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ASTM E983-05

(Guide)

Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy

Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy

SCOPE
1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.
1.3 General classes of materials are identified which are most likely to exhibit unwanted electron beam effects. In addition, a tabulation of some specific materials which have been observed to undergo electron damage effects is provided.
1.4 A simple method is outlined for establishing the existence and extent of these effects during routine AES analysis.
1.5 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.

General Information

Status
Historical
Publication Date
24-Jul-2005
ICS
17.180.30 - Optical measuring instruments
Technical Committee
E42 - Surface Analysis
Drafting Committee
E42.03 - Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy
Current Stage
Ref Project

Relations

Replaces
ASTM E983-94(1999) - Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
Effective Date
25-Jul-2005
Replaced By
ASTM E983-10 - Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
Effective Date
01-Nov-2010
Referred By
ASTM E996-19 - Standard Practice for Reporting Data in Auger Electron Spectroscopy and X-ray Photoelectron Spectroscopy
Effective Date
25-Jul-2005
Referred By
ASTM E984-12(2020) - Standard Guide for Identifying Chemical Effects and Matrix Effects in Auger Electron Spectroscopy
Effective Date
25-Jul-2005
Referred By
ASTM E1078-14(2020) - Standard Guide for Specimen Preparation and Mounting in Surface Analysis
Effective Date
25-Jul-2005

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ASTM E983-05 - Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron SpectroscopyASTM E983-05 - Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
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ASTM E983-05 - Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:E983–05
Standard Guide for
Minimizing Unwanted Electron Beam Effects in Auger
1
Electron Spectroscopy
This standard is issued under the fixed designation E983; 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 (´) indicates an editorial change since the last revision or reapproval.
Note— Changes were made throughout and the year date changed on July 25, 2005.
electron beam damage, sample damage, specimen damage, beam effects,
1. Scope
electron beam induced processes, and electron irradiation effects.
1.1 This guide outlines the origins and manifestations of
unwantedelectronbeam effects inAuger electron spectroscopy
4. Significance and Use
(AES).
4.1 When electron beam excitation is used in AES, the
1.2 Some general guidelines are provided concerning the
incident electron beam can interact with the specimen material
electron beam parameters which are most likely to produce
causing physical and chemical changes. In general, these
these effects and suggestions are offered on how to minimize
effects are a hindrance to AES analysis because they cause
them.
3
localized specimen modification (1, 2, 3, 4).
1.3 General classes of materials are identified which are
4.2 With specimens that have poor electrical conductivity
most likely to exhibit unwanted electron beam effects. In
the electron beam can stimulate the development of localized
addition, a tabulation of some specific materials which have
charge on the specimen surface. This effect is a hindrance to
been observed to undergo electron damage effects is provided.
AES analysis because the potentials associated with the charge
1.4 A simple method is outlined for establishing the exist-
can either adversely affect the integrity of Auger data or make
ence and extent of these effects during routine AES analysis.
Auger data collection difficult.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
5. Origins of Electron Beam Effects
responsibility of the user of this standard to establish appro-
5.1 Electron beam effects inAES may originate from one or
priate safety and health practices and determine the applica-
more distinct processes.
bility of regulatory limitations prior to use.
5.1.1 Charge accumulation (5) (see Chapter 9) in materials
with poor electrical conductivity leading to potentials that
2. Referenced Documents
cause distortion of Auger data or make AES data collection
2
2.1 ASTM Standards:
difficult by virtue of:
E673 Terminology Relating to Surface Analysis
5.1.1.1 Auger peak shift on energy scale.
E996 Practice for Reporting Data in Auger Electron Spec-
5.1.1.2 Auger peak shape and size distortion.
troscopy and X-ray Photoelectron Spectroscopy
5.1.1.3 Auger signal strength instability.
5.1.2 Electronic excitation of surface, subsurface, and bulk
3. Terminology
atoms and molecules leading to specimen changes (6-8) which
3.1 See Terminology E673 for terms used inAuger electron
include:
spectroscopy.
5.1.2.1 Dissociation.
NOTE 1—Electron beam effects and their consequences are widely
5.1.2.2 Electron stimulated desorption (ESD) (9).
referred to in the literature using any one or more of the following terms:
5.1.2.3 Electron stimulated adsorption (ESA) (10).
5.1.2.4 Polymerization (11, 12).
5.1.2.5 Carburization (13-15).
1
This guide is under the jurisdiction of ASTM Committee E42 on Surface
5.1.2.6 Oxidation (16, 17).
Analysis and is the direct responsibility of Subcommittee E42.03 onAuger Electron
Spectroscopy and XPS.
5.1.2.7 Reduction (18).
Current edition approved July 25, 2005. Published July 2005. Originally
5.1.2.8 Decomposition (19, 20).
approved in 1984. Last previous edition approved in 2004 as E983 – 04. DOI:
5.1.2.9 Erosion.
10.1520/E0983-05.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to the references listed at the end of
the ASTM website. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E983–05
2
5.1.2.10 Diffusion. terms are being changed. A dose of C/cm is equivalent to
4 2 2 2
5.1.3 Charge accumulation in materials of poor electrical 10 C/m , while 1mA/cm is equivalent to 10A/m .
conductivity leading to specimen changes which include (21, 7.1.2 Specimenmaterialmodificationcanoftenberelatedto
22, 5) (see Chapter 8): the electron dose (D); that is, the number of elect
...

