Standard Test Method for Nondestructive Assay of Plutonium, Tritium and&#x2009;<sup >241</sup>Am by Calorimetric Assay

SIGNIFICANCE AND USE
5.1 This test method is considered to be the most accurate NDA technique for the assay of many physical forms of Pu. Isotopic measurements by gamma-ray spectroscopy or destructive analysis techniques are part of this test method when it is applied to the assay of Pu.  
5.1.1 Calorimetry has been applied to a wide variety of Pu-bearing solids including metals, alloys, oxides, fluorides, mixed Pu-U oxides, mixed oxide fuel pins, waste, and scrap, for example, ash, ash heels, salts, crucibles, and graphite scarfings) (2, 3). This test method has been routinely used at U.S. and European facilities for Pu process measurements and nuclear material accountability since the mid 1960’s (2-9).  
5.1.2 Pu-bearing materials have been measured in calorimeter containers ranging in size from about 0.025 m to about 0.63 m in diameter and from about 0.076 m to about 1.38 m in height.  
5.1.3 Gamma-ray spectroscopy typically is used to determine the Pu isotopic composition and 241Am to Pu ratio (see Test Method C1030). However, isotopic information from mass spectrometry and alpha counting measurements may be used instead (see Test Method C697).  
5.2 This test method is considered to be the most accurate NDA method for the measurement of tritium. For many physical forms of tritium compounds calorimetry is currently the only practical measurement technique available.  
5.3 Physical standards representative of the materials being assayed are not required for the test method.  
5.3.1 This test method is largely independent of the elemental distribution of the nuclear materials in the matrix.  
5.3.2 The accuracy of the method can be degraded for materials with inhomogeneous isotopic composition.  
5.4 The thermal power measurement is traceable to national measurement systems through electrical standards used to directly calibrate the calorimeters or to calibrate secondary 238Pu heat standards.  
5.5 Heat-flow calorimetry has been used to prepare secondary standards for neutron...
SCOPE
1.1 This test method describes the nondestructive assay (NDA) of plutonium, tritium, and 241Am using heat flow calorimetry. For plutonium the typical range of applicability, depending on the isotopic composition, corresponds to ~0.1 g to ~5 g quantities while for tritium the typical range extends from ~0.001 g to ~400 g. This test method can be applied to materials in a wide range of container sizes up to 380 L. It has been used routinely to assay items whose thermal power ranges from 0.001 W to 135 W.  
1.2 This test method requires knowledge of the relative abundances of the plutonium isotopes and the  241Am/Pu mass ratio to determine the total plutonium mass.  
1.3 This test method provides a direct measure of tritium content.  
1.4 This test method provides a measure of  241Am either as a single isotope or mixed with plutonium.  
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.

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ASTM C1458-16 - Standard Test Method for Nondestructive Assay of Plutonium, Tritium and&#x2009;<sup >241</sup>Am by Calorimetric Assay
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Standards Content (Sample)

