SIGNIFICANCE AND USE
4.1 This compilation is limited to artifacts observed in scanning tunneling microscopes and contact-mode atomic force microscopes. In particular, this document focuses on artifacts related to probe motion and geometrical considerations of the tip and surface interaction. Many of the artifacts described here extend to other scanned probe microscopies where piezoscanners are used as positioning elements or where tips of similar geometries are used. These are not the only artifacts associated with measurements obtained by STM or AFM. Artifacts can also arise from the following: control electronics (for example, improper feedback gains); noise (mechanical, acoustic, or electronic); drift (thermal or mechanical); problems unique to signal detection methods (for example, laser spillover in optical lever schemes); improper use of image processing (real time or post processed); sample preparation, environment (for example, humidity) and tip-surface interaction (for example, excessive electrostatic, adhesive, shear, and compressive forces). It is suggested that these other types of artifacts form the basis of future ASTM guides.
SCOPE
1.1 All microscopes are subject to artifacts. The purpose of this document is to provide a description of commonly observed artifacts in scanning tunneling microscopy (STM) and atomic force microscopy (AFM) relating to probe motion and geometric considerations of the tip and surface interaction, provide literature references of examples and, where possible, to offer an interpretation as to the source of the artifact. Because the scanned probe microscopy field is a burgeoning one, this document is not meant to be comprehensive but rather to serve as a guide to practicing microscopists as to possible pitfalls one may expect. The ability to recognize artifacts should assist in reliable evaluation of instrument operation and in reporting of data.  
1.2 A limited set of terms will be defined here. A full description of terminology relating to the description, operation, and calibration of STM and AFM instruments is beyond the scope of this document.  
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 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.

  • Guide
    20 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
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.  
1.2 This guide offers an organized collection of information or a series of options and does not recommend a specific course of action. This guide cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this guide will be applicable in all circumstances.  
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 is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title of this document means only that the document has been approved through the ASTM consensus process.  
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.

  • Guide
    6 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
4.1 Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation 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 in the preparation and mounting process. The goal must be to preserve the state of the surface so that the analysis remains representative of the original.  
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1)4 or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.  
4.3 This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.  
4.4 Guide E1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following 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 and ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will 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 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.

  • Guide
    10 pages
    English language

SIGNIFICANCE AND USE
4.1 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.  
4.2 AES, XPS, and 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).4  
4.3 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 E1078 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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.

  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
5.1 Pressing cryosections flat onto a conducting substrate has been one of the most challenging problems in SIMS analysis of cryogenically prepared tissue specimens. Frozen cryosections often curl or peel off, or both, from the substrate during freeze-drying. The curling of cryosections results in an uneven sample surface for SIMS analysis. Furthermore, if freeze-dried cryosections are not attached tightly to the substrate, the impact of the primary ion beam may result in further curling and even dislodging of the cryosection from the substrate. These problems render SIMS analysis difficult, frustrating and time consuming. The use of indium as a substrate for pressing cryosections flat has provided a practical approach for analyzing cryogenically prepared tissue specimens (1).4  
5.2 The procedure described herein has been successfully used for SIMS imaging of calcium and magnesium transport and localization of anticancer drugs in animal models (2, 3, 4, 5).  
5.3 The procedure described here is amenable to soft tissues of both animal and plant origin.
SCOPE
1.1 This practice provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a method for analyzing tissue cryosections in the imaging mode of the instrument. This practice is suitable for frozen-freeze-dried and frozen-hydrated cryosection analysis.  
1.2 This practice does not describe methods for optimal freezing of the specimen for immobilizing diffusible chemical species in their native intracellular sites.  
1.3 This practice does not describe methods for obtaining cryosections from a frozen specimen.  
1.4 This practice is not suitable for any plastic embedded tissues.  
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.

  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
5.1 The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.  
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).  
1.3 The values stated in inch-pound 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.  
1.5 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.

