ISO/TS 15338:2020
(Main)Surface chemical analysis — Glow discharge mass spectrometry — Operating procedures
Surface chemical analysis — Glow discharge mass spectrometry — Operating procedures
This document gives procedures for the operation and use of glow discharge mass spectrometry (GD-MS). There are several GD-MS systems from different manufacturers in use and this document describes the differences in their operating procedures when appropriate. NOTE This document is intended to be read in conjunction with the instrument manufacturers' manuals and recommendations.
Analyse chimique des surfaces — Spectrométrie de masse à décharge luminescente (GD-MS) — Introduction à l'utilisation
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TECHNICAL ISO/TS
SPECIFICATION 15338
Second edition
2020-02
Surface chemical analysis — Glow
discharge mass spectrometry —
Operating procedures
Analyse chimique des surfaces — Spectrométrie de masse à décharge
luminescente (GD-MS) — Introduction à l'utilisation
Reference number
©
ISO 2020
© ISO 2020
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 2020 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 1
6 Routine operations . 6
6.1 Cleaning the system . 6
6.2 Support gas handling . 6
7 Calibration . 7
7.1 Mass calibration . 7
7.2 Detector calibration . 7
7.3 Routine checks . 8
8 Data acquisition. 9
8.1 Sample preparation . 9
8.2 Procedure setup . 9
8.3 Data acquiring .10
9 Quantification .10
9.1 Element integral calculation .10
9.2 Ion beam ratios .11
9.3 Fully quantitative analysis .11
9.4 Semi quantitative analysis .12
9.5 Combination of semi quantitative and quantitative analysis .12
Bibliography .13
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
www .iso .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis,
Subcommittee SC 8, Glow discharge spectroscopy.
This second edition cancels and replaces the first edition (ISO/TS 15338:2009), which has been
technically revised.
The main changes compared to the previous edition are as follows:
— This document is more generic and covers not only the static, cryogenic cooled source, but also the
fast flow high power source.
— This document no longer refers to calibration factors specific to one particular instrument type.
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 2020 – All rights reserved
TECHNICAL SPECIFICATION ISO/TS 15338:2020(E)
Surface chemical analysis — Glow discharge mass
spectrometry — Operating procedures
1 Scope
This document gives procedures for the operation and use of glow discharge mass spectrometry (GD-
MS). There are several GD-MS systems from different manufacturers in use and this document describes
the differences in their operating procedures when appropriate.
NOTE This document is intended to be read in conjunction with the instrument manufacturers’ manuals and
recommendations.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle
In a glow discharge source, a potential difference is applied between the cathode (the sample to be
analysed) and the anode, and a plasma is supported by the introduction of an inert gas, normally argon.
This potential difference can be either direct current (DC) or radio frequency (RF), the advantage of
RF being that electrically insulating materials can be analysed directly. Inert gas ions and fast neutrals
formed within the plasma are attracted to the surface of the sample and their impact results in the
production of neutrals by sputtering from surface.
These neutrals diffuse into the plasma where they are subsequently ionised within the equipotential
area of the plasma and can then be extracted to a mass spectrometer for analysis. Both magnetic sector
and time of flight spectrometers are available.
5 Apparatus
5.1 Ion source
There are two fundamental types of ion source used for the GD-MS, a low flow or “static” source, and a
fast flow source. Both types can accept pin samples or samples with a flat surface. A typical pin would
be 20 mm long with a diameter of 3 mm, and a typical flat sample would be 20 mm to 40 mm diameter.
More details of these dimensions can be found later.
In the low flow source the plasma cell is effectively a sealed unit held within a high vacuum chamber,
with a small exit slit or hole to allow the ions to exit the cell and enter the mass spectrometer. The cell
body is at anode potential, the acceleration potential of the mass spectrometer, and the sample is held at
cathode potential, typically 1 kV below anode potential. In this type of source, the argon flow is typically
one sccm (standard atmosphere cubic centimetres per minute) or less, and the gas used, normally
argon, should be of very high purity, six nines five or better. The power of the plasma is relatively low,
typically 2 W or 3 W; the potential difference is typically 1 kV and the current 2 mA or 3 mA.
