ASTM C1168-15
(Practice)Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
Standard Practice for Preparation and Dissolution of Plutonium Materials for Analysis
SIGNIFICANCE AND USE
5.1 Plutonium and uranium mixtures are used as nuclear reactor fuels. For use as a nuclear reactor fuel, the material must meet certain criteria for combined uranium and plutonium content, effective fissile content, and impurity content as described in Specifications C757 and C833. After dissolution using one of the procedures described in this practice, the material is assayed for plutonium and uranium to determine if the content is correct as specified by the purchaser.
5.2 Unique plutonium materials, such as alloys, compounds, and scrap metals, are typically dissolved with various acid mixtures or by fusion with various fluxes. Many plutonium salts are soluble in hydrochloric acid. One or more of the procedures included in this practice may be effective for some of these materials; however their applicability to a particular plutonium material shall be verified by the user.
SCOPE
1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for other components are listed. Aliquots of the dissolved samples are dispensed on a weight basis when one of the analyses must be highly reliable, such as plutonium assay; otherwise they are dispensed on a volume basis.
1.2 Procedures in this practice are intended for the dissolution of plutonium metal, plutonium oxide, and uranium-plutonium mixed oxides. Aliquots of dissolved samples are analyzed using test methods, such as those developed by Subcommittee C26.05 on Methods of Test, to demonstrate compliance with applicable requirements. These may include product specifications such as Specifications C757 and C833.
1.3 One or more of the procedures in this practice may be applicable to unique plutonium materials, such as alloys, compounds, and scrap materials. The user must determine the applicability of this practice to such materials.
1.4 The treatments, in order of presentation, are as follows:
Procedure Number
Procedure Title
Section
1
Dissolution of Plutonium Metal with Hydrochloric Acid at Room Temperature
9
2
Dissolution of Plutonium Metal with Hydrochloric Acid and Heating
10
3
Dissolution of Plutonium Metal with Sulfuric Acid
11
4
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed
Oxide by the Sealed-Reflux Technique
12
5
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed Oxides by Sodium Bisulfate Fusion
13
6
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired Plutonium Oxide in Beakers
14
7
Open-Vessel (with Reflux Condenser) Dissolution of Plutonium Oxide Powder
15
8
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Powder
16
9
Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder
17
10
Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide Pellets
18
1.5 The values stated in SI units are to be regarded as standard. Values in parentheses (non-SI units), where provided, are for information only and are not considered 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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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: C1168 − 15
Standard Practice for
Preparation and Dissolution of Plutonium Materials for
1
Analysis
This standard is issued under the fixed designation C1168; 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 the analyses must be highly reliable, such as plutonium assay;
otherwise they are dispensed on a volume basis.
1.1 This practice is a compilation of dissolution techniques
1.2 Procedures in this practice are intended for the dissolu-
for plutonium materials that are applicable to the test methods
tion of plutonium metal, plutonium oxide, and uranium-
used for characterizing these materials. Dissolution treatments
plutonium mixed oxides. Aliquots of dissolved samples are
for the major plutonium materials assayed for plutonium or
analyzed using test methods, such as those developed by
analyzed for other components are listed. Aliquots of the
Subcommittee C26.05 on Methods of Test, to demonstrate
dissolved samples are dispensed on a weight basis when one of
compliance with applicable requirements. These may include
product specifications such as Specifications C757 and C833.
1.3 One or more of the procedures in this practice may be
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
applicable to unique plutonium materials, such as alloys,
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
compounds, and scrap materials. The user must determine the
Current edition approved Sept. 1, 2015. Published October 2015. Originally
applicability of this practice to such materials.