  • Guide
    4 pages
    English language

SIGNIFICANCE AND USE
5.1 The presence of cell growth medium complicates a direct analysis of cells with SIMS. Attempts to wash out the nutrient medium results in the exposure of cells to unphysiological reagents that may also alter their chemical composition. This obstacle is overcome by using a sandwich freeze-fracture method (1). This cryogenic method has provided a unique way of sampling individual cells in their native state for SIMS analysis.  
5.2 The procedure described here has been successfully used for imaging Na+ and K+ ion transport  (3), calcium alterations in stimulated cells (4,5), and localization of therapeutic drugs and isotopically labeled molecules in single cells (6). The frozen freeze-dried cells prepared according to this method have been checked for SIMS matrix effects  (7). Ion image quantification has also been achieved in this sample type (8).  
5.3 The procedure described here is amenable to a wide variety of cell cultures and provides a way for studying the response of individual cells for chemical alterations in the state of health and disease and localization of isotopically-labeled molecules and theraputic drugs in cell culture models.
SCOPE
1.1 This guide provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a cryogenic method for analyzing individual tissue culture cells growing in vitro. This guide is suitable for frozen-hydrated and frozen-freeze-dried sample types. Included are procedures for correlating optical, laser scanning confocal and secondary electron microscopies to complement SIMS analysis.  
1.2 This guide is not suitable for cell cultures that do not attach to the substrate.  
1.3 This guide is not suitable for any plastic embedded cell culture specimens.  
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.  
1.5 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.

  • Guide
    3 pages
    English language

SIGNIFICANCE AND USE
5.1 Although it would be desirable to measure the extent of profile distortion in any unknown sample by using a standard sample and this guide, measurements of interface width (profile distortion) can be unique to every sample composition (1, 2).4 This guide, describes a method that determines the unique width of a particular interface for the chosen set of operating conditions. It is intended to provide a method for checking on proper or consistent, or both, instrument performance. Periodic analysis of the same sample followed by a measurement of the interface width, in accordance with this guide, will provide these checks.  
5.2 The procedure described in this guide is adaptable to any layered sample with an interface between layers in which a nominated element is present in one layer and absent from the other. It has been shown that for SIMS in particular (3, 4) and for surface analysis in general (5, 6), only rigorous calibration methods can determine accurate interface widths. Such procedures are prohibitively time-consuming. Therefore the interface width measurement obtained using the procedure described in this guide may contain significant systematic error (7). Therefore, this measure of interface width may have no relation to similar measures made with other methods. However, this does not diminish its use as a check on proper or consistent instrument performance, or both.  
5.3 This guide can be used for both elemental and molecular depth profiles, provided that the materials have constant sputter rates throughout the depth of the overlayer, and minimal interlayer mixing is occurring. For more detailed information regarding measurements of interface widths during organic depth profiling, please see Mahoney (8).
SCOPE
1.1 This guide provides the SIMS analyst with a method for determining the width of interfaces from SIMS sputtering data obtained from analyses of layered specimens (both organic and inorganic). This guide does not apply to data obtained from analyses of specimens with thin markers or specimens without interfaces such as ion-implanted specimens.  
1.2 This guide does not describe methods for the optimization of interface width or the optimization of depth resolution.  
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.

  • Guide
    3 pages
    English language

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.  
4.2 Data obtained from surface profilometry are useful in monitoring instrumental parameters (for example, raster size, shape, and any irregularities in topography of the sputtered crater) used for depth profiles.
SCOPE
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.  
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.

  • Guide
    3 pages
    English language

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.  
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...
SCOPE
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.  
1.5 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 Recomm...

  • Standard
    9 pages
    English language

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.

  • Standard
    2 pages
    English language

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.  
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.  
1.5 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.

  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
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).  
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.

  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.  
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
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.  
1.5 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.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

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).
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

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.

  • Standard
    3 pages
    English language

SCOPE
1.1 This standard specifies the dimensions of knife-edge style flanges and their associated gaskets used in vacuum systems for pressures ranging from 105 Pa to 10-11 Pa. Such flanges are widely used throughout vacuum technology applications in semiconductor processing tools, surface analysis systems, space simulation systems, and general research requiring vacuum.  
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the 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.

