ISO/TS 15338:2025
(Main)Surface chemical analysis — Glow discharge mass spectrometry — Operating procedures
Surface chemical analysis — Glow discharge mass spectrometry — Operating procedures
This document specifies 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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Standards Content (Sample)
Technical
Specification
ISO/TS 15338
Third edition
Surface chemical analysis — Glow
2025-03
discharge mass spectrometry —
Operating procedures
Analyse chimique des surfaces — Spectrométrie de masse à
décharge luminescente (GD-MS) — Introduction à l'utilisation
Reference number
© ISO 2025
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ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
5 Apparatus . 1
5.1 Ion source .1
5.2 Mass analyser .5
5.3 Detector system.5
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
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 ISO/TC 201, Surface chemical analysis, Subcommittee
SC 8, Glow discharge spectroscopy.
This third edition cancels and replaces the second edition (ISO/TS 15338:2020), which has been technically
revised.
The main changes are as follows:
— additional technical information have been added to the principle, apparatus and routine operations
— minor editorial changes.
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
Technical Specification ISO/TS 15338:2025(en)
Surface chemical analysis — Glow discharge mass
spectrometry — Operating procedures
1 Scope
This document specifies 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 terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// 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, but other inert
gases can be used. 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. The impacts of inert
gas ions and fast neutrals formed within the plasma on the surface of the sample result 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. It must
be big enough to cover the hole in the chosen anode plate and provide a good gas seal. 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. If a metal pipe is used, then an insulating
material must be included in the gas line as the cell is at anode potential. This is normally a piece of quartz
with a very small diameter hole through which the gas passes. 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 1 mm 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 fo
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