ASTM C1458-09

Standard Test Method for Nondestructive Assay of Plutonium, Tritium and ²⁴¹Am by Calorimetric Assay

SIGNIFICANCE AND USE
This test method is 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 the test method when it is applied to the assay of Pu.
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 for the last 40 years (2-9).
Pu-bearing materials have been measured in calorimeter containers ranging in size from about 0.025 m to about 0.60 m in diameter and from about 0.076 m to about 0.9 m in height.
Gamma-ray spectroscopy typically is used to determine the Pu-relative isotopic composition and 241Am to Pu ratio (see Test Method C 1030). Isotopic information from mass spectrometry and alpha counting measurements may be used (see Test Method C 697).
This test method is the most accurate NDA method for the measurement of tritium. For many physical forms of tritium compounds calorimetry is the only practical measurement technique available.
Physical standards representative of the materials being assayed are not required for the test method.
This test method is largely independent of the elemental distribution of the nuclear materials in the matrix.
The accuracy of the method can be degraded for materials with inhomogeneous isotopic composition.
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.
Heat-flow calorimetry has been used to prepare secondary standards for neutron and gamma-ray assay systems (7-12).
Calorimetry measurement times are typically longer than other NDA techni...
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 corresponds to ~1 g to ~2000 g quantities while for tritium the typical range extends from ~0.001 g to~ 10 g. This test method can be applied to materials in a wide range of container sizes up to 50 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.

General Information

• Status: Historical
• Publication Date: 31-Jan-2009
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.10 - Non Destructive Assay

Relations

• Replaces: ASTM C1458-00 - Standard Test Method for Nondestructive Assay of Plutonium, Tritium and ²⁴¹Am by Calorimetric Assay
• Effective Date: 01-Feb-2009
• Replaced By: ASTM C1458-09e1 - Standard Test Method for Nondestructive Assay of Plutonium, Tritium and ²⁴¹Am by Calorimetric Assay
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1500-08(2017) - Standard Test Method for Nondestructive Assay of Plutonium by Passive Neutron Multiplicity Counting
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1490-14(2023) - Standard Guide for the Selection, Training and Qualification of Nondestructive Assay (NDA) Personnel
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1133/C1133M-10(2018) - Standard Test Method for Nondestructive Assay of Special Nuclear Material in Low-Density Scrap and Waste by Segmented Passive Gamma-Ray Scanning
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1030-10(2018) - Standard Test Method for Determination of Plutonium Isotopic Composition by Gamma-Ray Spectrometry
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1592/C1592M-21 - Standard Guide for Making Quality Nondestructive Assay Measurements
• Effective Date: 01-Feb-2009
• Referred By: ASTM C1207-10(2018) - Standard Test Method for Nondestructive Assay of Plutonium in Scrap and Waste by Passive Neutron Coincidence Counting
• Effective Date: 01-Feb-2009