approved in 1990. Last previous edition approved in 2008 as C1168 – 08. DOI:
10.1520/C1168-15. 1.4 The treatments, in order of presentation, are as follows:
Procedure Number Procedure Title Section
1 Dissolution of Plutonium Metal with Hydrochloric Acid at Room 9
Temperature
2 Dissolution of Plutonium Metal with Hydrochloric Acid and Heating 10
3 Dissolution of Plutonium Metal with Sulfuric Acid 11
4 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 12
Oxide by the Sealed-Reflux Technique
5 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 13
Oxides by Sodium Bisulfate Fusion
6 Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 14
Plutonium Oxide in Beakers
7 Open-Vessel (with Reflux Condenser) Dissolution of Plutonium 15
Oxide Powder
8 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 16
Powder
9 Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder 17
10 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 18
Pellets
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1168 − 15
1.5 The values stated in SI units are to be regarded as 4.2 The dissolved materials are quantitatively transferred to
standard.Valuesinparentheses(non-SIunits),whereprovided, ataredpolyethylenedispensingbottleforsubsequentdeliveries
are for information only and are not considered standard. of weighed aliquots for high-precision analysis methods, such
as assays, or to a volumetric flask for deliveries of volume
1.6 This standard does not purport to address all of the
aliquots for less precise analysis methods, such as impurity
safety concerns, if any, associated with its use. It is the
analyses. Dilute acids are used as rinses to effect quantitative
responsibility of the user of this standard to establish appro-
transfers and as diluents in the polyethylene dispensing bottles
priate safety and health practices and determine the applica-
and volumetric flasks.The use of water for these purposes can,
bility of regulatory limitations prior to use.
in some cases, result in hydrolysis of plutonium to produce
polymers that, although soluble, are nonreactive in separation
2. Referenced Documents
treatments or in plutonium assay methods that have no
2
2.1 ASTM Standards:
pretreatments, such as fuming with acid.
C757 Specification for Nuclear-Grade Plutonium Dioxide
4.3 The procedures included in this practice are briefly
Powder, Sinterable
described in
4.4 through 4.8. Other dissolution reagents are
C833 Specification for Sintered (Uranium-Plutonium) Diox-
possible, but are not addressed in this practice. When alternate
ide Pellets
reagents are employed, the user shall verify their suitability for
C859 Terminology Relating to Nuclear Materials
the intended use.
C1
...
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.
Designation: C1168 − 08 C1168 − 15
Standard Practice for
Preparation and Dissolution of Plutonium Materials for
1
Analysis
This standard is issued under the fixed designation C1168; 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
1.1 This practice is a compilation of dissolution techniques for plutonium materials that are applicable to the test methods used
for characterizing these materials. Dissolution treatments for the major plutonium materials assayed for plutonium or analyzed for
other components are listed. AliquantsAliquots of the dissolved samples are dispensed on a weight basis when one of the analyses
must be highly reliable, such as plutonium assay; otherwise they are dispensed on a volume basis.
1.2 Procedures in this practice are intended for the dissolution of plutonium metal, plutonium oxide, and uranium-plutonium
mixed oxides. Aliquots of dissolved samples are analyzed using test methods, such as those developed by Subcommittee C26.05
on Methods of Test, to demonstrate compliance with applicable requirements. These may include product specifications such as
Specifications C757 and C833.
1.3 One or more of the procedures in this practice may be applicable to unique plutonium materials, such as alloys, compounds,
and scrap materials. The user must determine the applicability of this practice to such materials.
1.4 The treatments, in order of presentation, are as follows:
Procedure Number Procedure Title Section
1 Dissolution of Plutonium Metal with Hydrochloric Acid at Room 9
Temperature
2 Dissolution of Plutonium Metal with Hydrochloric Acid and Heating 10
3 Dissolution of Plutonium Metal with Sulfuric Acid 11
4 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 12
Oxide by the Sealed-Reflux Technique
5 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 13
Oxides by Sodium Bisulfate Fusion
6 Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 14
Plutonium Oxide in Beakers
7 Open-Vessel (with Reflux Condenser) Dissolution of Plutonium 15
Oxide Powder
8 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 16
Powder
9 Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder 17
10 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 18
Pellets
Procedure Title Section
Dissolution of Plutonium Metal with Hydrochloric Acid 9.1
Dissolution of Plutonium Metal with Sulfuric Acid 9.2
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.3
Oxide by the Sealed-Reflux Technique
Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 9.4
Oxides by Sodium Bisulfate Fusion
Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 9.5
Plutonium Oxide in Beakers
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Jan. 1, 2008Sept. 1, 2015. Published February 2008October 2015. Originally approved in 1990. Last previous edition approved in 20012008 as
C1168 – 01.C1168 – 08. DOI: 10.1520/C1168-08.10.1520/C1168-15.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1168 − 15
1.5 The values stated in SI units are to be regarded as standard. Values in parentheses (non-SI units), where provided, are for
information only and are not considered 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:
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder, Sinterable
C833 Specification for Sintered (Uranium-Plutonium) Dioxide Pellets
C859 Terminology Relating to Nuclear Materials
C1145 Terminology of Advanced Ceramics
C1210 Guide for Establishing a Measurement System Quality Control Program for Analytical Chemistry Laboratories Within
the Nuclear Industry
C1008D1193 Specification for Sintered (Uranium-Plutonium) DioxidePellets—Fast Reactor FuelReagent Water (Withdrawn
2014)
D7439 Test Method for Determination of Elements in Airborne Par
...