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ASTM E983-19(Guide)
Standard Guide for Minimizing Unwanted Electron Beam Effects in Auger Electron Spectroscopy

SIGNIFICANCE AND USE
4.1 When electron beam excitation is used in AES, the incident electron beam can interact with the specimen material causing physical and chemical changes. In general, these effects are a hindrance to AES analysis because they cause localized specimen modification (1-4).5  
4.2 With specimens that have poor electrical conductivity the electron beam can stimulate the development of localized charge on the specimen surface. This effect is a hindrance to AES analysis because the potentials associated with the charge can either adversely affect the integrity of Auger data or make Auger data collection difficult (5, 6).
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1.1 This guide outlines the origins and manifestations of unwanted electron beam effects in Auger electron spectroscopy (AES).  
1.2 Some general guidelines are provided concerning the electron beam parameters which are most likely to produce these effects and suggestions are offered on how to minimize them.  
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5.1 Background subtraction techniques in AES were originally employed as a method of enhancement of the relatively weak Auger signals to distinguish them from the slowly varying background of secondary and backscattered electrons. Interest in obtaining useful information from the Auger peak line shape, concern for greater quantitative accuracy from Auger spectra, and improvements in data gathering techniques, have led to the development of various background subtraction techniques.  
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SCOPE
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5.1 Turbidity is a measure of scattered light that results from the interaction between a beam of light and particulate material in a liquid sample. Particulate material is typically undesirable in water from a health perspective and its removal is often required when the water is intended for consumption. Thus, turbidity has been used as a key indicator for water quality to assess the health and quality of environmental water sources. Higher turbidity values are typically associated with poorer water quality.  
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SCOPE
1.1 This guide covers the best practices for use of various turbidimeter designs for measurement of turbidity in waters including: drinking water, wastewater, industrial waters, and for regulatory and environmental monitoring. This guide covers both continuous and static measurements.  
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5.1 Cryo-TEM is a technique used to record high resolution images of samples that are frozen and embedded in a thin layer of vitrified, amorphous ice (2-5). Because vitrification occurs so rapidly, the resultant specimen is almost instantly frozen, yielding a very accurate representation of the specimen at the moment of freezing, without the distortions typically associated with air drying delicate wet samples. Once frozen, images of the specimen are recorded at low temperature using a specially designed electron microscope equipped with a cryo-holder capable of operating under low dose conditions in order to prevent beam induced structural damage to the specimen. The cryo-TEM technique is the consensus choice to directly observe, analyze and accurately measure liposomes suspended in aqueous solutions. Fig. 1 illustrates this by comparing an electron micrograph from an air-dried negatively stained liposomal preparation with an electron micrograph of the same solution imaged by cryo-TEM.
FIG. 1 Left—An Electron Micrograph of an Air-Dried Liposomal Preparation that has been Negatively Stained with 2 % Uranyl Acetate for Contrast; Right—An Electron Micrograph of the Same Liposomal Preparation Prepared as a Frozen Vitrified Specimen for Cryo-TEM
Note 1: Both images are shown to the same scale; scale bar is 200 nm.  
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FIG. 1 SRM 2241 Measured on Four Commercial Raman Spectrometers Utilizing 785 nm Excitation  
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SCOPE
1.1 This guide is designed to enable the user to correct a Raman spectrometer for its relative spectral-intensity response function using NIST Standard Reference Materials2 in the 224X series (currently SRMs 2241, 2242, 2243, 2244, 2245, 2246), or a calibrated irradiance source. This relative intensity correction procedure will enable the intercomparison of Raman spectra acquired from differing instruments, excitation wavelengths, and laboratories.  
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Standard Practice for Describing Photomultiplier Detectors in Emission and Absorption Spectrometry

