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ASTM E2108-05

(Practice)

Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer

Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer

SCOPE
1.1 This practice describes a procedure for calibrating the electron binding-energy (BE) scale of an X-ray photoelectron spectrometer that is to be used for surface analysis with unmonochromated aluminum or magnesium K X-rays or monochromated aluminum K X rays.
1.2 It is recommended that the BE scale be calibrated after the instrument is installed or modified in any substantive way. Also, it is recommended that the instrumental BE scale be checked, and if necessary, recalibrated at intervals chosen to ensure that BE measurements are statistically unlikely to be made with greater uncertainty than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst's needs. Information is provided by which an analyst can select an appropriate tolerance limit for the BE measurements and the frequency of calibration checks.
1.3 This practice is based on the assumption that the BE scale of the spectrometer is sufficiently close to linear that the BE scale can be calibrated by measurements of reference photoelectron lines made near the extremes of the working BE scale. In most commercial instruments, X-ray sources with aluminum or magnesium anodes are employed and BEs are typically measured over the 0-1000 eV range. This practice can be used for the BE range from 0 eV to 1040 eV.
1.4 The assumption that the BE scale is linear is checked by a measurement made with a reference photoelectron line or Auger-electron line that appears at an intermediate position. A single check is a necessary but not sufficient condition for establishing linearity of the BE scale. Additional checks can be made with specified reference lines on instruments equipped with magnesium or unmonochromated aluminum X-ray sources, with secondary BE standards, or by following the procedures of the instrument manufacturer. Deviations from BE-scale linearity can occur because of mechanical misalignments, excessive magnetic fields in the region of the analyzer, or imperfections or malfunctions in the power supplies. This practice does not check for, nor identify, problems of this type.
1.5 After an initial check of the BE-scale linearity and measurements of the repeatability standard deviation for the main calibration lines for a particular instrument, a simplified procedure is given for routine checks of the calibration at subsequent times.
1.6 This practice is recommended for use with X-ray photoelectron spectrometers operated in the constant-pass-energy or fixed-analyzer-transmission mode and for which the pass energy is less than 200 eV; otherwise, depending on the configuration of the instrument, a relativistic equation could be needed for the calibration equation. The practice should not be used for instruments operated in the constant-retardation-ratio mode at retardation ratios less than 10, for instruments with an energy resolution worse than 1.5 eV, or in applications for which BE measurements are desired with tolerance limits of 0.03 eV or less.
1.7 On instruments equipped with a monochromated aluminum K X-ray source, a measurement of the position of a specified Auger-electron line can be used, if desired, to determine the average energy of the X rays incident on the specimen. This information is needed for the determination of modified Auger parameters.
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
31-Oct-2005
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E42 - Surface Analysis
Drafting Committee
E42.03 - Auger Electron Spectroscopy and X-Ray Photoelectron Spectroscopy
Current Stage
Ref Project

Relations

Replaced By
ASTM E2108-10 - Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
Effective Date
01-Nov-2010

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ASTM E2108-05 - Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron SpectrometerASTM E2108-05 - Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
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ASTM E2108-05 - Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer
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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: E2108 – 05
Standard Practice for
Calibration of the Electron Binding-Energy Scale of an
1
X-Ray Photoelectron Spectrometer
This standard is issued under the fixed designation E2108; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope 1.5 After an initial check of the BE-scale linearity and
measurements of the repeatability standard deviation for the
1.1 This practice describes a procedure for calibrating the
main calibration lines for a particular instrument, a simplified
electron binding-energy (BE) scale of an X-ray photoelectron
procedure is given for routine checks of the calibration at
spectrometer that is to be used for surface analysis with
subsequent times.
unmonochromated aluminum or magnesium Kα X-rays or
1.6 This practice is recommended for use with X-ray
monochromated aluminum Kα X rays.
photoelectron spectrometers operated in the constant-pass-
1.2 It is recommended that the BE scale be calibrated after
energy or fixed-analyzer-transmission mode and for which the
the instrument is installed or modified in any substantive way.
pass energy is less than 200 eV; otherwise, depending on the
Also, it is recommended that the instrumental BE scale be
configurationoftheinstrument,arelativisticequationcouldbe
checked, and if necessary, recalibrated at intervals chosen to
needed for the calibration equation.The practice should not be
ensure that BE measurements are statistically unlikely to be
used for instruments operated in the constant-retardation-ratio
made with greater uncertainty than a tolerance limit, specified
mode at retardation ratios less than 10, for instruments with an
by the analyst, based on the instrumental stability and the
energy resolution worse than 1.5 eV, or in applications for
analyst’s needs. Information is provided by which an analyst
whichBEmeasurementsaredesiredwithtolerancelimitsof 6
can select an appropriate tolerance limit for the BE measure-
0.03 eV or less.
ments and the frequency of calibration checks.
1.7 On instruments equipped with a monochromated alumi-
1.3 This practice is based on the assumption that the BE
num Kα X-ray source, a measurement of the position of a
scale of the spectrometer is sufficiently close to linear that the
specified Auger-electron line can be used, if desired, to
BE scale can be calibrated by measurements of reference
determine the average energy of the X rays incident on the
photoelectron lines made near the extremes of the working BE
specimen. This information is needed for the determination of
scale. In most commercial instruments, X-ray sources with
modified Auger parameters.
aluminum or magnesium anodes are employed and BEs are
1.8 This standard does not purport to address all of the
typically measured over the 0–1000 eV range. This practice
safety concerns, if any, associated with its use. It is the
can be used for the BE range from 0 eV to 1040 eV.
responsibility of the user of this standard to establish appro-
1.4 TheassumptionthattheBEscaleislinearischeckedby
priate safety and health practices and determine the applica-
a measurement made with a reference photoelectron line or
bility of regulatory limitations prior to use.
Auger-electron line that appears at an intermediate position.A
single check is a necessary but not sufficient condition for
2. Referenced Documents
establishinglinearityoftheBEscale.Additionalcheckscanbe
2
2.1 ASTM Standards:
made with specified reference lines on instruments equipped
E456 Terminology Relating to Quality and Statistics
with magnesium or unmonochromated aluminum X-ray
E673 Terminology Relating to Surface Analysis
sources, with secondary BE standards, or by following the
E902 PracticeforCheckingtheOperatingCharacteristicsof
procedures of the instrument manufacturer. Deviations from
X-Ray Photoelectron Spectrometers
BE-scale linearity can occur because of mechanical misalign-
E1016 Guide for Literature Describing Properties of Elec-
ments, excessive magnetic fields in the region of the analyzer,
trostatic Electron Spectrometers
or imperfections or malfunctions in the power supplies. This
E1078 Guide for Specimen Preparation and Mounting in
practice does not check for, nor identify, problems of this type.
Surface Analysis
1
This practice is under the jurisdiction of ASTM Committee E42 on Surface
AnalysisandisthedirectresponsibilityofSubcommitteeE42.03onAugerElectron
2
Spectroscopy and X-Ray Photoelectron Spectroscopy. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2005. Published December 2005. Originally contact ASTM Customer Servi
...

