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ASTM E1504-11(2019)

(Practice)

Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)

Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)

SIGNIFICANCE AND USE
5.1 This practice is intended for use in reporting the experimental and data reduction procedures described in other publications.
SCOPE
1.1 This practice provides the minimum information necessary to describe the instrumental, experimental, and data reduction procedures used in acquiring and reporting secondary ion mass spectrometry (SIMS) mass spectral data.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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.

General Information

Status
Published
Publication Date
31-Oct-2019
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E42 - Surface Analysis
Drafting Committee
E42.06 - SIMS
Current Stage
Ref Project

Relations

Replaces
ASTM E1504-11 - Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)
Effective Date
01-Nov-2019
Refers
ASTM E673-03 - Standard Terminology Relating to Surface Analysis (Withdrawn 2012)
Effective Date
01-Dec-2003
Refers
ASTM E673-02a - Standard Terminology Relating to Surface Analysis
Effective Date
10-Dec-2002
Refers
ASTM E673-01 - Standard Terminology Relating to Surface Analysis
Effective Date
10-Nov-2001
Refers
ASTM E673-98E1 - Standard Terminology Relating to Surface Analysis
Effective Date
10-Nov-2001
Referred By
ASTM F2847-17 - Standard Practice for Reporting and Assessment of Residues on Single-Use Implants and Single-Use Sterile Instruments
Effective Date
01-Nov-2019
Referred By
ASTM E1635-06(2019) - Standard Practice for Reporting Imaging Data in Secondary Ion Mass Spectrometry (SIMS)
Effective Date
01-Nov-2019

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ASTM E1504-11(2019) - Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)ASTM E1504-11(2019) - Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)
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ASTM E1504-11(2019) - Standard Practice for Reporting Mass Spectral Data in Secondary Ion Mass Spectrometry (SIMS)
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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.
Designation: E1504 − 11 (Reapproved 2019)
Standard Practice for
Reporting Mass Spectral Data in Secondary Ion Mass
Spectrometry (SIMS)
This standard is issued under the fixed designation E1504; 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.
1. Scope standardize the reporting of such data to facilitate comparisons
with other laboratories and analytical techniques.
1.1 This practice provides the minimum information neces-
sary to describe the instrumental, experimental, and data
5. Significance and Use
reduction procedures used in acquiring and reporting second-
5.1 This practice is intended for use in reporting the
ary ion mass spectrometry (SIMS) mass spectral data.
experimental and data reduction procedures described in other
1.2 The values stated in SI units are to be regarded as
publications.
standard. No other units of measurement are included in this
standard.
6. Information to be Reported
1.3 This standard does not purport to address all of the
6.1 Instrumentation:
safety concerns, if any, associated with its use. It is the
6.1.1 If a standard commercial SIMS instrument is used,
responsibility of the user of this standard to establish appro-
specify the manufacturer, model number, and type of analyzer
priate safety, health, and environmental practices and deter-
used. Specify the manufacturer and model number of any
mine the applicability of regulatory limitations prior to use.
accessory or auxiliary equipment that would affect the data
1.4 This international standard was developed in accor-
contained within the mass spectrum (for example, additional
dance with internationally recognized principles on standard-
vacuum pumping attachments, primary ion mass filter, primary
ization established in the Decision on Principles for the
ion sources, electron flood guns, etc.). If any nonstandard
Development of International Standards, Guides and Recom-
modification has been made to the instrumentation, describe
mendations issued by the World Trade Organization Technical
the modification in detail.
Barriers to Trade (TBT) Committee.
6.1.2 If a noncommercial SIMS system is used, specify the
components composing the system (for example, ion gun,
2. Referenced Documents
pumping system, vacuum chamber, and mass filter). Specify
2.1 ASTM Standards:
the manufacturer and model number if the components are of
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
commercial origin. If the components are home-built, specify
2012)
them in such detail that their potential effect on the obtained
mass spectrum may be deduced by an individual experienced
3. Terminology
in SIMS and vacuum technology.
3.1 Definitions—For definitions of terms used in this
6.2 Specimen—Describe the specimen in as much detail as
practice, refer to Terminology E673.
possible. Such factors would include, but are not limited to,
4. Summary of Practice sample preparation and handling, sample history, bulk and
trace composition, physical dimensions, sample homogeneity,
4.1 Experimental conditions and reporting procedures that
crystallinity, and any preanalysis cleaning procedure used.
affect SIMS mass spectral data are presented in order to
Describe in detail the method of sample mounting. Describe
any conductive coating or grids placed on the sample for
This practice is under the jurisdiction of ASTM Committee E42 on Surface
charge compensation. If a substrate is used, include substrate
Analysis and is the direct responsibility of Subcommittee E42.06 on SIMS.
composition, purity, and any methods of cleaning.
Current edition approved Nov. 1, 2019. Published November 2019. Originally
approved in 1992. Last previous edition approved in 2011 as E1504 – 11. DOI:
6.3 Experimental Conditions:
10.1520/E1504-11R19.
6.3.1 Primary Ion Source and Ion Optical Column—If a
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
commercial ion source is being used, then the manufacturer
Standards volume information, refer to the standard’s Document Summary page on
and model number should be specified. If the ion source is a
the ASTM website.
3 custom design, then it should be described in detail and
The last approved version of this historical standard is referenced on
www.astm.org. appropriate literature references given, if applicable. The
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1504 − 11 (2019)
species extracted from the ion source must be specified. If the should be specified. Specify and describe the type of secondary
primary ion column provides mass filtering, then the selected ion detection system used (such as, Faraday cup, pulse-
ma
...