  • Technical specification
    4 pages
    English language

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, ...

  • Standard
    17 pages
    English language
  • Standard
    17 pages
    English language

SIGNIFICANCE AND USE
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.  
5.2 Similarly, the use of background subtraction techniques in XPS has evolved mainly from the interest in the determination of chemical states (from the binding-energy values for component peaks that may often overlap), greater quantitative accuracy from the XPS spectra, and improvements in data acquisition. Post-acquisition background subtraction is normally applied to XPS data.  
5.3 The procedures outlined in Section 7 are popular in XPS and AES; less popular procedures and rarely used procedures are described in Sections 8 and 9, respectively. General reviews of background subtraction methods and curve-fitting techniques have been published elsewhere (1-5).6  
5.4 Background subtraction is commonly performed prior to peak fitting, although it can be assessed (fitted) during peak fitting (active approach  (6, 7)). Some commercial data analysis packages require background removal before peak fitting. Nevertheless, a measured spectral region consisting of one or more peaks and background intensities due to inelastic scattering, Bremsstrahlung (for XPS with unmonochromated X-ray sources), and scattered primary electrons (for AES) can often be satisfactorily represented by applying peak functions for each component with parameters for each one determined in a single least-squares fit. The choice of the background to be removed, if required or desired, before or during peak fitting is suggested by the experience of the analysts, the capabilities of the peak fitting software, and the p...
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with the principal background subtraction techniques presently in use together with the nature of their application to data acquisition and manipulation.  
1.2 This guide is intended to apply to background subtraction in electron, X-ray, and ion-excited Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS).  
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    6 pages
    English language
  • Guide
    6 pages
    English language

SIGNIFICANCE AND USE
5.1 Auger electron spectroscopy yields information concerning the chemical and physical state of a solid surface in the near surface region. Nondestructive depth profiling is limited to this near surface region. Techniques for measuring the crater depths and film thicknesses are given in (1).5  
5.2 Ion sputtering is primarily used for depths of less than the order of 1 μm.  
5.3 Angle lapping or mechanical cratering is primarily used for depths greater than the order of 1 μm.  
5.4 The choice of depth profiling methods for investigating an interface depends on surface roughness, interface roughness, and film thickness (2).  
5.5 The depth profile interface widths can be measured using a logistic function which is described in Practice E1636.
SCOPE
1.1 This guide covers procedures used for depth profiling in Auger electron spectroscopy.  
1.2 Guidelines are given for depth profiling by the following:    
Section  
Ion Sputtering  
6  
Angle Lapping and Cross-Sectioning  
7  
Mechanical Cratering  
8  
Mesh Replica Method  
9  
Nondestructive Depth Profiling  
10  
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 problems, 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.

  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
5.1 The acquisition of chemical information from variations in the energy position of peaks in the XPS spectrum is of primary interest in the use of XPS as a surface analytical tool. Surface charging acts to shift spectral peaks independent of their chemical relationship to other elements on the same surface. The desire to eliminate the influence of surface charging on the peak positions and peak shapes has resulted in the development of several empirical methods designed to assist in the interpretation of the XPS peak positions, determine surface chemistry, and allow comparison of spectra of conducting and non-conducting systems of the same element. It is assumed that the spectrometer is generally working properly for non-insulating specimens (see Practice E902).  
5.2 Although highly reliable methods have now been developed to stabilize surface potentials during XPS analysis of most materials (5, 6), no single method has been developed to deal with surface charging in all circumstances (10, 11). For insulators, an appropriate choice of any control or referencing system will depend on the nature of the specimen, the instruments, and the information needed. The appropriate use of charge control and referencing techniques will result in more consistent, reproducible data. Researchers are strongly urged to report both the control and referencing techniques that have been used, the specific peaks and binding energies used as standards (if any), and the criteria applied in determining optimum results so that the appropriate comparisons may be made.
SCOPE
1.1 This guide acquaints the X-ray photoelectron spectroscopy (XPS) user with the various charge control and charge shift referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens and provides information needed for reporting the methods used to customers or in the literature.  
1.2 This guide is intended to apply to charge control and charge referencing techniques in XPS and is not necessarily applicable to electron-excited systems.  
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    7 pages
    English language
  • Guide
    7 pages
    English language

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).4  
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).
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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.