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5.1 Auger electron spectroscopy and X-ray photoelectron spectroscopy are used extensively for the surface analysis of materials. This practice summarizes methods for determining the specimen area contributing to the detected signal (a) for instruments in which a focused electron beam can be scanned over a region with dimensions greater than the dimensions of the specimen area viewed by the analyzer, and (b) by employing a sample with a sharp edge.  
5.2 This practice is intended as a means for determining the observed specimen area for selected conditions of operation of the electron energy analyzer. The observed specimen area depends on whether or not the electrons are retarded before energy analysis, the analyzer pass energy or retarding ratio if the electrons are retarded before energy analysis, the size of selected slits or apertures, and the value of the electron energy to be measured. The observed specimen area depends on these selected conditions of operation and also can depend on the adequacy of alignment of the specimen with respect to the electron energy analyzer.  
5.3 Any changes in the observed specimen area as a function of measurement conditions, for example, electron energy or analyzer pass energy, may need to be known if the specimen materials in regular use have lateral inhomogeneities with dimensions comparable to the dimensions of the specimen area viewed by the analyzer.  
5.4 This practice can give useful information on the imaging properties of the electron energy analyzer for particular conditions of operation. This information can be helpful in comparing analyzer performance with manufacturer's specifications.  
5.5 Information about the shape and size of the area viewed by the analyzer can also be employed to predict the signal intensity in XPS experiments when the sample is rotated and to assess the axis of rotation of the sample manipulator.  
5.6 Examples of the application of the methods described in this practice have been publis...
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1.1 This practice describes methods for determining the specimen area contributing to the detected signal in Auger electron spectrometers and some types of X-ray photoelectron spectrometers (spectrometer analysis area) when this area is defined by the electron collection lens and aperture system of the electron energy analyzer. The practice is applicable only to those X-ray photoelectron spectrometers in which the specimen area excited by the incident X-ray beam is larger than the specimen area viewed by the analyzer, in which the photoelectrons travel in a field-free region from the specimen to the analyzer entrance. Some of the methods described here require an auxiliary electron gun mounted to produce an electron beam of variable energy on the specimen (“electron-gun method”). Other experiments require a sample with a sharp edge, such as a wafer covered with a uniform clean layer (for example, gold (Au) or silver (Ag)) and cleaved to obtain a long side (“sharp-edge method”).  
1.2 This practice is recommended as a useful means for determining the specimen area viewed by the analyzer for different conditions of spectrometer operation, for verifying adequate specimen and beam alignment, and for characterizing the imaging properties of the electron energy analyzer.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
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ASTM E2426-10(2019)(Practice)
Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS

SIGNIFICANCE AND USE
5.1 Electron multipliers are commonly used in pulse-counting mode to detect ions from magnetic sector mass spectrometers. The electronics used to amplify, detect and count pulses from the electron multipliers always have a characteristic time interval after the detection of a pulse, during which no other pulses can be counted. This characteristic time interval is known as the “dead time.” The dead time has the effect of reducing the measured count rate compared with the “true” count rate.  
5.2 In order to measure count rates accurately over the entire dynamic range of a pulse counting detector, such as an electron multiplier, the dead time of the entire pulse counting system must be well known. Accurate count rate measurement forms the basis of isotopic ratio measurements as well as elemental abundance determinations.  
5.3 The procedure described herein has been successfully used to determine the dead time of counting systems on SIMS instruments.6 The accurate determination of the dead time by this method has been a key component of precision isotopic ratio measurements made by SIMS.
SCOPE
1.1 This practice provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a method for determining the dead time of the pulse-counting detection systems on the instrument. This practice also allows the analyst to determine whether the apparent dead time is independent of count rate.  
1.2 This practice is applicable to most types of mass spectrometers that have pulse-counting detectors.  
1.3 This practice does not describe methods for precise or accurate isotopic ratio measurements.  
1.4 This practice does not describe methods for the proper operation of pulse counting systems and detectors for mass spectrometry.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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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