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4.1 The purpose of this guide is assist users and analysts in selecting the standardization procedures relevant to a defined XPS experiment. These experiments may be based, for example, upon material failure analysis, the determination of surface chemistry of a solid, or the composition profile of a thin film or coating. A series of options will be summarized giving the standards that are related to specific information requirements. ISO 15470 and ISO 10810 also aid XPS users in experiment design for typical samples. ASTM Committee E42 and ISO TC201 are in a continuous process of updating and adding standards and guides. It is recommended to refer to the ASTM and ISO websites for a current list of standards.
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1.1 This guide describes an approach to enable users and analysts to determine the calibrations and standards useful to obtain meaningful surface chemistry data with X-ray photoelectron spectroscopy (XPS) and to optimize the instrument for specific analysis objectives and data collection time.  
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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),  
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4.1 Auger electron spectroscopy is often capable of yielding information concerning the chemical and physical environment of atoms in the near-surface region of a solid as well as giving elemental and quantitative information. This information is manifested as changes in the observed Auger electron spectrum for a particular element in the specimen under study compared to the Auger spectrum produced by the same element when it is in some reference form. The differences in the two spectra are said to be due to a chemical effect or a matrix effect. Despite sometimes making elemental identification and quantitative measurements more difficult, these effects in the Auger spectrum are considered valuable tools for characterizing the environment of the near-surface atoms in a solid.
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Standard Practice for Determination of the Specimen Area Contributing to the Detected Signal in Auger Electron Spectrometers and Some X-Ray Photoelectron Spectrometers

SIGNIFICANCE AND USE
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.  
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SIGNIFICANCE AND USE
5.1 This practice is used for reporting the experimental conditions as specified in Section 6 in the “Methods” or “Experimental” sections of other publications (subject to editorial restrictions).  
5.2 The report would include specific conditions for each data set, particularly, if any parameters are changed for different sputter depth profile data sets in a publication. For example, footnotes of tables or figure captions would be used to specify differing conditions.
SCOPE
1.1 This practice covers the information needed to describe and report instrumentation, specimen parameters, experimental conditions, and data reduction procedures. SIMS sputter depth profiles can be obtained using a wide variety of primary beam excitation conditions, mass analysis, data acquisition, and processing techniques (1-4).2  
1.2 Limitations—This practice is limited to conventional sputter depth profiles in which information is averaged over the analyzed area in the plane of the specimen. Ion microprobe or microscope techniques permitting lateral spatial resolution of secondary ions within the analyzed area, for example, image depth profiling, are excluded.  
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5.1 This practice is to be used for reporting the experimental and data reduction procedures to be described with the publication of the data.
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1.1 This practice lists the minimum information necessary to describe the instrumental, experimental, and data reduction procedures used in acquiring and reporting images generated by secondary ion mass spectrometry (SIMS).  
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Standard Guide for Performing Sputter Crater Depth Measurements

SIGNIFICANCE AND USE
4.1 Sputter crater depth measurements are performed in order to determine a sputter rate (depth/time) for each matrix sputtered during a sputter depth profile or similar in-depth type analyses. From sputter rate values, a linear depth scale can be calculated and displayed for the sputter depth profile.  
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1.1 This guide covers the preferred procedure for acquiring and post-processing of sputter crater depth measurements. This guide is limited to stylus-type surface profilometers equipped with a stage, stylus, associated scan and sensing electronics, video system for sample and scan alignment, and computerized system.  
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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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ASTM E2108-16(Practice)
Standard Practice for Calibration of the Electron Binding-Energy Scale of an X-Ray Photoelectron Spectrometer

SIGNIFICANCE AND USE
5.1 X-ray photoelectron spectroscopy is used extensively for the surface analysis of materials. Elements (with the exception of hydrogen and helium) are identified from comparisons of the binding energies determined from photoelectron spectra with tabulated values. Information on chemical state can be derived from the chemical shifts of measured photoelectron and Auger-electron features with respect to those measured for elemental solids.  
5.2 Calibrations of the BE scales of XPS instruments are required for four principal reasons. First, meaningful comparison of BE measurements from two or more XPS instruments requires that the BE scales be calibrated, often with an uncertainty of about 0.1 eV to 0.2 eV. Second, identification of chemical state is based on measurement of chemical shifts of photoelectron and Auger-electron features, again with an uncertainty of typically about 0.1 eV to 0.2 eV; individual measurements, therefore, should be made and literature sources need to be available with comparable or better accuracies. Third, the availability of databases (3) of measured BEs for reliable identification of elements and determination of chemical states by computer software requires that published data and local measurements be made with uncertainties of about 0.1 eV to 0.2 eV. Finally, the growing adoption of quality management systems, such as, ISO 9001:2015, in many analytical laboratories has led to requirements that the measuring and test equipment be calibrated and that the relevant measurement uncertainties be known.  
5.3 The actual uncertainty of a BE measurement depends on instrument properties and stability, measurement conditions, and the method of data analysis. This practice makes use of tolerance limits ±δ (chosen, for example, at the 95 % confidence level) that represent the maximum likely uncertainty of a BE measurement, associated with the instrument in a specified time interval following a calibration (ISO 15472:2010). A user should select a...
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 performing spectroscopic analysis of photoelectrons excited by unmonochromated aluminum or magnesium Kα X-rays or by monochromated aluminum Kα X-rays.  
1.2 The calibration of the BE scale is recommended after the instrument is installed or modified in any substantive way. Additional checks and, if necessary, recalibrations are recommended at intervals chosen to ensure that BE measurements are statistically unlikely to be made with an uncertainty greater than a tolerance limit, specified by the analyst, based on the instrumental stability and the analyst’s needs. Information is provided by which the 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 to allow for calibration by measurements of reference photoelectron lines having BEs 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 at least over the 0–1200 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, ...

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