  • Guide
    4 pages
    English language
  • Guide
    4 pages
    English language

SIGNIFICANCE AND USE
5.1 Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.  
5.2 Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.  
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.  
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.  
1.5 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.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
4.1 Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation 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 in the preparation and mounting process. The goal must be to preserve the state of the surface so that the analysis remains representative of the original.  
4.2 AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1)4 or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.  
4.3 This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.  
4.4 Guide E1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following 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 and ESCA), and  
1.1.3 Secondary ion mass spectrometry (SIMS).  
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will 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 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    10 pages
    English language
  • Guide
    10 pages
    English language

SIGNIFICANCE AND USE
4.1 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.  
4.2 AES, XPS, and 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).4  
4.3 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 E1078 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.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
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.  
1.2 This guide offers an organized collection of information or a series of options and does not recommend a specific course of action. This guide cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this guide will be applicable in all circumstances.  
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 is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title of this document means only that the document has been approved through the ASTM consensus process.  
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.

  • Guide
    6 pages
    English language
  • Guide
    6 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
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.  
1.2 This guide offers an organized collection of information or a series of options and does not recommend a specific course of action. This guide cannot replace education or experience and should be used in conjunction with professional judgment. Not all aspects of this guide will be applicable in all circumstances.  
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 is not intended to represent or replace the standard of care by which the adequacy of a given professional service must be judged, nor should this document be applied without consideration of a project’s many unique aspects. The word “Standard” in the title of this document means only that the document has been approved through the ASTM consensus process.    
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.

  • Guide
    6 pages
    English language

SIGNIFICANCE AND USE
5.1 Pressing cryosections flat onto a conducting substrate has been one of the most challenging problems in SIMS analysis of cryogenically prepared tissue specimens. Frozen cryosections often curl or peel off, or both, from the substrate during freeze-drying. The curling of cryosections results in an uneven sample surface for SIMS analysis. Furthermore, if freeze-dried cryosections are not attached tightly to the substrate, the impact of the primary ion beam may result in further curling and even dislodging of the cryosection from the substrate. These problems render SIMS analysis difficult, frustrating and time consuming. The use of indium as a substrate for pressing cryosections flat has provided a practical approach for analyzing cryogenically prepared tissue specimens (1).4  
5.2 The procedure described herein has been successfully used for SIMS imaging of calcium and magnesium transport and localization of anticancer drugs in animal models (2, 3, 4, 5).  
5.3 The procedure described here is amenable to soft tissues of both animal and plant origin.
SCOPE
1.1 This practice provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a method for analyzing tissue cryosections in the imaging mode of the instrument. This practice is suitable for frozen-freeze-dried and frozen-hydrated cryosection analysis.  
1.2 This practice does not describe methods for optimal freezing of the specimen for immobilizing diffusible chemical species in their native intracellular sites.  
1.3 This practice does not describe methods for obtaining cryosections from a frozen specimen.  
1.4 This practice is not suitable for any plastic embedded tissues.  
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.

  • Standard
    2 pages
    English language
  • Standard
    2 pages
    English language

