ISO/TS 20177:2018
(Main)Vacuum technology — Vacuum gauges — Procedures to measure and report outgassing rates
Vacuum technology — Vacuum gauges — Procedures to measure and report outgassing rates
This document describes procedures to measure outgassing rates from components designed for vacuum chambers and of vacuum chambers as a whole. The outgassing rates are expected to be lower than 10−5 Pa m3 s−1 (10−2 Pa L s−1) at 23 °C and to emerge from devices that are suitable for high or ultra-high vacuum applications. The molecular mass of the outgassing species or vapour is below 300 u. The upper limit 10−5 Pa m3 s−1 of total outgassing rate is specified independent of the size, the total surface area and texture or state of the outgassing material. If a specific outgassing rate (outgassing rate per area) is determined, the area is not a specific surface area including the surface roughness, but the nominal geometrical one. When it is difficult to determine the nominal geometrical surface area of the sample, such as powders, porous materials, very rough surfaces, or complex devices, mass specific outgassing rate (e.g. outgassing rate per gram) is used. For many practical applications, it is sufficient to determine the total outgassing rate. If a measuring instrument, which sensitivity is gas species dependent, is used, the total outgassing rate are given in nitrogen equivalent. In cases, however, where the total outgassing rate is too high, the disturbing gas species is identified, and its outgassing rate is measured in order to improve the sample material. This document covers both cases. Some outgassing molecules can adsorb on a surface with a residence time that is much longer than the total time of measurement. Such molecules cannot be detected by a detecting instrument when there is no direct line of sight. This is considered as a surface effect and surface analytical investigations are more useful than general outgassing rate measurements considered here. Also, molecules that are released from the surface by irradiation of UV light or X-rays, are out of the scope of this document. This document is written to standardize the measurement of outgassing rates in such a way that values obtained at different laboratories and by different methods are comparable. To this end, for any of the described methods, traceability is provided to the System International (SI) for the most important parameters of each method and according to the metrological level. Outgassing rate measurements by mass loss, which were mainly developed for testing of spacecraft and satellite materials, are not gas specific. For acceptable measurement times, mass loss measurements require significantly higher outgassing rates (>10−5 Pa m3 s−1) than typical for high and ultrahigh vacuum components. Also, it is not possible to measure the sample in situ due to the weight of the vacuum chamber, since the balances are not vacuum compatible. For these reasons, mass loss measurements are not considered in this document. It is assumed that the user of this document is familiar with high and ultra-high vacuum technology and the corresponding measuring instrumentation such as ionization gauges and quadrupole mass spectrometers.
Technique du vide — Manomètres à vide — Méthodes de mesurage et de rapport du taux de dégagement de gaz
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TECHNICAL ISO/TS
SPECIFICATION 20177
First edition
2018-06
Vacuum technology — Vacuum gauges
— Procedures to measure and report
outgassing rates
Technique du vide — Manomètres à vide — Méthodes de mesurage et
de rapport du taux de dégagement de gaz
Reference number
©
ISO 2018
© ISO 2018
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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Symbols and abbreviated terms . 3
5 Measurement systems . 4
5.1 General . 4
5.1.1 Overview . 4
5.1.2 Recommendations for systems .4
5.1.3 Vacuum chambers and pumps .5
5.1.4 Vacuum gauges .6
5.1.5 Purity of gases .6
5.2 Systems applying the throughput method .6
5.2.1 General. 6
5.2.2 Continuous expansion system as flow comparator .6
5.2.3 Throughput system with calculated conductance element .8
5.2.4 Throughput system with measured effective pumping speed . 10
5.2.5 Throughput system with modulated conductance . 12
5.3 Accumulation systems . 13
5.3.1 General.13
5.3.2 Basic accumulation system . 13
5.3.3 Accumulation system with gas analysis system (extended
accumulation system) . 13
6 Measurement procedures .14
6.1 General .14
6.2 Recommended sample preparation . 15
6.3 Course and time period of measurement . 16
6.4 Measurement procedures . 16
6.4.1 Procedure with continuous expansion system as flow comparator . 16
6.4.2 Procedure with throughput system with calculated conductance element
(pressure difference system) . 17
6.4.3 Procedure with throughput system with measured effective pumping speed . 18
6.4.4 Procedure with throughput system with modulated conductance . 19
6.4.5 Procedure with accumulation systems . 20
7 Measurement uncertainties .23
7.1 General .23
7.2 Continuous expansion system as flow comparator (5.2.2) .23
7.3 Throughput system with calculated conductance element (5.2.3) .23
7.4 Throughput system with measured effective pumping speed (5.2.4) .24
7.5 Throughput system with modulated conductance (5.2.5) .24
7.6 Basic accumulation system (5.3.2) .24
7.7 Accumulation system with gas analysis system (5.3.3) .25
8 Reporting results .28
Annex A (informative) Schemes of principles of measurement systems .30
Annex B (informative) Applicability and characteristics of the different measurement system .36
Annex C (informative) Traceability of the different measurement systems to the SI .37
Bibliography .39
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 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/directives).
