ASTM D6239-03e2

Standard Test Method for Uranium in Drinking Water by High-Resolution Alpha-Liquid-Scintillation Spectrometry

SIGNIFICANCE AND USE
This test method is a fast, cost-effective method that can yield limited isotopic activity levels for  238U and  234U, as well as total uranium activity. Although  232U is incorporated as a tracer, uranium recoveries for this test measured during the developmental work on this test method were usually between 95 and 105%.
The high-resolution alpha-liquid-scintillation spectrometer offers a constant 99.6 ± 0.1 % counting efficiency and instrument backgrounds as low as 0.001 counts per minute (cpm) over a 4 to 7 MeV energy range according to McDowell and McDowell (2). Count rates for extractive scintillator blanks and reagent blanks usually range from 0.01 cpm to 0.1 cpm.
SCOPE
1.1 This test method covers determining the total soluble uranium activity in drinking water in the range of 0.037 Bq/L (1 pCi/L) or greater by selective solvent extraction and high-resolution alpha-liquid-scintillation spectrometry. The energy resolution obtainable with this technique also allows estimation of the  238U to  234U activity ratio.
1.2 This test method was tested successfully with reagent water and drinking water. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.4 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.  For specific hazard statements, see Section 9.

General Information

• Status: Historical
• Publication Date: 09-Jun-2003
• ICS: 13.060.60 - Examination of physical properties of water
• Technical Committee: D19 - Water
• Drafting Committee: D19.04 - Methods of Radiochemical Analysis

