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ASTM E2426-10(2019)

(Practice)

Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS

Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS

SIGNIFICANCE AND USE
5.1 Electron multipliers are commonly used in pulse-counting mode to detect ions from magnetic sector mass spectrometers. The electronics used to amplify, detect and count pulses from the electron multipliers always have a characteristic time interval after the detection of a pulse, during which no other pulses can be counted. This characteristic time interval is known as the “dead time.” The dead time has the effect of reducing the measured count rate compared with the “true” count rate.  
5.2 In order to measure count rates accurately over the entire dynamic range of a pulse counting detector, such as an electron multiplier, the dead time of the entire pulse counting system must be well known. Accurate count rate measurement forms the basis of isotopic ratio measurements as well as elemental abundance determinations.  
5.3 The procedure described herein has been successfully used to determine the dead time of counting systems on SIMS instruments.6 The accurate determination of the dead time by this method has been a key component of precision isotopic ratio measurements made by SIMS.
SCOPE
1.1 This practice provides the Secondary Ion Mass Spectrometry (SIMS) analyst with a method for determining the dead time of the pulse-counting detection systems on the instrument. This practice also allows the analyst to determine whether the apparent dead time is independent of count rate.  
1.2 This practice is applicable to most types of mass spectrometers that have pulse-counting detectors.  
1.3 This practice does not describe methods for precise or accurate isotopic ratio measurements.  
1.4 This practice does not describe methods for the proper operation of pulse counting systems and detectors for mass spectrometry.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-Dec-2018
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E42 - Surface Analysis
Drafting Committee
E42.06 - SIMS
Current Stage
Ref Project

Relations

Replaces
ASTM E2426-10 - Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS
Effective Date
01-Jan-2019
Refers
ASTM E673-03 - Standard Terminology Relating to Surface Analysis (Withdrawn 2012)
Effective Date
01-Dec-2003
Refers
ASTM E673-02a - Standard Terminology Relating to Surface Analysis
Effective Date
10-Dec-2002
Refers
ASTM E673-01 - Standard Terminology Relating to Surface Analysis
Effective Date
10-Nov-2001
Refers
ASTM E673-98E1 - Standard Terminology Relating to Surface Analysis
Effective Date
10-Nov-2001

