Provenance information to be collected or retained . 2
5.1 Information record .2
5.2 Verification or generation of sample information and analysis objectives .3
6 Information about sample handling and preparation for analysis to be documented and
added to the sample information record . 3
6.1 General .3
6.2 Adherence or exceptions to the general sample handling requirements.3
6.3 Description of ex situ sample handling .4
6.4 Method of mounting samples for analysis .4
6.5 In situ sample cleaning or other sample preparation or processing .5
6.6 Post analysis handling and storage . .5
Annex A (normative) Information on approaches, issues and good practices regarding sample
handling and mounting in preparation for analysis . 6
Annex B (normative) Sources of contamination, sample handling and storage practices .18
Bibliography .24
iii
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.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee TC 201, Surface Chemical Analysis, Subcommittee SC 2,
General Procedures.
This first edition of ISO 20579-2 cancels and replaces ISO 18116:2005, which has been technically revised.
A list of all parts in the ISO 20579 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
0.1 General introduction to the ISO 20579 series
Because sample preparation and handling can have a significant impact on the physical and chemical
properties of a sample surface, reliable surface analysis depends upon knowing the analysis objective and
knowledge of the sample history including aspects of how the sample has been prepared, stored, processed,
and handled prior to and during analysis. The ISO 20579 series specifies information that is required to
be collected and included as part of the sample history (sample provenance information). The ISO 20579
[2]
series describes information that anyone seeking surface analysis is required to provide to an analyst
and additional information that an analyst is required to include in the sample provenance record regarding
[3]
sample handling, storage, and processing. ISO 20579-1 and ISO 20579-2 describe the information to be
recorded regarding sample selection, handling, and storage. ISO 20579-1 describes information that is
necessary for the sample provenance record and an analyst regarding sample selection and preparation
when requesting surface analysis. ISO 20579-2 indicates information about sample handling, preparation,
mounting and processing to be recorded and reported by the analyst. ISO 20579-3 and ISO 20579-4 focus
[5] [4]
on specific reporting requirements associated with biomaterials and nanomaterials, respectively. Each
part of the ISO 20579 series can be used independently of the other parts, although the general reporting
requirements described in ISO 20579-1 and ISO 20579-2 are applicable to a wide range of materials and are
not reproduced in ISO 20579-3 and ISO 20579-4.
Although primarily prepared for the surface-analysis techniques of Auger-electron spectroscopy (AES),
X-ray photoelectron spectroscopy (XPS) and secondary-ion mass spectrometry (SIMS), the methods
described in this document are also applicable to many other surface-sensitive analytical techniques such
as ion-scattering spectrometry (ISS and including low- and medium-energy scattering LEIS, MEIS), scanning
probe microscopy (SPM), low-energy electron diffraction (LEED) and electron energy-loss spectroscopy
(EELS), where specimen handling can influence surface-sensitive measurements. AES, XPS, and SIMS
are sensitive to surface layers that are typically a few nanometers thick. Such thin layers can be subject
to severe perturbations caused by specimen handling or surface treatments that can be necessary prior
to introduction into the analytical chamber. Proper handling and preparation of specimens is particularly
critical for dependable analysis. Improper handling of specimens can result in alteration of the surface
[6][7]
composition and unreliable data.
0.2 Introduction to ISO 20579-2
This document is intended for the analyst and describes information that is required to be recorded and
reported regarding the sample handling, storage, mounting and other aspects of preparing a sample for
surface analysis. This information becomes part of sample provenance record to help validate the reliability
[8]
and usefulness of data obtained from surface-analysis methods.
Although the categories of necessary reporting are similar for all specimens, the details of the required
sample handling can vary depending on the nature of the sample and analysis objectives. When the outer
surface of a specimen is to be analysed the specimen needs to be handled carefully so that the introduction
of spurious contaminants is avoided or minimized. The goal is to preserve the state of the surface during
preparation and mounting so that the analysis remains representative of the original specimen. In other
cases, sample processing is required to enable access to the surface or interface to be analysed and some
aspects of the sample handling might be less stringent. In all cases, the nature of sample handling and
preparation for the desired analyses need to be recorded and reported.
Normative annexes to this document describe methods that the surface analyst can use to minimize the
effects of specimen preparation when using any surface-sensitive analytical technique. Annexes also
describe methods to mount specimens to ensure that the desired analytical information is not compromised.
Annex A describes approaches, issues, and good practices regarding sample handling in preparation for
analysis. Annex B provides information about sources of contamination, sample handling and storage
requirements for differing analysis objectives.
v
FINAL DRAFT International Standard ISO/FDIS 20579-2:2024(en)
Surface chemical analysis — Sample handling, preparation
and mounting —
Part 2:
Documenting and reporting the preparation and mounting of
specimens for analysis
1 Scope
This document specifies information to be reported by an analyst in a datasheet, certificate of analysis,
report or other publication regarding the handling, preparation, processing and mounting of specimens for
surface analysis. Appropriate sample handling with adequate documentation is needed to ensure and assess
reliability and reproducibility of analyses. Such information is in addition to other details associated with
specimen synthesis, processing history and characterization, and should become part of the data record
(sometimes identified as provenance information) regarding the source of the material and changes that
have taken place since it was originated.