SIGNIFICANCE AND USE
5.1 The presence of cell growth medium complicates a direct analysis of cells with SIMS. Attempts to wash out the nutrient medium results in the exposure of cells to unphysiological reagents that may also alter their chemical composition. This obstacle is overcome by using a sandwich freeze-fracture method (1). This cryogenic method has provided a unique way of sampling individual cells in their native state for SIMS analysis.  
5.2 The procedure described here has been successfully used for imaging Na+ and K+ ion transport  (3), calcium alterations in stimulated cells (4,5), and localization of therapeutic drugs and isotopically labeled molecules in single cells (6). The frozen freeze-dried cells prepared according to this method have been checked for SIMS matrix effects  (7). Ion image quantification has also been achieved in this sample type (8).  
5.3 The procedure described here is amenable to a wide variety of cell cultures and provides a way for studying the response of individual cells for chemical alterations in the state of health and disease and localization of isotopically-labeled molecules and theraputic drugs in cell culture models.
SCOPE
1.1 This guide provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a cryogenic method for analyzing individual tissue culture cells growing in vitro. This guide is suitable for frozen-hydrated and frozen-freeze-dried sample types. Included are procedures for correlating optical, laser scanning confocal and secondary electron microscopies to complement SIMS analysis.  
1.2 This guide is not suitable for cell cultures that do not attach to the substrate.  
1.3 This guide is not suitable for any plastic embedded cell culture specimens.  
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    3 pages
    English language
  • Guide
    3 pages
    English language

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This guide outlines the types of chemical effects and matrix effects which are observed in Auger electron spectroscopy.  
1.2 Guidelines are given for the reporting of chemical and matrix effects in Auger spectra.  
1.3 Guidelines are given for utilizing Auger chemical effects for identification or characterization.  
1.4 This guide is applicable to both electron excited and X-ray excited Auger electron spectroscopy.  
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.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
4.1 This compilation is limited to artifacts observed in scanning tunneling microscopes and contact-mode atomic force microscopes. In particular, this document focuses on artifacts related to probe motion and geometrical considerations of the tip and surface interaction. Many of the artifacts described here extend to other scanned probe microscopies where piezoscanners are used as positioning elements or where tips of similar geometries are used. These are not the only artifacts associated with measurements obtained by STM or AFM. Artifacts can also arise from the following: control electronics (for example, improper feedback gains); noise (mechanical, acoustic, or electronic); drift (thermal or mechanical); problems unique to signal detection methods (for example, laser spillover in optical lever schemes); improper use of image processing (real time or post processed); sample preparation, environment (for example, humidity) and tip-surface interaction (for example, excessive electrostatic, adhesive, shear, and compressive forces). It is suggested that these other types of artifacts form the basis of future ASTM guides.
SCOPE
1.1 All microscopes are subject to artifacts. The purpose of this document is to provide a description of commonly observed artifacts in scanning tunneling microscopy (STM) and atomic force microscopy (AFM) relating to probe motion and geometric considerations of the tip and surface interaction, provide literature references of examples and, where possible, to offer an interpretation as to the source of the artifact. Because the scanned probe microscopy field is a burgeoning one, this document is not meant to be comprehensive but rather to serve as a guide to practicing microscopists as to possible pitfalls one may expect. The ability to recognize artifacts should assist in reliable evaluation of instrument operation and in reporting of data.  
1.2 A limited set of terms will be defined here. A full description of terminology relating to the description, operation, and calibration of STM and AFM instruments is beyond the scope of this document.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

  • Guide
    18 pages
    English language

SIGNIFICANCE AND USE
The analyst may use this document to obtain information on the properties of electron spectrometers and instrumental aspects associated with quantitative surface analysis.
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with some of the relevant literature describing the physical properties of modern electrostatic electron spectrometers.  
1.2 This guide is intended to apply to electron spectrometers generally used in Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS).  
1.3 The values stated in inch-pound 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    4 pages
    English language

SIGNIFICANCE AND USE
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.
Data obtained from surface profilometry are useful in monitoring instrumental parameters (for example, raster size, shape, and any irregularities in topography of the sputtered crater) used for depth profiles.
SCOPE
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    3 pages
    English language
  • Guide
    3 pages
    English language

SIGNIFICANCE AND USE
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.
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.
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.
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.
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.
Examples of the application of the methods described in this practice have been published (1-7).  
There are diffe...
SCOPE
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    9 pages
    English language
  • Standard
    9 pages
    English language

SIGNIFICANCE AND USE
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.
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.