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ASTM E2426-10(2019) - Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMSASTM E2426-10(2019) - Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS
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ASTM E2426-10(2019) - Standard Practice for Pulse Counting System Dead Time Determination by Measuring Isotopic Ratios with SIMS
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E2426 − 10 (Reapproved 2019)
Standard Practice for
Pulse Counting System Dead Time Determination by
Measuring Isotopic Ratios with SIMS
This standard is issued under the fixed designation E2426; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 ISO Standard:
ISO 21270 Surface chemical analysis -- X-ray photoelectron
1.1 This practice provides the Secondary Ion Mass Spec-
and Auger electron spectrometers -- Linearity of intensity
trometry (SIMS) analyst with a method for determining the
scale; and references 1, 2, 10, 13 and 14 therein.
dead time of the pulse-counting detection systems on the
instrument. This practice also allows the analyst to determine
3. Terminology
whether the apparent dead time is independent of count rate.
3.1 Definitions:
1.2 This practice is applicable to most types of mass 3.1.1 See Terminology E673 for definitions of terms used in
spectrometers that have pulse-counting detectors. SIMS.
3.1.2 See Terminology ISO 21270 for definitions of terms
1.3 This practice does not describe methods for precise or
related to counting system measurements.
accurate isotopic ratio measurements.
m2 m1
3.1.3 isotopic ratio, n—written as X/ X, for an element
1.4 This practice does not describe methods for the proper
X with isotopes m1 and m2, refers to the ratios of their atomic
operation of pulse counting systems and detectors for mass
abundances. When it is a value measured in a mass spectrom-
spectrometry.
eter it refers to the ratio of the signal intensities for the two
species.
1.5 This standard does not purport to address all of the
m2 m2
3.1.3.1 Discussion—Thenotation∆ Xorδ Xreferstothe
safety concerns, if any, associated with its use. It is the
fractional deviation of the measured isotopic ratio from the
responsibility of the user of this standard to establish appro-
m2
standard ratio or reference. In this practice, ∆ X will refer to
priate safety, health, and environmental practices and deter-
the fractional deviation of the measured ratio, uncorrected for
mine the applicability of regulatory limitations prior to use.
m2
mass-fractionation (see 3.1.4) and δ X will refer to the
1.6 This international standard was developed in accor-
fractional deviation of the measured ratio that has been
dance with internationally recognized principles on standard-
corrected for mass-fractionation. An example for magnesium
ization established in the Decision on Principles for the
(Mg) is:
Development of International Standards, Guides and Recom-
25 24
mendations issued by the World Trade Organization Technical Mg/ Mg
~ !
Meas
∆ Mg 5 21 (1)
25 24
Barriers to Trade (TBT) Committee.
~ Mg/ Mg!
Ref
where:
2. Referenced Documents
25 24 5
( Mg/ Mg) = 0.12663.
Ref
2.1 ASTM Standard:
3.1.4 mass-fractionation, n—sometimes called “mass-bias,”
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
referstothetotalmass-dependent,intra-isotopevariationinion
2012)
intensity observed in the measured isotopic ratios for a given
elementcomparedwiththereferenceratios.Itcanbeexpressed
as the fractional deviation per unit mass.
3.1.4.1 Discussion—The mass of an isotope i of element X
This practice is under the jurisdiction of ASTM Committee E42 on Surface
mi
Analysis and is the direct responsibility of Subcommittee E42.06 on SIMS.
( X) shall be represented by the notation m, where “i”isan
i
Current edition approved Jan. 1, 2019. Published January 2019. Originally
integer.
approved in 2005. Last previous edition approved in 2010 as E2426–10. DOI:
10.1520/E2426–10R19.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from International Organization for Standardization (ISO), ISO
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
Standards volume information, refer to the standard’s Document Summary page on Geneva, Switzerland, http://www.iso.org.
the ASTM website. Catanzaro, E. J., Murphy, T. J., Garner, E. L., and Shields, W. R., “Absolute
The last approved version of this historical standard is referenced on IsotopicAbundanceRatiosandAtomicWeightofMagnesium,” Journal of Research
www.astm.org. of the National Bureau of Standards, Vol 70a, 1966, pp. 453–458.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2426 − 10 (2019)
4. Summary of Practice retriggerable (non-paralyzable, or non-extendable), or a com-
bination of the two. In a retriggerable system the length of the
4.1 This practice describes a method whereby the overall
discriminator output pulse is increased if a pulse arrives at the
effective dead time of a pulse counting system can be deter-
discriminator input before the output has returned to its
mined by measuring isotopic ratios of an element having at
quiescentstate.Somesystemshaveanadditionalrecoverytime
least 3 isotopes. One of the isotopes should be approximately
after the output has returned to its quiescent state during which
afactorof10moreabundantthantheotherssothatafirstorder
they will not react to input pulses. This time just adds to the
estimate of the dead time can be calculated that will be close to
system dead time. In such a system the dead time is given by:
the true value. The efficacy of the method is increased if the
2τC
True
sample is flat and uniform, such as a silver (Si) wafer or a C 5 C e (2)
Meas True
polished metal block so that the count rate of the isotopes
where:
varies minimally during the individual measurements.
C = the measured count rate,
Meas
C = the true count rate, and
True
5. Significance and Use
τ = the dead time.
5.1 Electron multipliers are commonly used in pulse-
7.1.1.1 In a non-retriggerable system a pulse is simply
counting mode to detect ions from magnetic sector mass
ignored if it arrives before the discriminator output has
spe
...

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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...
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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.  
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