Key
1 insulator
2 sample (cathode)
3 anode (GD cell)
a
Gas inlet (0,3 sccm to 0,6 sccm)
b
To mass spectrometer
Figure 1 — Low flow source pin geometry
A schematic diagram of the low flow source in pin geometry is shown in Figure 1. The gas is introduced
into the cell through a metal pipe which forms a metal to metal seal with the cell body. On some systems
an alternative of a PEEK tube with a ferrule seal to the cell body is used. The pin sample is held in a
chuck which sits at cathode potential and the cell body is at anode potential, so the two are separated
by an insulating disc. The chuck is actually located against a metal (tantalum) plate which also sits at
cathode potential (not shown in the schematic diagram). The whole assembly forms a good gas seal
while maintaining good electrical insulation. The only escape for the gas and any ions formed in the
plasma is through a small slit or hole at the back of the cell, and this creates a pressure differential
between the cell and the surrounding source vacuum chamber. It is normal to measure the pressure
outside the cell in a low flow source rather than in the cell itself, the presence of a plasma making
the measurement difficult. In this geometry, the potential difference between the anode and cathode
“drops” in a small sheath approximately 1mm around the sample, thus leaving the main gas volume in
the cell at the same potential. So any ions formed in the “plasma cloud” will not be electrically attracted
back to the cathode.
It is standard practice in the low flow source to cool the plasma to near liquid nitrogen temperatures.
This has been shown to reduce significantly the formation of molecular species associated with the
matrix and plasma support gas combined as dimers or trimers, or with gas backgrounds such as
hydrogen, nitrogen and oxygen. Cooling the sample in this way also allows for the measurement of low
melting point materials such as gallium and indium, materials that would melt under normal plasma
conditions.
Heat transfer between the components of the plasma cell needs to be considered. The whole cell
assembly is floated up to the accelerating potential, so the anode will typically be around 6 kV to 8 kV
while the sample (cathode) is at approximately 1 kV lower during operation. The design of the heat
exchanger, or cooling assembly, means that it will be sitting at ground potential, and so it is connected
to the cell insulating disc which is of a larger diameter than the cell body (not shown in Figure 1). Thus,
it is necessary for the insulating disc to have a good coefficient of heat transfer at the same time as
being electrically insulating; the material boron nitride is ideal for this and is used in most systems.
It is important to consider heat transfer through all junctions, particularly from the cell body and
cathode plate through the insulator to the heat exchanger. And in order to make the sample cold, it is
2 © ISO 2020 – All rights reserved
...
TECHNICAL ISO/TS
SPECIFICATION 15338
Second edition
2020-02
Surface chemical analysis — Glow
discharge mass spectrometry —
Operating procedures
Analyse chimique des surfaces — Spectrométrie de masse à décharge
luminescente (GD-MS) — Introduction à l'utilisation
Reference number
©
ISO 2020
© ISO 2020
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 2020 – All rights reserved
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 1
6 Routine operations . 6
6.1 Cleaning the system . 6
6.2 Support gas handling . 6
7 Calibration . 7
7.1 Mass calibration . 7
7.2 Detector calibration . 7
7.3 Routine checks . 8
8 Data acquisition. 9
8.1 Sample preparation . 9
8.2 Procedure setup . 9
8.3 Data acquiring .10
9 Quantification .10
9.1 Element integral calculation .10
9.2 Ion beam ratios .11
9.3 Fully quantitative analysis .11
9.4 Semi quantitative analysis .12
9.5 Combination of semi quantitative and quantitative analysis .12
Bibliography .13
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
www .iso .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 201, Surface chemical analysis,
Subcommittee SC 8, Glow discharge spectroscopy.
This second edition cancels and replaces the first edition (ISO/TS 15338:2009), which has been
technically revised.
The main changes compared to the previous edition are as follows:
— This document is more generic and covers not only the static, cryogenic cooled source, but also the
fast flow high power source.
— This document no longer refers to calibration factors specific to one particular instrument type.
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 2020 – All rights reserved
TECHNICAL SPECIFICATION ISO/TS 15338:2020(E)
Surface chemical analysis — Glow discharge mass
spectrometry — Operating procedures
1 Scope
This document gives procedures for the operation and use of glow discharge mass spectrometry (GD-
MS). There are several GD-MS systems from different manufacturers in use and this document describes
the differences in their operating procedures when appropriate.
