Standard Guide for Handling Specimens Prior to Surface Analysis

SIGNIFICANCE AND USE
Proper handling and preparation of specimens is particularly critical for analysis. Improper handling of specimens can result in alteration of the surface composition and unreliable data. Specimens should be handled carefully so as to avoid the introduction of spurious contaminants. The goal must be to preserve the state of the surface so that analysis remains representative of the original subject.
Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and secondary ion mass spectroscopy (SIMS) are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations from improper specimen handling (1).3  
This guide describes methods to minimize the effects of specimen handling on the results obtained using surface-sensitive analytical techniques. It is intended for the specimen owner or the purchaser of surface analytical services and the surface analyst. Because of the wide range of types of specimens and desired information, only broad guidelines and general examples are presented here. The optimum handling procedures will be dependent on the particular specimen and the needed information. It is recommended that the specimen supplier consult the surface analyst as soon as possible with regard to specimen history, the specific problem to be solved or information needed, and the particular specimen preparation or handling procedures required. The surface analyst also is referred to Guide E 1078 that discusses additional procedures for preparing, mounting, and analysis of specimens.
SCOPE
1.1 This guide covers specimen handling and preparation prior to surface analysis and applies to the following surface analysis disciplines:
1.1.1 Auger electron spectroscopy (AES),
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA), and
1.1.3 Secondary ion mass spectrometry, SIMS.
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods may also apply to many surface-sensitive analysis methods, such as ion scattering spectrometry, low-energy electron diffraction, and electron energy loss spectroscopy, where specimen handling can influence surface-sensitive measurements.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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Publication Date
09-Apr-2002
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Designation:E1829–02
Standard Guide for
1
Handling Specimens Prior to Surface Analysis
This standard is issued under the fixed designation E 1829; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.2 Auger electron spectroscopy (AES), X-ray photoelec-
tronspectroscopy(XPS),andsecondaryionmassspectroscopy
1.1 This guide covers specimen handling and preparation
(SIMS) are sensitive to surface layers that are typically a few
prior to surface analysis and applies to the following surface
nanometres thick. Such thin layers can be subject to severe
analysis disciplines:
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perturbations from improper specimen handling (1).
1.1.1 Auger electron spectroscopy (AES),
4.3 This guide describes methods to minimize the effects of
1.1.2 X-ray photoelectron spectroscopy (XPS or ESCA),
specimen handling on the results obtained using surface-
and
sensitive analytical techniques. It is intended for the specimen
1.1.3 Secondary ion mass spectrometry, SIMS.
owner or the purchaser of surface analytical services and the
1.1.4 Although primarily written forAES, XPS, and SIMS,
surface analyst. Because of the wide range of types of
these methods may also apply to many surface-sensitive
specimens and desired information, only broad guidelines and
analysis methods, such as ion scattering spectrometry, low-
general examples are presented here. The optimum handling
energy electron diffraction, and electron energy loss spectros-
procedures will be dependent on the particular specimen and
copy, where specimen handling can influence surface-sensitive
the needed information. It is recommended that the specimen
measurements.
supplier consult the surface analyst as soon as possible with
1.2 This standard does not purport to address all of the
regardtospecimenhistory,thespecificproblemtobesolvedor
safety concerns, if any, associated with its use. It is the
information needed, and the particular specimen preparation or
responsibility of the user of this standard to establish appro-
handling procedures required. The surface analyst also is
priate safety and health practices and determine the applica-
referred to Guide E 1078 that discusses additional procedures
bility of regulatory limitations prior to use.
for preparing, mounting, and analysis of specimens.
2. Referenced Documents
5. General Requirements
2.1 ASTM Standards:
2
5.1 The degree of cleanliness required by surface-sensitive
E 673 Terminology Relating to Surface Analysis
analyticaltechniquesoftenismuchgreaterthanforotherforms
E 1078 Guide for Specimen Preparation and Mounting in
2
of analysis.
Surface Analysis
5.2 Specimens must never be in contact with the bare hand.
3. Terminology
Handling of the surface to be analyzed should be eliminated or
minimized whenever possible.
3.1 Definitions—For definitions of surface analysis terms
5.3 Specimens should be transported to the analyst in a
used in this guide, see Terminology E 673.
container that does not come into direct contact with the
4. Significance and Use
surface of interest.
5.4 In most cases, the analysis will be performed on the “as
4.1 Proper handling and preparation of specimens is par-
received” specimen. Surface contamination or atmospheric
ticularly critical for analysis. Improper handling of specimens
adsorbates are not usually removed because of the importance
can result in alteration of the surface composition and unreli-
of analyzing an unaltered surface and as these are often the
abledata.Specimensshouldbehandledcarefullysoastoavoid
regions of interest. Care must then be taken in the handling the
the introduction of spurious contaminants. The goal must be to
specimen to ensure that no outside agents come in contact with
preserve the state of the surface so that analysis remains
thesurfacetobeinvestigated.Theseagentsinclude:solventsor
representative of the original subject.
cleaning solutions, gases (including compressed air) or vapors,
metals, tissue or other wrapping materials, tape, cloth, tools,
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface packing materials or the walls of containers. If the specimen
Analysis and is the direct responsibility of Subcommittee E42.03 onAuger Electron
Spectroscopy and X-ray Photoelectron Spectroscopy.
Current edition approved April 10, 2002. Published April 2002. Originally
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published as E 1829 – 96. Last previous edition E 1829 – 97. The boldface numbers in parentheses refer to the list of references at the end of
2
Annual Book of ASTM Standards, Vol 03.06. this standard.
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