ASTM C1416-99
(Test Method)Standard Test Method for Uranium Analysis in Natural and Waste Water by X-Ray Fluorescence
Standard Test Method for Uranium Analysis in Natural and Waste Water by X-Ray Fluorescence
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.
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Designation: C 1416 – 99
Standard Test Method for
Uranium Analysis in Natural and 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 large concentration (the maximum capacity of the paper is 8.5
μeq/cm ). As an example, for a solution containing 1 mg/L of
1.1 This test method applies for the determination of trace
each Pb, Bi, Sn, Zr, and As, and 0.3 mg/L of uranium, a bias of
uranium content in natural and waste water. It covers concen-
5 % was detected on the uranium content. See also 9.2.
trations of U between 0.05 mg/L and 2 mg/L.
4.2 Other elements such as Fe, Cu, Ni, Al, Cr ., which have
1.2 This standard does not purport to address all of the
a higher phosphate solubility at low pH were found to have no
safety concerns, if any, associated with its use. It is the
effect even at concentration of 10 mg/L.
responsibility of the user of this standard to establish appro-
4.3 The excess of anions forming strong complexes with the
priate safety and health practices and determine the applica-
uranyl cation can also bias the uranium determination. As an
bility of regulatory limitations prior to use.
example, for a solution containing 100 mg/L of F (added as
2. Summary of Test Method
NaF) and 0.3 mg/L of uranium, a bias of 30 % was found on
the uranium determination. On the contrary, anions forming
2.1 Uranyl cations are collected on ion exchange cellulose
2- –
weak uranyl complexes (such as SO ,Cl .) were seen to
phosphate papers by circulating the water to be analysed 4
have no effect even at concentration of several g/L.
through the paper with a peristaltic pump. After drying, the
uranium is determined using X-ray fluorescence.
5. Apparatus
3. Significance and Use 5.1 Wavelength dispersive X-ray fluorescence spectrom-
eter equipped with a LiF (200) crystal, a molybdenum, tung-
3.1 Uranium production facilities must control trace ura-
sten or rhodium target tube and a scintillation detector.
nium content in their waste waters as well as in nearby
environmental waters.
NOTE 1—Energy dispersive instruments may be applicable.
3.2 Colorimetric and fluorimetric methods have been devel-
5.2 Peristaltic pump capable of achieving a flow rate of 50
oped but require a tedious separation of interfering elements.
mL/min.
Trace uranium can also be determined by ICP-MS but not all
5.3 A filtration apparatus which comprises a filter holder, a
water matrices are adapted (for example, waters with high salt
250 mL flask located on top of the filter, and a pipe on bottom
content). Direct X-ray fluorescence can be done on the liquid
of the filter connected to the peristaltic pump. The sample to be
but with a detection limit of ;5 mg/L
analyzed is poured in the flask, flows through the phosphate
3.3 X-ray fluorescence after collection of uranium offers the
filter and the liquid collected on bottom is brought back to the
advantages to reach low detection limits (0.05 mg/L) and to
flask through the peristaltic pump.
avoid handling a liquid in the spectrometer.
5.4 Pipet—0.2 mL, 1 mL, 5 mL, 10 mL, 20 mL.
5.5 pH - meter.
4. Interferences
5.6 100 mL volumetric flasks.
4.1 Uranium is collected on the paper by the precipitation of
a uranyl phosphate complex at pH 5 2.5. Other cations (for
6. Reagents and Materials
example, Pb, Bi, Sn, Zr, As,.) having a low phosphate
6.1 Purity of Materials—Reagent grade chemicals shall be
solubility at low pH are also collected and will interfere only at
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specification of the Committee on
This test method is under the jurisdiction of ASTM Committee C-26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test. Dilution detailed in 6.5 and 6.7 may also be done by weight. In that case, pipets
Current edition approved January 10, 1999. Published February 1999. are not necessary.
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C 1416
Analytical Reagents of the American Chemical Society where 7.2.3 Position the drain line so that sample solution is
such specifications are available. Other grades may be used returned to the 250 mL flask. Pour the 100 mL solution (7.2.1)
provided it is first ascertained that the reagent is of sufficiently in the 250 mL flask. Let it flow for 1.5 h.
high purity to permit its use without lessening the accuracy of 7.2.4 Recover the filter and let it dry at 50° C for 1 h.
the determination. 7.3 Place the seven filters in the spectrometer holder, and
6.2 Purity of Water—Conventional distilled water is found analyze each by X rays at the uranium La peak, according to
acceptable for this analysis. manufacturer’s recommendations to achieve the user’s perfor-
6.3 Phosphate paper filters. mance and quality assurance criteria.
7.4 Calibrate the spectrometer with the seven standards.
6.4 Concentrated hydrochloric acid, 12.1 M (sp gr 1.187).
When plotting the X rays fluorescence intensity versus the
6.5 Diluted hydrochloric acid,5 M. Add 41 mL of concen-
concentration, a linear curve should be obtained.
trated hydrochloric acid (sp gr 1.187) to 50 mL H Oina1
...
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