This document also includes normative annexes that summarize important processes and common
approaches relevant to sample preparation and mounting for surface analysis. The d
...
ISO/DISFDIS 20579-2
ISO/TC 201/SC 2
Secretariat: ANSI
Date: 2024-09-3011-06
Surface chemical analysis — Sample handling, preparation and
mounting —
Part 2:
Documenting and reporting the preparation and mounting of
specimens for analysis
FDIS stage
Warning for WD’s and CD’s
This document is not an ISO International Standard. It is distributed for review and comment. It is subject to change
without notice and may not be referred to as an International Standard.
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/DISFDIS 20579-2:2024(en)
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication
may be reproduced or utilized otherwise in any form or by any means, 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 ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
E-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO/DISFDIS 20579-2:2024(en)
Contents
Foreword . v
Introduction . vi
Part 2: Documenting and reporting the preparation and mounting of specimens for analysis . 1
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms . 2
5 Provenance information to be collected or retained . 2
5.1 Information record . 2
5.2 Verification or generation of sample information and analysis objectives . 3
6 Information about sample handling and preparation for analysis to be documented and
added to the sample information record . 3
6.1 General . 3
6.2 Adherence or exceptions to the general sample handling requirements . 3
6.3 Description of ex situ sample handling . 4
6.4 Method of mounting samples for analysis . 4
6.5 In situ sample cleaning or other sample preparation or processing . 5
6.6 Post analysis handling and storage . 5
Annex A (normative Information about approaches, issues and good practices regarding
sample handling and mounting in preparation for analysis . 6
A.1 Introduction and overview . 6
A.1.1 General handing requirements for surface analysis . 6
A.2 Assessment and Planning . 6
A.2.1 Introduction . 6
A.2.2 Visual Inspection Before and After Analysis . 7
A.2.3 Analysis Order . 7
A.2.4 Differences in handling and mounting requirements for AES, XPS, SIMS and other Surface
Analysis methods . 7
A.2.5 Sample charging issues . 8
A.2.6 Storage and Transfer Prior to Analysis . 8
A.3 Ex situ sample handling (e.g. cleaning, cutting/sectioning, polishing, or exposing the
region of interest before insertion into the analysis chamber) . 9
A.3.1 Introduction and Overview . 9
A.3.2 Sample cleaning techniques . 10
A.3.3 Sectioning/cutting techniques - altering the size or shape of a sample . 10
A.3.4 Exposing the surface or buried interface of interest (ex situ). 11
A.3.5 Sample coatings . 12
A.4 Mounting techniques . 12
A.4.1 Introduction . 13
A.4.2 General Procedures . 13
A.4.3 Powders and Particles . 13
A.4.4 Wires, Fibers, and Filaments . 13
A.4.5 Pedestal mounting . 14
A.4.6 Special Cases: gassy specimens, viscous liquids, solute residues, freezing samples . 14
A.4.7 Masking for charge control . 14
A.5 In situ sample cleaning or other sample preparation or processing to expose the region of
interest . 14
iii
ISO/DISFDIS 20579-2:2024(en)
A.5.1 Sample Heating: Cleaning/Decontamination, Segregation Studies, Reactive Layer
Formation . 15
A.5.2 Ion sputtering and cluster cleaning . 15
A.5.3 UV radiation . 15
A.5.4 Fracturing, cleaving, and scribing in situ . 16
A.5.5 Coatings and Growth of overlayers . 16
A.5.6 FIB Cross sections and crater edge profiling . 17
Annex B (normative Sources of contamination, sample handling and storage practices . 18
B.1 Introduction . 18
B.2 Potential Sources of contamination during handling . 18
B.3 Handling procedures to minimize contamination . 19
B.3.1 Introduction . 19
B.3.2 Description of important generic sample handling requirements . 19
B.3.3 Analysis objectives determine specific sample handling requirements . 19
B.4 Storage requirements and needs . 22
B.4.1 General . 22
B.4.2 Storage time, temperature, and humidity . 22
B.4.3 Containers . 23
Bibliography . 24
Foreword . v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Symbols and abbreviated terms . 2
5 Provenance information to be collected or retained . 2
6 Information about sample handling and preparation for analysis to be documented and
added to the sample information record . 3
Annex A (normative) Information on approaches, issues and good practices regarding sample
handling and mounting in preparation for analysis . 7
Annex B (normative) Sources of contamination, sample handling and storage practices . 20
Bibliography . 27
iv
ISO/DISFDIS 20579-2:2024(en)
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.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types of
ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent rights
in respect thereof. As of the date of publication of this document, ISO had not received notice of (a) patent(s)
which may be required to implement this document. However, implementers are cautioned that this may not
represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents.www.iso.org/patents. ISO shall not be held responsible for identifying any or all such
patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.htmlwww.iso.org/iso/foreword.html.
This document was prepared by Techn
...
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