NOTE This document is intended to be read in conjunction with the instrument manufacturers’ manuals and
recommendations.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle
In a glow discharge source, a potential difference is applied between the cathode (the sample to be
analysed) and the anode, and a plasma is supported by the introduction of an inert gas, normally argon.
This potential difference can be either direct current (DC) or radio frequency (RF), the advantage of
RF being that electrically insulating materials can be analysed directly. Inert gas ions and fast neutrals
formed within the plasma are attracted to the surface of the sample and their impact results in the
production of neutrals by sputtering from surface.
These neutrals diffuse into the plasma where they are subsequently ionised within the equipotential
area of the plasma and can then be extracted to a mass spectrometer for analysis. Both magnetic sector
and time of flight spectrometers are available.
5 Apparatus
5.1 Ion source
There are two fundamental types of ion source used for the GD-MS, a low flow or “static” source, and a
fast flow source. Both types can accept pin samples or samples with a flat surface. A typical pin would
be 20 mm long with a diameter of 3 mm, and a typical flat sample would be 20 mm to 40 mm diameter.
More details of these dimensions can be found later.
In the low flow source the plasma cell is effectively a sealed unit held within a high vacuum chamber,
with a small exit slit or hole to allow the ions to exit the cell and enter the mass spectrometer. The cell
body is at anode potential, the acceleration potential of the mass spectrometer, and the sample is held at
cathode potential, typically 1 kV below anode potential. In this type of source, the argon flow is typically
one sccm (standard atmosphere cubic centimetres per minute) or less, and the gas used, normally
argon, should be of very high purity, six nines five or better. The power of the plasma is relatively low,
typically 2 W or 3 W; the potential difference is typically 1 kV and the current 2 mA or 3 mA.
Key
1 insulator
2 sample (cathode)
3 anode (GD cell)
a
Gas inlet (0,3 sccm to 0,6 sccm)
b
To mass spectrometer
Figure 1 — Low flow source pin geometry
A schematic diagram of the low flow source in pin geometry is shown in Figure 1. The gas is introduced
into the cell through a metal pipe which forms a metal to metal seal with the cell body. On some systems
an alternative of a PEEK tube with a ferrule seal to the cell body is used. The pin sample is held in a
chuck which sits at cathode potential and the cell body is at anode potential, so the two are separated
by an insulating disc. The chuck is actually located against a metal (tantalum) plate which also sits at
cathode potential (not shown in the schematic diagram). The whole assembly forms a good gas seal
while maintaining good electrical insulation. The only escape for the gas and any ions formed in the
plasma is through a small slit or hole at the back of the cell, and this creates a pressure differential
between the cell and the surrounding source vacuum chamber. It is normal to measure the pressure
outside the cell in a low flow source rather than in the cell itself, the presence of a plasma making
the measurement difficult. In this geometry, the potential difference between the anode and cathode
“drops” in a small sheath approximately 1mm around the sample, thus leaving the main gas volume in
the cell at the same potential. So any ions formed in the “plasma cloud” will not be electrically attracted
back to the cathode.
It is standard practice in the low flow source to cool the plasma to near liquid nitrogen temperatures.
This has been shown to reduce significantly the formation of molecular species associated with the
matrix and plasma support gas combined as dimers or trimers, or with gas backgrounds such as
hydrogen, nitrogen and oxygen. Cooling the sample in this way also allows for the measurement of low
melting point materials such as gallium and indium, materials that would melt under normal plasma
conditions.
Heat transfer between the components of the plasma cell needs to be considered. The whole cell
assembly is floated up to the accelerating potential, so the anode will typically be around 6 kV to 8 kV
while the sample (cathode) is at approximately 1 kV lower during operation. The design of the heat
exchanger, or cooling assembly, means that it will be sitting at ground potential, and so it is connected
to the cell insulating disc which is of a larger diameter than the cell body (not shown in Figure 1). Thus,
it is necessary for the insulating disc to have a good coefficient of heat transfer at the same time as
being electrically insulating; the material boron nitride is ideal for this and is used in most systems.
It is important to consider heat transfer through all junctions, particularly from the cell body and
cathode plate through the insulator to the heat exchanger. And in order to make the sample cold, it is
2 © ISO 2020 – All rights reserved
...
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