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: C1458 − 16
Standard Test Method for
241
Nondestructive Assay of Plutonium, Tritium and Am by
1
Calorimetric Assay
This standard is issued under the fixed designation C1458; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope C1009Guide for Establishing and Maintaining a Quality
AssuranceProgramforAnalyticalLaboratoriesWithinthe
1.1 This test method describes the nondestructive assay
241 Nuclear Industry
(NDA) of plutonium, tritium, and Am using heat flow
C1030TestMethodforDeterminationofPlutoniumIsotopic
calorimetry. For plutonium the typical range of applicability,
Composition by Gamma-Ray Spectrometry
depending on the isotopic composition, corresponds to ~0.1 g
C1592Guide for Nondestructive Assay Measurements
to ~5 g quantities while for tritium the typical range extends
C1673Terminology of C26.10 NondestructiveAssay Meth-
from ~0.001 g to ~400 g. This test method can be applied to
ods
materials in a wide range of container sizes up to 380 L. It has
3
beenusedroutinelytoassayitemswhosethermalpowerranges 2.2 ANSI Standard:
from 0.001 W to 135 W. ANSI N15.36Measurement Control Program–Nondestruc-
tive Assay Measurement Control and Assurance
1.2 This test method requires knowledge of the relative
241
abundances of the plutonium isotopes and the Am/Pu mass
3. Terminology
ratio to determine the total plutonium mass.
3.1 Definitions:
1.3 This test method provides a direct measure of tritium
3.1.1 Terms shall be defined in accordance with C26.10
content.
Terminology C1673 except for the following:
241
1.4 This test method provides a measure of Am either as
3.1.2 active mode—a mode of calorimeter operation where
a single isotope or mixed with plutonium.
anexternalpower,appliedbymeansofaseriesofbandheaters
1.5 The values stated in SI units are to be regarded as
for instance, is used to maintain the calorimeter at constant
standard. No other units of measurement are included in this
temperature.
standard.
3.1.3 baseline, n—the calorimeter output signal with no
1.6 This standard does not purport to address all of the
heat-generating item in the calorimeter item chamber.
safety concerns, if any, associated with its use. It is the
3.1.4 base power, n—a constant thermal power applied in a
responsibility of the user of this standard to establish appro-
calorimeter through an electrical resistance heater with no
priate safety and health practices and determine the applica-
heat-generating item in the item chamber.
bility of regulatory limitations prior to use.
3.1.5 equilibrium, n—the point at which the temperature of
2. Referenced Documents
the calorimeter measurement cell and the item being measured
2
stabilizes.
2.1 ASTM Standards:
C697Test Methods for Chemical, Mass Spectrometric, and
3.1.6 heat distribution error, n—the bias arising from the
Spectrochemical Analysis of Nuclear-Grade Plutonium
location of the heat source within the calorimeter chamber.
Dioxide Powders and Pellets
3.1.7 passive mode, n—a mode of calorimeter operation
wheretemperaturechange(causedbytheheattobequantified)
1
is measured by means of temperature sensors with no external
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.10 on Non
power applied except in the case of Wheatstone bridge tem-
Destructive Assay.
peraturesensorswhereelectricalcurrentisneededtoexcitethe
Current edition approved March 1, 2016. Published April 2016. Originally
ɛ1 bridge circuit.
approved in 2000. Last previous edition approved in 2009 as C1458– 09 . DOI:
10.1520/C1458-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1458 − 16
241
3.1.8 power compensation mode, n—a mode of calorimeter 4.4.3 The Am mass, m , in a plutonium-bearing item is
Am
operation where a constant applied thermal power is main- determined by multiplying the Pu mass by the Am/Pu mass
tained in a calorimeter measurement chamber through the use ratio. T
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: C1458 − 09 C1458 − 16
Standard Test Method for
241
Nondestructive Assay of Plutonium, Tritium and Am by
1
Calorimetric Assay
This standard is issued under the fixed designation C1458; 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
ε NOTE—Section 6.2 was corrected editorially in March 2009.
1. Scope
241
1.1 This test method describes the nondestructive assay (NDA) of plutonium, tritium, and Am using heat flow calorimetry.
For plutonium the typical range of applicability applicability, depending on the isotopic composition, corresponds to ~1~0.1 g to
~2000~5 g quantities while for tritium the typical range extends from ~0.001 g to ~10~400 g. This test method can be applied to
materials in a wide range of container sizes up to 50380 L. It has been used routinely to assay items whose thermal power ranges
from 0.001 W to 135 W.
241
1.2 This test method requires knowledge of the relative abundances of the plutonium isotopes and the Am/Pu mass ratio to
determine the total plutonium mass.
1.3 This test method provides a direct measure of tritium content.
241
1.4 This test method provides a measure of Am either as a single isotope or mixed with plutonium.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
C697 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powders and Pellets
C1009 Guide for Establishing and Maintaining a Quality Assurance Program for Analytical Laboratories Within the Nuclear
Industry
C1030 Test Method for Determination of Plutonium Isotopic Composition by Gamma-Ray Spectrometry
C1592 Guide for Nondestructive Assay Measurements
C1673 Terminology of C26.10 Nondestructive Assay Methods
3
2.2 ANSI Standards:Standard:
ANSI N15.22 N15.36 Plutonium—Bearing Solids–Calibration Techniques for Calorimetric AssayMeasurement Control
Program – Nondestructive Assay Measurement Control and Assurance
ANSI N15.54 Radiometric Calorimeters–Measurement Control Program
3. Terminology
3.1 Definitions:
3.1.1 Terms shall be defined in accordance with C26.10 Terminology C1673 except for the following:
1
This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.10 on Non Destructive
Assay.
Current edition approved Feb. 1, 2009March 1, 2016. Published March 2009April 2016. Originally approved in 2000. Last previous edition approved in 20002009 as
ɛ1
C1458 – 00.C1458 – 09 . DOI: 10.1520/C1458-09E01.10.1520/C1458-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1458 − 16
3.1.2 active mode—a mode of calorimeter operation where an external power, applied by means of a series of band heaters for
instance, is used to maintain the calorimeter at constant temperature.
3.1.3 baseline, n—the calorimeter output signal with no heat-generating item in the calorimeter item chamber.
3.1.4 basepower, base power, n—a constant thermal power applied in a calorimeter through an electrical resistance heater with
no heat-generating item in the item chamber.
3.1.5 equilibrium, n—the point at which the temperature of the calorimeter measurement cell and the item being measured stops
changing.stabilizes.
3.1.6 heat distribution error, n—the bias arising from the location of the heat source within the calorimeter chamber.
3.1.7 passive mode, n—a mode of calorimeter operation where temperature change (caused by
...

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