ASTM C1022-05(2010)
(Test Method)Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate
SIGNIFICANCE AND USE
The test methods in this standard are designed to show whether a given material meets the specifications prescribed in Specification C967.
Because of the variability of matrices of uranium-ore concentrate and the lack of suitable reference or calibration materials, the precision and bias of these test methods should be established by each individual laboratory that will use them. The precision and bias statements given for each test method are those reported by various laboratories and can be used as a guideline.
Instrumental test methods such as X-ray fluorescence and emission spectroscopy can be used for the determination of some impurities where such equipment is available.
SCOPE
1.1 These test methods cover procedures for the chemical and atomic absorption analysis of uranium-ore concentrates to determine compliance with the requirements prescribed in Specification C967.
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Standards Content (Sample)
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Designation:C1022–05(Reapproved2010)
Standard Test Methods for
Chemical and Atomic Absorption Analysis of Uranium-Ore
Concentrate
This standard is issued under the fixed designation C1022; 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 C761 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and Radiochemical Analysis of
1.1 These test methods cover procedures for the chemical
Uranium Hexafluoride
and atomic absorption analysis of uranium-ore concentrates to
C859 Terminology Relating to Nuclear Materials
determine compliance with the requirements prescribed in
C967 Specification for Uranium Ore Concentrate
Specification C967.
C1110 Practice for Sample Preparation for X-Ray Emission
1.2 The analytical procedures appear in the following order:
Spectrometric Analysis of Uranium in Ores Using the
Sections
Glass Fusion or Pressed Powder Method
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
Titrimetry 9 C1219 Test Methods for Arsenic in Uranium Hexafluoride
Nitric Acid-Insoluble Uranium 10 to 18
C1254 Test Method for Determination of Uranium in Min-
Extractable Organic Material 19 to 26
eral Acids by X-Ray Fluorescence
Determination of Arsenic 27
Carbonate by CO Gravimetry 28 to 34 C1267 Test Method for Uranium by Iron (II) Reduction in
Fluoride by Ion-Selective Electrode 35 to 42
Phosphoric Acid Followed by Chromium (VI) Titration in
Halides by Volhard Titration 43 to 50
the Presence of Vanadium
Moisture by Loss of Weight at 110°C 51 to 57
Phosphorus by Spectrophotometry 58 to 66 C1287 Test Method for Determination of Impurities in
Determination of Silicon 67
Nuclear Grade Uranium Compounds by Inductively
Determination of Thorium 68
Coupled Plasma Mass Spectrometry
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
dium by Atomic Absorption Spectrophotometry 69 to 78 C1347 Practice for Preparation and Dissolution of Uranium
Potassium and Sodium by Atomic Absorption
Materials for Analysis
Spectrophotometry 79 to 88
D1193 Specification for Reagent Water
Boron by Spectrophotometry 89 to 98
E60 Practice for Analysis of Metals, Ores, and Related
1.3 This standard does not purport to address all of the
Materials by Molecular Absorption Spectrometry
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 Definitions—For definitions of terms used in these test
bility of regulatory limitations prior to use. A specific precau-
methods, refer to Terminology C859.
tionary statement is given in Section 7.
4. Significance and Use
2. Referenced Documents
4.1 The test methods in this standard are designed to show
2.1 ASTM Standards:
whether a given material meets the specifications prescribed in
Specification C967.
4.2 Because of the variability of matrices of uranium-ore
These test methods are under the jurisdiction of ASTM Committee C26 on
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on
concentrate and the lack of suitable reference or calibration
Methods of Test.
materials, the precision and bias of these test methods should
Current edition approved June 1, 2010. Published June 2010. Originally
be established by each individual laboratory that will use them.
approved in 1984. Last previous edition approved in 2005 as C1022 – 05. DOI:
10.1520/C1022-05R10. The precision and bias statements given for each test method
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
are those reported by various laboratories and can be used as a
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
guideline.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
C1022–05 (2010)
4.3 Instrumental test methods such as X-ray fluorescence NITRIC ACID-INSOLUBLE URANIUM
andemissionspectroscopycanbeusedforthedeterminationof
10. Scope
some impurities where such equipment is available.
10.1 This test method covers the determination of that
5. Interferences
quantity of uranium in uranium-ore concentrate that is not
soluble in nitric acid.
5.1 Interferences are identified in the individual test meth-
ods.
11. Summary of Test Method
5.2 Oreconcentratesareofaveryvariablenature;therefore,
11.1 A sample of ore concentrate is digested in 10 M nitric
all interferences are very difficult to predict. The individual
acidat95to100°Cfor1h.Theslurryisfilteredandtheresidue
user should verify the applicability of each procedure for
washed with 1 M nitric acid until the filtrate gives a negative
specific ore concentrates.
test for uranium. The washed residue is then dried and ignited
at 1000 6 25°C for 1 h. The uranium content is determined on
6. Reagents
the ignited residue by spectrophotometry.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
12. Interference
all reagents shall conform to the specifications of the Commit-
12.1 At the specification limit for nitric acid insoluble
tee onAnalytical Reagents of theAmerican Chemical Society,
3 uranium usually established for uranium-ore concentrates,
where such specifications are available. Other grades may be
interference effects are insignificant.