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 the 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 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 the following
URL: www .iso .org/iso/foreword .html.
This document was prepared by Technical Committee TC 112, Vacuum technology.
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 © ISO 2018 – All rights reserved
Introduction
Outgassing from the inner wall of a vacuum chamber and from components in a vacuum chamber
limit the achievable lowest pressure in a vacuum system and its cleanliness. The lowest achievable
pressure is usually important in research facilities as accelerators, in facilities that need to ensure
a clean surface, e.g. molecular beam epitaxy, or in devices that need to ensure high vacuum without
pump for long times, such as transmitters or X-ray tubes, medical instruments, surface analytical
instrumentation or insulation panels. Cleanliness of a vacuum, i.e. the absence or sufficiently low partial
pressure of specific gas species or vapours, is important in many different industrial applications such
as coating, EUV lithography, catalysis, drying processes in the pharmaceutical or food industry but also
in accelerators, fusion reactors, etc. The measurement of outgassing rates is therefore an important
tool of quality assurance in vacuum technology. This document recommends well-defined procedures
with the possibility of getting traceability of the results of an outgassing rate measurement.
Annex A lists schemes of principles of measurement systems.
TECHNICAL SPECIFICATION ISO/TS 20177:2018(E)
Vacuum technology — Vacuum gauges — Procedures to
measure and report outgassing rates
1 Scope
This document describes procedures to measure outgassing rates from components designed for
vacuum chambers and of vacuum chambers as a whole. The outgassing rates are expected to be lower
−5 3 −1 −2 −1
than 10 Pa m s (10 Pa L s ) at 23 °C and to emerge from devices that are suitable for high or
ultra-high vacuum applications. The molecular mass of the outgassing species or vapour is below 300 u.
−5 3 −1
The upper limit 10 Pa m s of total outgassing rate is specified independent of the size, the total
surface area and texture or state of the outgassing material. If a specific outgassing rate (outgassing
rate per area) is determined, the area is not a specific surface area including the surface roughness, but
the nominal geometrical one. When it is difficult to determine the nominal geometrical surface area of
the sample, such as powders, porous materials, very rough surfaces, or complex devices, mass specific
outgassing rate (e.g. outgassing rate per gram) is used.
For many practical applications, it is sufficient to determine the total outgassing rate. If a measuring
instrument, which sensitivity is gas species dependent, is used, the total outgassing rate are given in
nitrogen equivalent. In cases, however, where the total outgassing rate is too high, the disturbing gas
species is identified, and its outgassing rate is measured in order to improve the sample material. This
document covers both cases.
Some outgassing molecules can adsorb on a surface with a residence time that is much longer than the
total time of measurement. Such molecules cannot be detected by a detecting instrument when there
is no direct line of sight. This is considered as a surface effect and surface analytical investigations
are more useful than general outgassing rate measurements considered here. Also, molecules that are
released from the surface by irradiation of UV light or X-rays, are out of the scope of this document.
This document is written to standardize the measurement of outgassing rates in such a way that values
obtained at different laboratories and by different methods are comparable. To this end, for any of the
described methods, traceability is provided to the System International (SI) for the most important
parameters of each method and according to the metrological level.
Outgassing rate measurements by mass loss, which were mainly developed for testing of spacecraft and
satellite materials, are not gas specific. For acceptable measurement times, mass loss measurements
−5 3 −1
require significantly higher outgassing rates (>10 Pa m s ) than typical for high and ultrahigh
vacuum components. Also, it is not possible to measure the sample in situ due to the weight of the vacuum
chamber, since the balances are not vacuum compatible. For these reasons, mass lo
...