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This practice describes the photomultiplier properties that are essential to their judicious selection and use of in emission and absorption spectrometry. The properties covered here include structural features, electrical properties, and characteristics involved in precautions and problems. The structural features covered are envelope configurations, window materials, electrical connections, and housing for the external structure, and the photocathode, dynodes and anode, and rigidness of structural components for the internal structure. Electrical properties, on the other hand, incorporate the following: optical-electronic characteristics of the photocathode including spectral response; current amplification including gain per stage, overall gain, gain control (voltage-divider bridge), linearity of response, and anode saturation; signal nature; dark current including cathode size, internal aperture, and refrigeration effects; noise nature including additivity of noise power, signal-to-noise ratio, equivalent noise input; and photomultiplier properties as a component in an electrical circuit including output impedance, response time, and signal gating and integration possibilities. Finally, the characteristics involved in precautions and problems cover fatigue and hysteresis effects, illumination of photocathode, and gas leakage.
SCOPE
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Section  
Structural Features  
4  
General  
4.1  
External Structure  
4.2  
Internal Structure  
4.3  
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5  
General  
5.1  
Optical-Electronic Characteristics of the Photocathode  
5.2  
Current Amplification  
5.3  
Signal Nature  
5.4  
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5.5  
Noise Nature  
5.6  
Photomultiplier as a Component in an Electrical Circuit  
5.7  
Precautions and Problems  
6  
General  
6.1  
Fatigue and Hysteresis Effects  
6.2  
Illumination of Photocathode  
6.3  
Gas Leakage  
6.4  
Recommendations on Important Selection Criteria  
7  
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SCOPE
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SCOPE
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1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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4.2 A laboratory may implement this practice or an X-ray fluorescence method in partnership with a manufacturer of the analytical instrumentation. If a laboratory chooses to consult with an instrument manufacturer, then the following should be considered. The laboratory should know the alloy matrices to be analyzed, elements and mass fraction ranges to be determined, and the expected performance requirements for each of these elements. The laboratory should inform the instrument manufacturer of these requirements so an analytical method may be developed which meets the laboratory’s expectations. Typically, instrument manufacturers customize the instrument configuration to satisfy the end-user’s requirements for elemental coverage, elemental precision, and detection limits. Instrument manufacturer developed analytical methods may include specific parameters for sample excitation, wavelengths, inter-element interference corrections, calibration and regression, equipment configuration/installation, and sample preparation requirements. Laboratories should have a basic understanding of the parameters derived by the manufacturer.
SCOPE
1.1 This practice covers the components of a wavelength dispersive X-ray spectrometer that are basic to its operation and to the quality of its performance. It is not the intent of this practice to specify component tolerances or performance criteria, as these are unique for each instrument. However, the practice does attempt to identify which tolerances are critical and thus which should be specified.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 7.  
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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