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
13. Apparatus
accuracy of the determination.
13.1 Digestion Flask, 500-mL, with side entry tube and
6.2 Purity of Water—Unless otherwise indicated, references
attached reservoir.
towatershallbeunderstoodtomeanreagentwaterconforming
13.2 Stirring Apparatus, with sleeve-type stirrer.
to Specification D1193.
13.3 Heating Mantle, 250-W, controlled by a variable trans-
former.
7. Precautions
13.4 Büchner Funnel.
7.1 Properprecautionsshouldbetakentopreventinhalation
13.5 Porcelain Crucibles, 40-mL.
or ingestion of uranium during sample preparation and any
13.6 Muffle Furnace.
subsequent sample analysis.
13.7 Filter Paper, of medium porosity.
13.8 Spectrophotometer, with 1-cm cells that are in accor-
8. Sampling
dance with Practice E60.
8.1 Collect samples in accordance with Specification C967.
8.2 Special requirements for subsampling are given in the
14. Reagents
individual test methods.
14.1 Nitric Acid (10 M)—Dilute 62.5 mL of HNO (sp gr
1.42) to 100 mL with distilled water.
URANIUM BY FERROUS SULFATE
14.2 Nitric Acid (1 M)—Dilute 62.5 mL of HNO (sp gr
REDUCTION—POTASSIUM DICHROMATE
1.42) to 1 L with distilled water.
TITRIMETRY
14.3 Sodium Hydroxide (100 g/L)—Dissolve 10 g of NaOH
in 100 mL of water.
9. Scope
14.4 Hydrogen Peroxide (H O , 30 %).
2 2
9.1 This test method covers the determination of uranium in
14.5 Hydrochloric Acid (HCl, sp gr 1.19).
uranium-ore concentrates. This test method was discontinued
14.6 Hydrofluoric Acid (HF, 48 %).
in January 2002 and replaced with Test Method C1267.
14.7 Sulfuric Acid (9 M)—Add 500 mLH SO (sp gr 1.84)
2 4
9.2 The uranium content of the sample may also be deter-
to 500 mLof iced water with constant stirring. Cool and dilute
mined using Test Method C1254. The user’s laboratory must
to 1 L with water.
establish and document method performance.
15. Procedure
NOTE 1—Dissolution of UOC samples may be achieved using the
15.1 Weigh a 50.0 6 0.1-g sample directly into the diges-
techniques or combination of techniques described in C1347 The labora-
tory must validate the performance of C1347 using characterized UOC
tion flask.
samples. If C1347 methods are not suitable for UOC sample dissolution,
15.2 Place the flask in the heating mantle and adjust the
the user may establish and document applicable dissolution methods.
support ring so that the joints of the flask and sleeve stirrer are
engaged, and the stirrer blades turn freely but just clear the
bottom of the flask.
Reagent Chemicals, American Chemical Society Specifications, American
15.3 Transfer 95 mLof 10 M nitric acid to a 250-mLbeaker
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
and heat between 95 to 100°C.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. Whatman brand No. 40 or its equivalent has been found suitable.
C1022–05 (2010)
15.4 Slowly transfer the heated nitric acid solution to the 16.5 Wash down sides of beaker with water and add 5 mL
digestion flask through the entry side tube with the stirrer of HNO .
turning.
16.6 Cover with a watchglass and digest for approximately
10 min near the boiling point.
NOTE 2—The stirrer is started before the acid is added to prevent
material from sticking to the flask.
16.7 Quantitatively transfer the solution to a 250-mL volu-
metric flask.Add 25 mL of NaOH solution and a few drops of
15.5 Alignathermometerinsuchamannerthatthemercury
H O . Make up to mark with water and mix.
2 2
chamber of the thermometer is immersed in the stirring slurry,
but adequately clears the turning stirrer blades.
NOTE 4—The solution must be basic for yellow sodium peruranate
15.6 Quickly bring the sample to 97°C and digest between
color to develop.
95 to 100°C for 1 h while stirring. (Measure the 1-h digestion
16.8 Measure the absorbance of the solution in a spectro-
time after the temperature of the slurry has reached 97°C.)
photometerat425nmina1-cmcellusingablankasreference.
15.7 Turn off the variable transformer, but allow the stirrer
The blank is prepared by diluting 25 mL of NaOH, plus a few
to continue turning.
drops of H O , to 250 mL with water.
