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

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 after the detection of a pulse after which no other pulses can be counted. This characteristic time 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.5 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, or both.
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.

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Publication Date
31-Oct-2005
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Drafting Committee
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E2426–05
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 3.1.2 See Terminology ISO 21270 for definitions of terms
related to counting system measurements.
1.1 This practice provides the Secondary Ion Mass Spec-
m2 m1
3.1.3 isotopic ratio, n—written as X/ X, for an element
trometry (SIMS) analyst with a method for determining the
X with isotopes m1 and m2, refers to the ratios of their atomic
dead time of the pulse-counting detection systems on the
abundances. When it is a value measured in a mass spectrom-
instrument. This practice also allows the analyst to determine
eter it refers to the ratio of the signal intensities for the two
whether the apparent dead time is independent of count rate.
species.
1.2 This practice is applicable to most types of mass
m2 m2
3.1.3.1 Discussion—The notation D X or d X refers to
spectrometers that have pulse-counting detectors.
the fractional deviation of the measured isotopic ratio from the
1.3 This practice does not describe methods for precise or
m2
standard ratio or reference. In this guide, D X will refer to the
accurate isotopic ratio measurements, or both.
fractional deviation of the measured ratio, uncorrected for
1.4 This practice does not describe methods for the proper
m2
mass-fractionation (see 3.1.4) and d X will refer to the
operation of pulse counting systems and detectors for mass
fractional deviation of the measured ratio that has been
spectrometry.
corrected for mass-fractionation. An example for Mg is:
1.5 This standard does not purport to address all of the
25 24
safety concerns, if any, associated with its use. It is the
~ Mg/ Mg!
Meas
D Mg 5 – 1 (1)
25 24
responsibility of the user of this standard to establish appro-
~ Mg/ Mg!
Ref
priate safety and health practices and determine the applica-
where:
bility of regulatory limitations prior to use.
25 24 4
( Mg/ Mg) = 0.12663 .
Ref
2. Referenced Documents
3.1.4 mass-fractionation, n—sometimes called “ mass-
bias,”referstothetotalmass-dependent,intra-isotopevariation
2.1 ASTM Standards:
E673 Terminology Relating to Surface Analysis in ion intensity observed in the measured isotopic ratios for a
given element compared with the reference ratios. It can be
2.2 ISO Standard:
ISO 21270 Surface chemical analysis — X-ray photoelec- expressed as the fractional deviation per unit mass.
3.1.4.1 Discussion—The mass of an isotope i of element X
tron and Auger electron spectrometers — Linearity of
mi
intensity scale; and references 1, 2, 10, 13 and 14 therein. ( X) shall be represented by the notation m, where “i”isan
i
integer.
3. Terminology
4. Summary of Practice
3.1 Definitions:
4.1 This practice describes a method whereby the overall
3.1.1 SeeTerminology E673 for definitions of terms used in
effective dead time of a pulse counting system can be deter-
SIMS.
mined by measuring isotopic ratios of an element having at
least 3 isotopes. One of the isotopes should be approximately
This practice is under the jurisdiction of ASTM Committee E42 on Surface
afactorof10moreabundantthantheotherssothatafirstorder
Analysis and is the direct responsibility of Subcommittee E42.06 on SIMS.
estimate of the dead time can be calculated that will be close to
Current edition approved Nov. 1, 2005. Published January 2006. DOI: 10.1520/
the true value. The efficacy of the method is increased if the
E2426-05.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or sample is flat and uniform, such as a Si wafer or a polished
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Catanzaro E. J., Murphy T. J., Garner E. L., and Shields W. R., “Absolute
Available from International Organization for Standardization (ISO), 1 rue de Isotopic Abundance Ratios and Atomic Weight of Magnesium,” J. Res. Nat. Bur.
Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland. Stand., 70a, 1966, pp. 453-458.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E2426–05
metal block so that the count rate of the isotopes varies
minimally during the individual measurements.
5. 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 after the detection of a pulse after which no
other pulses can be counted. This characteristic time is known
asthe“deadtime.”Thedeadtimehastheeffectofreducingthe
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 FIG. 1 Representation of the Effects of Dead Time and Mass
Fractionation on Measured Isotopic Ratios Expressed as
used to determine the dead time of counting systems on SIMS
Fractional Deviations
instruments. The accurate determination of the dead time by
this method has b
...

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