Relations

• Replaces: ASTM D6239-03e1 - Standard Test Method for Uranium in Drinking Water by High-Resolution Alpha-Liquid-Scintillation Spectrometry
• Effective Date: 10-Jun-2003
• Replaced By: ASTM D6239-09 - Standard Test Method for Uranium in Drinking Water by High-Resolution Alpha-Liquid-Scintillation Spectrometry
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
´2
Designation:D6239–03
Standard Test Method for
Uranium in Drinking Water by High-Resolution Alpha-Liquid-
1
Scintillation Spectrometry
This standard is issued under the fixed designation D6239; 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
´ NOTE—Added research report reference to Section 14 editorially in March 2008.
2
´ NOTE—Added research report reference to Section 14 editorially in September 2008.
1. Scope 3.1.1 Fordefinitionsoftermsusedinthistestmethod,refer
to Terminology D1129. For terms not included in this refer-
1.1 This test method covers determining the total soluble
3
ence, refer to other published glossaries (1)
uranium activity in drinking water in the range of 0.037 Bq/L
(1 pCi/L) or greater by selective solvent extraction and
4. Summary of Test Method
high-resolutionalpha-liquid-scintillationspectrometry.Theen-
4.1 This test method is based on solvent extraction technol-
ergy resolution obtainable with this technique also allows
238 234 ogy to isolate and concentrate uranium in drinking water for
estimation of the Uto U activity ratio.
counting via a high-resolution alpha-liquid-scintillation spec-
1.2 This test method was tested successfully with reagent
trometer.
water and drinking water. It is the user’s responsibility to
4.2 To determine total uranium, as well as limited isotopic
ensure the validity of this test method for waters of untested
238 234
uranium ( U and U) by activity in drinking water, a
matrices.
232
200–mL acidified water sample is first spiked with Uasan
1.3 The values stated in SI units are to be regarded as
isotopic tracer, boiled briefly to remove radon, and evaporated
standard. The values given in parentheses are for information
until less than 50 mL remain. The solution is then made
only.
approximately 0.01 M in diethylenetriaminepentaacetic acid
1.4 This standard does not purport to address all of the
(DTPA) and the pH is adjusted to between 2.5 and 3.0. The
safety concerns, if any, associated with its use. It is the
sample is transferred to a separatory funnel and equilibrated
responsibility of the user of this standard to establish appro-
with 1.50 mL of an extractive scintillator containing a dialkyl
priate safety and health practices and determine the applica-
phosphoric acid extracting agent. Under these conditions only
bility of regulatory limitations prior to use. For specific hazard
uraniumisquantitativelytransferredtotheorganicphasewhile
statements, see Section 9.
the extraction of undesired ions is masked by the presence of
2. Referenced Documents DTPA. Following phase separation, 1.00 mL of the organic
2
phase is sparged with dry argon gas to remove oxygen, a
2.1 ASTM Standards:
chemical quench agent, and counted on a high-resolution
D1129 Terminology Relating to Water
alpha-liquid-scintillation spectrometer and multichannel ana-
D1193 Specifications for Reagent Water
lyzer (MCA).
D2777 Practice for Determination of Precision and Bias of
4.3 The alpha spectrum of a sample that contains natural
Applicable Methods of Committee D19 on Water
232
uranium and that is analyzed with an internal U tracer will
D3370 PracticesforSamplingWaterfromClosedConduits
appear similar to the spectrum in Fig. 1. An approximate
D3648 Practices for the Measurement of Radioactivity
238
resolution of 250 keV FWHM for U (4.2 MeV) allows
238 234 232
3. Terminology
resolution and analysis of the U, U, and U energy
spectrum peaks when their activities are of the same order of
3.1 Definitions:
235
magnitude.Resolutionofthe U(4.4MeV)alphapeakisnot
possible, but its activity, which accounts for approximately
1
This test method is under the jurisdiction ofASTM Committee D19 on Water
2.2% of the total natural uranium activity, is included in the
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi-
238 234
totaluraniumactivitycalculatedwhenthe Uand Upeaks
cal Analysis.
238 234
are in the region of interest (ROI). When the U and U
Current edition approved June 10, 2003. Published August 2003. Originally
approved in 1998. Last previous edition approved in 2002 as D 6239–02.
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 The boldface numbers in parenthesis refer to the list of references at the end of
the ASTM website. the text.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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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.
´2
Designation:D6239–02 Designation:D6239–03
Standard Test Method for
Uranium in Drinking Water by High-Resolution Alpha-Liquid-
1
Scintillation Spectrometry
This standard is issued under the fixed designation D6239; 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
´ NOTE—Added research report reference to Section 14 editorially in March 2008.
2
´ NOTE—Added research report reference to Section 14 editorially in September 2008.
1. Scope
1.1 Thistestmethodcoversdeterminingthetotalsolubleuraniumactivityindrinkingwaterintherangeof0.037Bq/L(1pCi/L)
or greater by selective solvent extraction and high-resolution alpha-liquid-scintillation spectrometry. The energy resolution
238 234
obtainable with this technique also allows estimation of the Uto U activity ratio.
1.2 This test method was tested successfully with reagent water and drinking water. It is the user’s responsibility to ensure the
validity of this test method for waters of untested matrices.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.4 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. For specific hazard statements, see Section 9.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specifications for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D3648 Practices for the Measurement of Radioactivity
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D1129. For terms not included in this reference,
3
refer to other published glossaries (1)
4. Summary of Test Method
4.1 Thistestmethodisbasedonsolventextractiontechnologytoisolateandconcentrateuraniumindrinkingwaterforcounting
via a high-resolution alpha-liquid-scintillation spectrometer.
238 234
4.2 To determine total uranium, as well as limited isotopic uranium ( U and U) by activity in drinking water, a 200–mL
232
acidifiedwatersampleisfirstspikedwith Uasanisotopictracer,boiledbrieflytoremoveradon,andevaporateduntillessthan
50 mL remain. The solution is then made approximately 0.01 M in diethylenetriaminepentaacetic acid (DTPA) and the pH is
adjusted to between 2.5 and 3.0. The sample is transferred to a separatory funnel and equilibrated with 1.50 mL of an extractive
scintillatorcontainingadialkylphosphoricacidextractingagent.Undertheseconditionsonlyuraniumisquantitativelytransferred
to the organic phase while the extraction of undesired ions is masked by the presence of DTPA. Following phase separation, 1.00
mL of the organic phase is sparged with dry argon gas to remove oxygen, a chemical quench agent, and counted on a
high-resolution alpha-liquid-scintillation spectrometer and multichannel analyzer (MCA).
1
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemical
Analysis.
Current edition approved August 10, 2002. Published September 2002. Originally published as D 6239–98. Last previous edition D 6239–98a.
Current edition approved June 10, 2003. Published August 2003. Originally approved in 1998. Last previous edition approved in 2002 as D 6239–02.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,[e-mail] Annual Book of ASTM Standards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Annual Book of ASTM Standards, Vol 11.02.
3
The boldface numbers in parenthesis refer to the list of references at the end of the text.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

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D6239–03
232
4.3 The alpha spectrum of a sample that contains natural uranium and that is analyzed with an internal U tracer will appear
238
similartothespectruminFig.1.Anapproximateresolutionof250keVFWHMfor U(
...