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: C1168 − 15
Standard Practice for
Preparation and Dissolution of Plutonium Materials for
1
Analysis
This standard is issued under the fixed designation C1168; 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 the analyses must be highly reliable, such as plutonium assay;
otherwise they are dispensed on a volume basis.
1.1 This practice is a compilation of dissolution techniques
1.2 Procedures in this practice are intended for the dissolu-
for plutonium materials that are applicable to the test methods
tion of plutonium metal, plutonium oxide, and uranium-
used for characterizing these materials. Dissolution treatments
plutonium mixed oxides. Aliquots of dissolved samples are
for the major plutonium materials assayed for plutonium or
analyzed using test methods, such as those developed by
analyzed for other components are listed. Aliquots of the
Subcommittee C26.05 on Methods of Test, to demonstrate
dissolved samples are dispensed on a weight basis when one of
compliance with applicable requirements. These may include
product specifications such as Specifications C757 and C833.
1.3 One or more of the procedures in this practice may be
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
applicable to unique plutonium materials, such as alloys,
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
compounds, and scrap materials. The user must determine the
Current edition approved Sept. 1, 2015. Published October 2015. Originally
applicability of this practice to such materials.
approved in 1990. Last previous edition approved in 2008 as C1168 – 08. DOI:
10.1520/C1168-15. 1.4 The treatments, in order of presentation, are as follows:
Procedure Number Procedure Title Section
1 Dissolution of Plutonium Metal with Hydrochloric Acid at Room 9
Temperature
2 Dissolution of Plutonium Metal with Hydrochloric Acid and Heating 10
3 Dissolution of Plutonium Metal with Sulfuric Acid 11
4 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 12
Oxide by the Sealed-Reflux Technique
5 Dissolution of Plutonium Oxide and Uranium-Plutonium Mixed 13
Oxides by Sodium Bisulfate Fusion
6 Dissolution of Uranium-Plutonium Mixed Oxides and Low-Fired 14
Plutonium Oxide in Beakers
7 Open-Vessel (with Reflux Condenser) Dissolution of Plutonium 15
Oxide Powder
8 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 16
Powder
9 Closed-Vessel Hot Block Dissolution of Plutonium Oxide Powder 17
10 Open-Vessel (with Reflux Condenser) Dissolution of Mixed Oxide 18
Pellets
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
C1168 − 15
1.5 The values stated in SI units are to be regarded as 4.2 The dissolved materials are quantitatively transferred to
standard. Values in parentheses (non-SI units), where provided, a tared polyethylene dispensing bottle for subsequent deliveries
are for information only and are not considered standard. of weighed aliquots for high-precision analysis methods, such
as assays, or to a volumetric flask for deliveries of volume
1.6 This standard does not purport to address all of the
aliquots for less precise analysis methods, such as impurity
safety concerns, if any, associated with its use. It is the
analyses. Dilute acids are used as rinses to effect quantitative
responsibility of the user of this standard to establish appro-
transfers and as diluents in the polyethylene dispensing bottles
priate safety and health practices and determine the applica-
and volumetric flasks. The use of water for these purposes can,
bility of regulatory limitations prior to use.
in some cases, result in hydrolysis of plutonium to produce
polymers that, although soluble, are nonreactive in separation
2. Referenced Documents
treatments or in plutonium assay methods that have no
2
2.1 ASTM Standards:
pretreatments, such as fuming with acid.
C757 Specification for Nuclear-Grade Plutonium Dioxide
4.3 The procedures included in this practice are briefly
Powder, Sinterable
described in 4.4 through 4.8. Other dissolution reagents are
C833 Specification for Sintered (Uranium-Plutonium) Diox-
possible, but are not addressed in this practice. When alternate
ide Pellets
reagents are employed, the user shall verify their suitability for
C859 Terminology Relating to Nuclear Materials
the intended use.
C1145 Terminology of Advanced Ceramics
C1210 Guide for Establishing a Measurement System Qual-
4.4 Plutonium metal is dissolved with
...
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