  • Standard
    2 pages
    English language
  • Standard
    2 pages
    English language

SIGNIFICANCE AND USE
This practice is to be used for reporting the experimental and data reduction procedures to be described with the publication of the data.
SCOPE
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).
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
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).
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).  
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.
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
Although it would be desirable to measure the extent of profile distortion in any unknown sample by using a standard sample and this guide, measurements of interface width (profile distortion) can be unique to every sample composition (1, 2, 3).3 This guide, that describes a method that determines the unique width of a particular interface for the chosen set of operating conditions. It is primarily intended to provide a method for checking on proper or consistent, or both, instrument performance. Periodic analysis of the same sample followed by a measurement of the interface width, in accordance with this guide, will provide these checks.
The procedure described in this guide is adaptable to any layered sample with an interface between layers in which a nominated element is present in one layer and absent from the other. It has been shown that for SIMS in particular (4, 5) and for surface analysis in general (6, 7), only rigorous calibration methods can determine accurate interface widths. Such procedures are prohibitively time-consuming. Therefore the interface width measurement obtained using the procedure described in this guide may contain significant systematic error (8). Therefore, this measure of interface width may have no relation to similar measures made with other methods. However, this does not diminish its use as a check on proper or consistent instrument performance, or both.
SCOPE
1.1 This guide provides the SIMS analyst with a method for determining the width of interfaces from SIMS sputtering data obtained from analyses of layered specimens. This guide does not apply to data obtained from analyses of specimens with thin markers or specimens without interfaces such as ion-implanted specimens.
1.2 This guide does not describe methods for the optimization of interface width or the optimization of depth resolution.
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.

  • Guide
    3 pages
    English language
  • Guide
    3 pages
    English language

SIGNIFICANCE AND USE
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.
Similarly, the use of background subtraction techniques in XPS has evolved mainly from the interest in the determination of chemical states (from the binding-energy values for component peaks that may often overlap), greater quantitative accuracy from the XPS spectra, and improvements in data acquisition. Post-acquisition background subtraction is normally applied to XPS data.
The procedures outlined in Section 7 are popular in XPS and AES; less popular procedures and rarely used procedures are described in Sections 8 and 9, respectively. General reviews of background subtraction methods and curve-fitting techniques have been published (1-5).  
Background subtraction is usually done before peak fitting. Some commercial systems require background removal. Nevertheless, a measured spectral region consisting of one or more peaks and background intensities due to inelastic scattering, Bremsstrahlung (for XPS with unmonochromated X-ray sources), and scattered primary electrons (for AES) can often be satisfactorily represented by choosing functions for each intensity component with parameters for each component determined in a single least-squares fit. The choice of the background to be removed if required or desired before peak fitting is suggested by the experience of the analysts and the peak complexity as noted above.
SCOPE
1.1 The purpose of this guide is to familiarize the analyst with the principal background subtraction techniques presently in use together with the nature of their application to data acquisition and manipulation.
1.2 This guide is intended to apply to background subtraction in electron, X-ray, and ion-excited Auger electron spectroscopy (AES), and X-ray photoelectron spectroscopy (XPS).
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
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).  
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).
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.

  • Guide
    4 pages
    English language
  • Guide
    4 pages
    English language

SIGNIFICANCE AND USE
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.
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 9001:2000, in many analytical laboratories has led to requirements that the measuring and test equipment be calibrated and that the relevant measurement uncertainties be known.
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 15472:2001). A user should select a value of δ ba...
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 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 ma...