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:C1458–09
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 C1030 Test Method for Determination of Plutonium Isoto-
pic Composition by Gamma-Ray Spectrometry
1.1 This test method describes the nondestructive assay
241
C1592 Guide for Nondestructive Assay Measurements
(NDA) of plutonium, tritium, and Am using heat flow
C 1673 Terminology of C26.10 Nondestructive Assay
calorimetry. For plutonium the typical range of applicability
Methods
corresponds to ~1 g to ~2000 g quantities while for tritium the
3
2.2 ANSI Standards:
typicalrangeextendsfrom~0.001gto~10g.Thistestmethod
ANSI N15.22 Plutonium—Bearing Solids–Calibration
can be applied to materials in a wide range of container sizes
Techniques for Calorimetric Assay
up to 50 L. It has been used routinely to assay items whose
ANSI N15.54 Radiometric Calorimeters–Measurement
thermal power ranges from 0.001 W to 135 W.
Control Program
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: Terms shall be defined in accordance with
1.3 This test method provides a direct measure of tritium
C26.10 Terminology C1673 except for the following:
content.
241
3.1.1 baseline, n—the calorimeter output signal with no
1.4 This test method provides a measure of Am either as
heat-generating item in the calorimeter item chamber.
a single isotope or mixed with plutonium.
3.1.2 basepower, n—a constant thermal power applied in a
1.5 The values stated in SI units are to be regarded as
calorimeter through an electrical resistance heater with no
standard. No other units of measurement are included in this
heat-generating item in the item chamber.
standard.
3.1.3 equilibrium, n—the point at which the temperature of
1.6 This standard does not purport to address all of the
the calorimeter measurement cell and the item being measured
safety concerns, if any, associated with its use. It is the
stops changing.
responsibility of the user of this standard to establish appro-
3.1.4 heat distribution error, n—the bias arising from the
priate safety and health practices and determine the applica-
location of the heat source within the calorimeter chamber.
bility of regulatory limitations prior to use.
3.1.5 passive mode, n—a mode of calorimeter operation
2. Referenced Documents wherenoexternalpowerisappliedtothecalorimeterexceptin
2
the case of Wheatstone bridge temperature sensors where
2.1 ASTM Standards:
electrical current is needed to excite the bridge circuit.
C697 TestMethodsforChemical,MassSpectrometric,and
3.1.6 sensitivity, n—the change in calorimeter response per
Spectrochemical Analysis of Nuclear-Grade Plutonium
Watt of thermal power (usually in units of micro Volts per
Dioxide Powders and Pellets
Watt) for a heat flow calorimeter.
C1009 Guide for Establishing a Quality Assurance Pro-
3.1.7 servo control mode, n—a mode of calorimeter opera-
gram for Analytical Chemistry Laboratories Within the
tionwhereaconstantappliedthermalpowerismaintainedina
Nuclear Industry
calorimeter measurement chamber through the use of an
electric resistance heater in a closed loop control system.
1
ThistestmethodisunderthejurisdictionofASTMCommitteeC26onNuclear
3.1.8 specific power, n—the rate of energy emission by
Fuel Cycle and is the direct responsibility of Subcommittee C26.10 on Non
ionizing radiation per unit mass of a radionuclide, such
Destructive Assay.
241
as Am or tritium.
Current edition approved Feb. 1, 2009. Published March 2009. Originally
approved in 2000. Last previous edition approved in 2000 as C1458–00.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. 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

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C1458–09
241 241
3.1.9 thermal diffusivity, n—the ratio of thermal conductiv- 4.3.3 For Am mixed with plutonium, the Am mass,
ity to the heat capacity. It measures the ability of a material to M , is determined by
Am
conduct thermal
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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.
Designation:C1458–00 Designation:C1458–09
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
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 corresponds to<1~1gto> 2000 ~2000 g quantities while for tritium the typical
range extends from ~0.001 g to > 10~10 g. This test method can be applied to materials in a wide range of container sizes up to
50 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
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 Spectrometry, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide
Powder and Pellets
2
C859Terminology Relating to Nuclear Materials Test Methods for Chemical, Mass Spectrometric, and Spectrochemical
Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
C1009 GuideforEstablishingaQualityAssuranceProgramforAnalyticalChemistryLaboratoriesWithintheNuclearIndustry
2
C1030 Test Method for Determination of Plutonium Isotopic Composition by Gamma-Ray Spectrometry 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:
ANSI N15.22 Plutonium—Bearing Solids–Calibration Techniques for Calorimetric Assay
ANSI N15.54 Radiometric Calorimeters–Measurement Control Program
3. Terminology
3.1 Definitions—Terms shall be defined in accordance with Terminology C859 Definitions: Terms shall be defined in
accordance with C26.10 Terminology C1673 except for the following:
3.1.1 baseline, n—the calorimeter output signal with no heat-generating item in the calorimeter sampleitem chamber.
3.1.2 basepower, n—a constant thermal power applied in a calorimeter through an electrical resistance heater with no
1
This test method is under the jurisdiction ofASTM Committee C-26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.10 on Nondestructive
Analysis.
Current edition approved Jan. 10, 2000. Published March 2000.
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.10 on Non Destructive
Assay.
Current edition approved Feb. 1, 2009. Published March 2009. Originally approved in 2000. Last previous edition approved in 2000 as C1458–00.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail]ards
, Vol 12.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Available from American National Standards Institute, 11 W. 42nd St., 13th Floor, New York, NY 10036.
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

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C1458–09
heat-generating item in the sampleitem chamber.
3.1.3 calorimeter—a device to measure heat or rate-of-heat generation. equilibrium, n—the point at which the temperature of
the calorimeter measurement cell and the item being measured stops changing.
3.1.4 calorime
...