Standard Test Method for Uranium Analysis in Natural and Waste Water by X-Ray Fluorescence

SIGNIFICANCE AND USE
Uranium production facilities must control trace uranium content in their waste waters.
Colorimetric and fluorimetric methods have been developed but require a tedious separation of interfering elements. Trace uranium can also be determined by ICP-MS but not all water matrices are adapted (for example, waters with high salt content). Direct X-ray fluorescence can be done on the liquid but with a detection limit of ∼5 mg/L
X-ray fluorescence after collection of uranium offers the advantages to reach low detection limits (0.05 mg/L) and to avoid handling a liquid in the spectrometer.
SCOPE
1.1 This test method applies for the determination of trace uranium content in natural and waste water. It covers concentration of U between 0.05 mg/L and 2mg/L.
1.2 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-May-2004
Technical Committee
Drafting Committee
Current Stage
Ref Project

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ASTM C1416-04 - Standard Test Method for Uranium Analysis in Natural and Waste Water by X-Ray Fluorescence
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:C1416–04
Standard Test Method for
1
Uranium Analysis Waste Water by X-ray Fluorescence
This standard is issued under the fixed designation C 1416; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 4.2 OtherelementssuchasFe,Cu,Ni,Al,Cr.,whichhave
a higher phosphate solubility at low pH were found to have no
1.1 This test method applies for the determination of trace
effect even at concentration of 10 mg/L.
uranium content in waste water. It covers concentrations of U
4.3 The excess of anions forming strong complexes with the
between 0.05 mg/L and 2 mg/L.
uranyl cation can also bias the uranium determination. As an
1.2 This standard does not purport to address all of the
example, for a solution containing 100 mg/L of F (added as
safety concerns, if any, associated with its use. It is the
NaF) and 0.3 mg/L of uranium, a bias of 30 % was found on
responsibility of the user of this standard to establish appro-
the uranium determination. On the contrary, anions forming
priate safety and health practices and determine the applica-
2- –
weak uranyl complexes (such as SO ,Cl .) were seen to
4
bility of regulatory limitations prior to use.
have no effect even at concentration of several g/L.
2. Summary of Test Method
5. Apparatus
2.1 Uranyl cations are collected on ion exchange cellulose
5.1 Wavelength dispersive X-ray fluorescence spectrom-
phosphate papers by circulating the water to be analysed
eter equipped with a LiF (200) crystal, a molybdenum, tung-
through the paper with a peristaltic pump. After drying, the
sten or rhodium target tube and a scintillation detector.
uranium is determined using X-ray fluorescence.
NOTE 1—Energy dispersive instruments may be applicable.
3. Significance and Use
5.2 Peristaltic pump capable of achieving a flow rate of 50
3.1 Uranium production facilities must control trace ura-
mL/min.
nium content in their waste waters.
5.3 A filtration apparatus which comprises a filter holder, a
3.2 Colorimetric and fluorimetric methods have been devel-
250 mL flask located on top of the filter, and a pipe on bottom
oped but require a tedious separation of interfering elements.
of the filter connected to the peristaltic pump.The sample to be
Trace uranium can also be determined by ICP-MS but not all
analyzed is poured in the flask, flows through the phosphate
water matrices are adapted (for example, waters with high salt
filter and the liquid collected on bottom is brought back to the
content). Direct X-ray fluorescence can be done on the liquid
flask through the peristaltic pump.
but with a detection limit of ;5 mg/L
2
5.4 Pipet—0.2 mL, 1 mL, 5 mL, 10 mL, 20 mL.
3.3 X-ray fluorescence after collection of uranium offers the
5.5 pH - meter.
advantages to reach low detection limits (0.05 mg/L) and to
5.6 100 mL volumetric flasks.
avoid handling a liquid in the spectrometer.
6. Reagents and Materials
4. Interferences
6.1 Purity of Materials—Reagent grade chemicals shall be
4.1 Uraniumiscollectedonthepaperbytheprecipitationof
used in all tests. Unless otherwise indicated, it is intended that
a uranyl phosphate complex at pH = 2.5. Other cations (for
all reagents conform to the specification of the Committee on
example, Pb, Bi, Sn, Zr, As,.) having a low phosphate
Analytical Reagents of the American Chemical Society where
solubility at low pH are also collected and will interfere only at
3
such specifications are available. Other grades may be used
large concentration (the maximum capacity of the paper is 8.5
2
µeq/cm ). As an example, for a solution containing 1 mg/L of
each Pb, Bi, Sn, Zr, andAs, and 0.3 mg/Lof uranium, a bias of
2
5 % was detected on the uranium content. See also 9.2.
Dilution detailed in 6.5 and 6.7 may also be done by weight. In that case, pipets
are not necessary.
3
Reagent Chemicals, American Chemical Society Specifications, American
1
This test method is under the jurisdiction ofASTM Committee C26 on Nuclear Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of listed by the American Chemical society, see Analar Standards for Laboratory
Test. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
CurrenteditionapprovedJune1,2004.PublishedJuly2004.Originallyapproved and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
in 1999. Last previous edition approved in 1999 as C 1416–99. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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