  • Standard
    16 pages
    English language
  • Standard
    16 pages
    English language

SIGNIFICANCE AND USE
Include the experimental conditions under which spectra are taken in the “Experiment” section of all reports and publications.
Identify any parameters that are changed between different spectra in the “Experiment” section of publications and reports, and include the specific parameters applicable to each spectrum in the figure caption.
SCOPE
1.1 Auger and X-ray photoelectron spectra are obtained using a variety of excitation methods, analyzers, signal processing, and digitizing techniques.
1.2 This practice lists the desirable information that shall be reported to fully describe the experimental conditions, specimen conditions, data recording procedures, and data transformation processes.
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

SIGNIFICANCE AND USE
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.
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.
The procedure described herein has been successfully used to determine the dead time of counting systems on SIMS instruments. 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

SCOPE
1.1 This standard specifies the dimensions of knife-edge style flanges and their associated gaskets used in vacuum systems for pressures ranging from 105 Pa to 10-11 Pa. Such flanges are widely used throughout vacuum technology applications in semiconductor processing tools, surface analysis systems, space simulation systems, and general research requiring vacuum.
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Technical specification
    4 pages
    English language

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.
AES, XPS, and 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).  
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 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

SIGNIFICANCE AND USE
The acquisition of chemical information from variations in the energy position of peaks in the XPS spectrum is of primary interest in the use of XPS as a surface analytical tool. Surface charging acts to shift spectral peaks independent of their chemical relationship to other elements on the same surface. The desire to eliminate the influence of surface charging on the peak positions and peak shapes has resulted in the development of several empirical methods designed to assist in the interpretation of the XPS peak positions, determine surface chemistry, and allow comparison of spectra of conducting and non-conducting systems of the same element. It is assumed that the spectrometer is generally working properly for non-insulating specimens (see Practice E 902).
Although highly reliable methods have now been developed to stabilize surface potentials during XPS analysis of most materials (5, 6), no single method has been developed to deal with surface charging in all circumstances (10, 11). For insulators, an appropriate choice of any control or referencing system will depend on the nature of the specimen, the instruments, and the information needed. The appropriate use of charge control and referencing techniques will result in more consistent, reproducible data. Researchers are strongly urged to report both the control and referencing techniques that have been used, the specific peaks and binding energies used as standards (if any), and the criteria applied in determining optimum results so that the appropriate comparisons may be made.
SCOPE
1.1 This guide acquaints the X-ray photoelectron spectroscopy (XPS) user with the various charge control and charge shift referencing techniques that are and have been used in the acquisition and interpretation of XPS data from surfaces of insulating specimens and provides information needed for reporting the methods used to customers or in the literature.
1.2 This guide is intended to apply to charge control and charge referencing techniques in XPS and is not necessarily applicable to electron-excited systems.
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    7 pages
    English language
  • Guide
    7 pages
    English language

SIGNIFICANCE AND USE
Proper preparation and mounting of specimens is particularly critical for surface analysis. Improper preparation 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 in the preparation and mounting process. The goal must be to preserve the state of the surface so that the analysis remains representative of the original.
AES, XPS or ESCA, and SIMS are sensitive to surface layers that are typically a few nanometres thick. Such thin layers can be subject to severe perturbations caused by specimen handling (1) or surface treatments that may be necessary prior to introduction into the analytical chamber. In addition, specimen mounting techniques have the potential to affect the intended analysis.
This guide describes methods that the surface analyst may need to minimize the effects of specimen preparation when using any surface-sensitive analytical technique. Also described are methods to mount specimens so as to ensure that the desired information is not compromised.
Guide E 1829 describes the handling of surface sensitive specimens and, as such, complements this guide.
SCOPE
1.1 This guide covers specimen preparation and mounting prior to, during, and following 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 and ESCA), and
1.1.3 Secondary ion mass spectrometry, (SIMS).
1.1.4 Although primarily written for AES, XPS, and SIMS, these methods will 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 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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Guide
    10 pages
    English language
  • Guide
    10 pages
    English language

SIGNIFICANCE AND USE
Auger electron spectroscopy yields information concerning the chemical and physical state of a solid surface in the near surface region. Nondestructive depth profiling is limited to this near surface region. Techniques for measuring the crater depths and film thicknesses are given in (1).  
Ion sputtering is primarily used for depths of less than the order of 1 μm.
Angle lapping or mechanical cratering is primarily used for depths greater than the order of 1 μm.
The choice of depth profiling methods for investigating an interface depends on surface roughness, interface roughness, and film thickness (2).
The depth profile interface widths can be measured using a logistic function which is described in Practice E 1636.
SCOPE
1.1 This guide covers procedures used for depth profiling in Auger electron spectroscopy.
1.2 Guidelines are given for depth profiling by the following:
Section Ion Sputtering 6 Angle Lapping and Cross-Sectioning 7 Mechanical Cratering 8 Mesh Replica Method9 Nondestructive Depth Profiling 10
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 problems, 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.

