ISO/TS 15338

ISO TC201 SC8 N348
ISO /DTS 15338(Ed.3): xxxx(E)
ISO /TC 201/SC 8
Secretariat: JISC
Date: 2024-11-25
Surface chemical analysis — Glow discharge mass
spectrometry — Operating procedures

DTS stage
Warning for WDs and CDs
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.

Analyse chimique des surfaces — Spectrométrie de masse à décharge luminescente (GD-MS) — Introduction à
l'utilisation
ISO TS 15338:20xx(E)
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ISO TS 15338:xxxx(E)
Contents
Foreword . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Apparatus . 1
5 Routine operations. 7
6 Calibration . 8
7 Data acquisition . 10
8 Quantification . 12
Bibliography . 15

Foreword . iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus . 1
6 Routine operations. 5
6.1 Cleaning the system . 5
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

iv © ISO 2024 – All rights reserved

ISO TS 15338:20xx(E)
Foreword
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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 minor
technically revised.
The main changes compared to the previous edition are as follows:
— — Minor editorial changes to and additional technical information have been added to the principle,
apparatus and routine operations.
A list of all parts in the ISO/TS15338 series can be found on the ISO website.
— minor editorial changes.
Any feedback or questions on this document should be directed to the user’s national standards body. A
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ISO TS /DTS 15338:xxxx(E:(en)
vi © ISO 2024 – All rights reserved
vi
TECHNICAL SPECIFICATION ISO TS 15338:20xx(E)

Surface chemical analysis — Glow discharge mass spectrometry —
Operating procedures
1 Scope
This document givesspecifies 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 terminologicalterminology databases for use in standardization at the following
addresses:
— — ISO Online browsing platform: available at https://www.iso.org/obphttps://www.iso.org/obp
— — IEC Electropedia: available at http://www.electropedia.org/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.
4 Apparatus
4.1 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
ISO/DTS 15338:(en)
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.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
...