TC /SCISO/TC 112/SC
Date: 2018-06
ISO/TC /112/SC //WG 2
Secretariat: DIN
Vacuum technology — Vacuum gauges — Procedures to measure and
report outgassing rates
Élément introductif — Élément central — Élément complémentaire
Document type: Technical Specification
Document subtype:
Document stage: (60) Publication
Document language: E
T:\KDV\K01_Normung\K1-3 ISO\K1-3-2 Gremien\K1-3-2-6 TC 112\TC 112 Standards & Drafts\ISO
20177 Outgassing rate\03 publication\ISO_DTS_20177_(E).docx STD Version 2.9d
All rights reserved. Unless otherwise specified, 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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
copyright@iso.org
www.iso.org
ii
Contents Page
Foreword . v
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Symbols and abbreviated terms . 3
5 Measurement systems . 4
5.1 General . 4
5.1.1 Overview . 4
5.1.2 Recommendations for systems . 4
5.1.3 Vacuum chambers and pumps . 6
5.1.4 Vacuum gauges . 6
5.1.5 Purity of gases . 6
5.2 Systems applying the throughput method . 7
5.2.1 General . 7
5.2.2 Continuous expansion system as flow comparator . 7
5.2.3 Throughput system with calculated conductance element . 8
5.2.4 Throughput system with measured effective pumping speed . 11
5.2.5 Throughput system with modulated conductance . 13
5.3 Accumulation systems . 14
5.3.1 General . 14
5.3.2 Basic accumulation system . 14
5.3.3 Accumulation system with gas analysis system (extended accumulation system) . 14
6 Measurement procedures . 15
6.1 General . 15
6.2 Recommended sample preparation . 16
6.3 Course and time period of measurement . 17
6.4 Measurement procedures . 17
6.4.1 Procedure with continuous expansion system as flow comparator . 17
6.4.2 Procedure with throughput system with calculated conductance element (pressure
difference system) . 18
6.4.3 Procedure with throughput system with measured effective pumping speed . 20
6.4.4 Procedure with throughput system with modulated conductance . 21
6.4.5 Procedure with accumulation systems . 22
7 Measurement uncertainties . 24
7.1 General . 24
7.2 Continuous expansion system as flow comparator (5.2.2) . 25
7.3 Throughput system with calculated conductance element (5.2.3) . 25
7.4 Throughput system with measured effective pumping speed (5.2.4) . 25
7.5 Throughput system with modulated conductance (5.2.5) . 26
7.6 Basic accumulation system (5.3.2) . 26
7.7 Accumulation system with gas analysis system (5.3.3) . 26
8 Reporting results . 29
Annex A (informative) Schemes of principles of measurement systems . 32
iii
Annex B (informative) Applicability and characteristics of the different measurement
system . 39
Annex C (informative) Traceability of the different measurement systems to the SI . 41
Bibliography . 43
iv
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 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/directives).
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 the 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 onof 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 the following URL:
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee TC 112, Vacuum technology.
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.
v
Introduction
Outgassing from the inner wall of a vacuum chamber and from components in a vacuum chamber limit
the achievable lowest pressure in a vacuum system and its cleanliness. The lowest achievable pressure is
usually important in research facilities as accelerators, in facilities that need to ensure a clean surface,
e.g. molecular beam epitaxy, or in devices that need to ensure high vacuum without pump for long times,
such as transmitters or X-ray tubes, medical instruments, surface analytical instrumentation or insulation
panels. Cleanliness of a vacuum, i.e. the absence or sufficiently low partial pressure of specific gas species
or vapours, is important in many different industrial applications such as coating, EUV lithography,
catalysis, drying processes in the pharmaceutical or food industry but also in accelerators, fusion
reactors, etc. The measurement of outgassing rates is therefore an important tool of quality assurance in
vacuum technology. This document recommends well-defined procedures with the possibility of getting
traceability of the results of an outgassing rate measurement.
Annex A lists schemes of principles of measurement systems.
vi
TECHNICAL SPECIFICATION
Vacuum technology — Vacuum gauges — Procedures to measure and
report outgassing rates
1 Scope
This document describes procedures to measure outgassing rates from components designed for vacuum
chambers and of vacuum chambers as a whole. The outgassing rates are expected to be lower than
−5 3 −1 −2 −1
10 Pa m s (10 Pa L s ) at 23 °C and that theto emerge from devices that are suitable for high or
ultra-high vacuum applications. The molecular mass of the outgassing species or vapour is below 300 u.
−5 3 −1
The upper limit 10 Pa m s of total outgassing rate is specified independent of the size, the total surface
area and texture or state of the outgassing material. If a specific outgassing rate (outgassing rate per area)
is determined, the area is not a specific surface area including the surface roughness, but the nominal
geometrical one. When it is difficult to determine the nominal geometrical surface area of the sample,
such as powders, porous materials, very rough surfaces, or complex devices, mass specific outgassing
rate (e.g. outgassing rate per gram) is used.
For many practical applications, it is sufficient to determine the total outgassing rate. If a measuring
instrument, which sensitivity is gas species dependent, is used, the total outgassing rate are given in
nitrogen equivalent. In cases, however, where the total outgassing rate is too high, the disturbing gas
species is identified, and its outgassing rate is measured in order to improve the sample material. This
document covers both cases.
Some outgassing molecules can adsorb on a surface with a residence time that is much longer than the
total time of measurement. Such molecules cannot be detected by a detecting instrument when there is
no direct line of sight. This is considered as a surface effect and surface analytical investigations are more
useful than general outgassing rate measurements considered here. Also, molecules that are released
from the surface by irradiation of UV light or X-rays, are out of the scope of this document.
This document is written to standardize the measurement of outgassing rates in such a way that values
obtained at different laboratories and by different methods are comparable. To this end, for any of the
described methods, traceability is provided to the System International (SI) for the most important
parameters of each method and according to the metrological level.
Outgassing rate measurements by mass loss, which were mainly developed for testing of spacecraft and
satellite materials, are not gas specific. For acceptable measurement times, mass loss measurements
−5 3 −1
require significantly higher outgassing rates (>10 Pa m s ) than typical for high and ultrahigh vacuum
components. Also, it is not possible to measure the sample
...
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