  • Guide
    5 pages
    English language
  • Guide
    5 pages
    English language

SCOPE
1.1 This practice outlines the necessary steps for the identification of elements in a given Auger spectrum obtained using conventional electron spectrometers. Spectra displayed as either the electron energy distribution (direct spectrum) or the first derivative of the electron energy distribution are considered.
1.2 This practice applies to Auger spectra generated by electron or X-ray bombardment of the specimen surface and can be extended to spectra generated by other methods such as ion bombardment.
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 and health practices and determine the applicability of regulatory limitations prior to use.

  • Standard
    3 pages
    English language
  • Standard
    3 pages
    English language

Frequently Asked Questions

E42 is a Technical Committee within ASTM International. It is named "Surface Analysis" and is responsible for: * Review and coordination of the development of standards for all methods of surface analysis by photon, electron, and ion emission or reflection methods. Typical methods include: Auger electron spectroscopy (AES); X-ray photoelectron spectroscopy (XPS or ESCA); ion-scattering spectroscopy (ISS); secondary ion mass spectroscopy (SIMS); Rutherford backscattering spectroscopy (RBS); and the use of ion bombardment and other methods to obtain composition versus depth information. * Preparation of standard practices for the methods included in Article 2.1.1. * Establishment of standard definitions of terms relating to methods included in Article 2.1.1. * Cooperation with agencies concerned with preparation and distribution of standard reference materials. * Advancement of the field of surface analysis by promoting the collection of exchange of information through surveys, cooperative programs, publication of suggested methods and practices, meeting, and symposia. * The formulation and evaluation of standard surface analysis methods shall be confined to those methods not included in the scope of other ASTM Committees, except by mutual agreement. * Maintenance of a current appraisal of new and developing surface analysis techniques, as to their principles, applicability, and limitations. * These activities will be coordinated with other ASTM Committees and other organizations having mutual interests. This committee has published 121 standards.

E42 develops ASTM standards in the area of Information technology. The scope of work includes: * Review and coordination of the development of standards for all methods of surface analysis by photon, electron, and ion emission or reflection methods. Typical methods include: Auger electron spectroscopy (AES); X-ray photoelectron spectroscopy (XPS or ESCA); ion-scattering spectroscopy (ISS); secondary ion mass spectroscopy (SIMS); Rutherford backscattering spectroscopy (RBS); and the use of ion bombardment and other methods to obtain composition versus depth information. * Preparation of standard practices for the methods included in Article 2.1.1. * Establishment of standard definitions of terms relating to methods included in Article 2.1.1. * Cooperation with agencies concerned with preparation and distribution of standard reference materials. * Advancement of the field of surface analysis by promoting the collection of exchange of information through surveys, cooperative programs, publication of suggested methods and practices, meeting, and symposia. * The formulation and evaluation of standard surface analysis methods shall be confined to those methods not included in the scope of other ASTM Committees, except by mutual agreement. * Maintenance of a current appraisal of new and developing surface analysis techniques, as to their principles, applicability, and limitations. * These activities will be coordinated with other ASTM Committees and other organizations having mutual interests. Currently, there are 121 published standards from this technical committee.

ASTM is a standardization organization that develops and publishes standards to support industry, commerce, and regulatory requirements.

A Technical Committee (TC) in ASTM is a group of experts responsible for developing international standards in a specific technical area. TCs are composed of national member body delegates and work through consensus to create standards that meet global industry needs. Each TC may have subcommittees (SCs) and working groups (WGs) for specialized topics.

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