2 2
15.8 Remove the thermometer and carefully rinse with
16.9 Prepare a calibration curve covering the range from 0
water all slurry that adheres to it.
to 50 mg of uranium from aliquots of a standard uranium
15.9 Wipe the immersed portion of the thermometer with
solution. Proceed as in 16.5-16.8. Plot the milligrams of
one fourth of a circle of filter paper and transfer the paper to a
uranium against absorbance readings.
prepared Büchner funnel fitted with a filter paper.
15.10 Add 10 mL of paper pulp to the slurry and continue
16.10 Determine the total milligrams of uranium in the
stirring for about 5 min.
sample solution from the calibration curve.
15.11 Turn off the stirrer, then lower the flask and mantle.
NOTE 5—If the sample solution falls outside the calibration range,
15.12 Carefully wash the slurry that adheres to the stirrer
dilute a portion with the reference-blank solution and read again.
shaft and blades into the flask with water.
15.13 Wipe the shaft and blades with one fourth of a circle
17. Calculation
of filter paper and transfer the filter paper to the Büchner
17.1 Calculate the percentage of insoluble residue, R,
funnel.
present as follows:
15.14 Filter the slurry through the Büchner funnel and wash
contents of the flask into the funnel.
R 3 100
w
R 5 (1)
15.15 Wash the residue with 1 M nitric acid until a 10-mL
S
w
portion of the filtrate shows no detectable yellow color when
where:
made basic with sodium hydroxide and after a few drops of
R = weight of residue (see 15.20), g, and
w
H O (30 %) have been added as a color developer.
2 2
S = weight of samples, g.
w
15.16 Wash the residue several times with water after a
17.2 If the insoluble residue exceeds 0.1 %, calculate the
negative test is obtained.
percentage of nitric acid-insoluble uranium, U , and present as
15.17 Draw air through the filter until the residue and filter
N
follows:
pad are dry.
15.18 Scrape the residue and paper into a preignited
U
U 5 (2)
N
(1000°C) tared 40-mLcrucible, place on a hot plate and slowly S 3 10
w
char off the organic material.
where:
15.19 Ignite the residue for1hat 1000°C in a muffle
U = uranium content calculated in 16.10, mg, and
furnace.
S = weight of sample, g.
w
15.20 Cool the crucible in a desiccator and weigh.
17.3 Calculate the percentage of nitric acid-insoluble ura-
15.21 Calculate the percentage of solids in accordance with
nium, U , on a uranium basis as follows:
u
17.1.
U 3 100
N
NOTE 3—If the percentage of solids (insoluble residue) is greater than
U 5 (3)
u
U
s
0.1 %, grind and mix the residue and determine the total milligrams of
uranium in the residue by the photometric procedure in 16.1-16.10.
where:
U = nitric acid-insoluble residue present (see 17.2), %,
N
16. Photometric Procedure for Uranium
and
16.1 Transfer the ground, blended residue from 15.20 to a
U = uranium in sample, %.
s
100-mL beaker.
16.2 Add 10 mL of water and 10 mL of HCl (sp gr 1.19),
18. Precision and Bias
cover, and boil for 10 min.
18.1 Precision—A relative standard deviation for this test
16.3 Add 5 mL of HNO (sp gr 1.42) and boil until fuming
methodhasbeenreportedas10 %atthe0.2 %HNO insoluble
of NO ceases. Remove cover glass. 3
uranium level (see 4.2).
16.4 Add 5 mL of 9M H SO and 2 mL of HF (48 %), then
2 4
heat to dryness on the hotplate. Bake to fume off remaining 18.2 Bias—For information on the bias of this test method
H SO and cool. see 4.2.
2 4
C1022–05 (2010)
EXTRACTABLE ORGANIC MATERIAL
19. Scope
19.1 This test method is used to determine the extractable
organic material in uranium-ore concentrates. It is recognized
that certain water-soluble organic materials, such as flocculat-
ing agents, are not measured by this test method.
20. Summary of Test Method
20.1 This test method consists of a dual extraction using
n-hexane on the solid uranium-ore concentrate sample and
chloroform on a subsequent nitric acid solution of the sample.
Each of the extractants is evaporated to measure the amount of
organic material extracted.
21. Interferences
21.1 At the specification limit for extractable organic mate-
rial established for uranium-ore concentrations, and within the
scope of this test method, interferences are insignificant.
22. Apparatus
22.1 Soxhlet Extraction Apparatus—The n-hexane extrac-
tion is done in a Soxhlet extraction apparatus. Construct as
follows (see Fig. 1):
22.1.1 Modify a medium Soxhlet extraction tube so that the
sidearm siphon is about 2 cm high, therefore, reducing the
volume of solvent needed. Inserta3to 4-cm long, 25-mm
outside diameter glass tube upright into the extraction tube in
such a m
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