ASTM C1022-05(2010)e1
(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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Designation: C1022 − 05 (Reapproved 2010)
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.
ε NOTE—Sections 1.4 and 7.2 were editorially corrected in August 2010.
1. Scope bility of regulatory limitations prior to use. A specific precau-
tionary statement is given in Section 7.
1.1 These test methods cover procedures for the chemical
and atomic absorption analysis of uranium-ore concentrates to
2. Referenced Documents
determine compliance with the requirements prescribed in
2.1 ASTM Standards:
Specification C967.
C761 Test Methods for Chemical, Mass Spectrometric,
1.2 The analytical procedures appear in the following order:
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
Sections
Uranium Hexafluoride
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
C859 Terminology Relating to Nuclear Materials
Titrimetry 9
C967 Specification for Uranium Ore Concentrate
Nitric Acid-Insoluble Uranium 10 to 18
Extractable Organic Material 19 to 26 C1110 Test Method for Determining Elements in Waste
Determination of Arsenic 27
StreamsbyInductivelyCoupledPlasma-AtomicEmission
Carbonate by CO Gravimetry 28 to 34
Spectroscopy (Withdrawn 2014)
Fluoride by Ion-Selective Electrode 35 to 42
Halides by Volhard Titration 43 to 50 C1219 Test Methods for Arsenic in Uranium Hexafluoride
Moisture by Loss of Weight at 110°C 51 to 57
(Withdrawn 2015)
Phosphorus by Spectrophotometry 58 to 66
C1254 Test Method for Determination of Uranium in Min-
Determination of Silicon 67
Determination of Thorium 68 eral Acids by X-Ray Fluorescence
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
C1267 Test Method for Uranium by Iron (II) Reduction in
dium by Atomic Absorption Spectrophotometry 69 to 78
PhosphoricAcid Followed by Chromium (VI) Titration in
Potassium and Sodium by Atomic Absorption
Spectrophotometry 79 to 88 the Presence of Vanadium
Boron by Spectrophotometry 89 to 98
C1287 Test Method for Determination of Impurities in
1.3 The values stated in SI units are to be regarded as
Nuclear Grade Uranium Compounds by Inductively
standard. No other units of measurement are included in this
Coupled Plasma Mass Spectrometry
standard.
C1347 Practice for Preparation and Dissolution of Uranium
Materials for Analysis
1.4 This standard does not purport to address all of the
D1193 Specification for Reagent Water
safety concerns, if any, associated with its use. It is the
E60 Practice for Analysis of Metals, Ores, and Related
responsibility of the user of this standard to establish appro-
Materials by Spectrophotometry
priate safety and health practices and determine the applica-
1 2
These test methods are under the jurisdiction of ASTM Committee C26 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Methods of Test. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved June 1, 2010. Published June 2010. Originally the ASTM website.
approved in 1984. Last previous edition approved in 2005 as C1022 – 05. DOI: The last approved version of this historical standard is referenced on
10.1520/C1022-05R10E1. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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C1022 − 05 (2010)
3. Terminology skin, causing destruction of deep tissue layers. Unlike other
acids that are rapidly neutralized, hydrofluoric acid reactions
3.1 Definitions—For definitions of terms used in these test
with tissue may continue for days if left untreated. Due to
methods, refer to Terminology C859.
serious consequences of hydrofluoric acid burns, prevention of
exposure or injury of personnel is the primary goal. Utilization
4. Significance and Use
of appropriate laboratory controls (hoods) and wearing ad-
4.1 The test methods in this standard are designed to show
equate personal protective equipment to protect from skin and
whether a given material meets the specifications prescribed in
eye contact is essential.
Specification C967.
4.2 Because of the variability of matrices of uranium-ore
8. Sampling
concentrate and the lack of suitable reference or calibration
8.1 Collect samples in accordance with Specification C967.
materials, the precision and bias of these test methods should
8.2 Special requirements for subsampling are given in the
be established by each individual laboratory that will use them.
individual test methods.
The precision and bias statements given for each test method
are those reported by various laboratories and can be used as a
URANIUM BY FERROUS SULFATE
guideline.
REDUCTION—POTASSIUM DICHROMATE
4.3 Instrumental test methods such as X-ray fluorescence
TITRIMETRY
andemissionspectroscopycanbeusedforthedeterminationof
some impurities where such equipment is available.
9. Scope
9.1 This test method covers the determination of uranium in
5. Interferences
uranium-ore concentrates. This test method was discontinued
5.1 Interferences are identified in the individual test meth-
in January 2002 and replaced with Test Method C1267.
ods.
9.2 The uranium content of the sample may also be deter-
5.2 Oreconcentratesareofaveryvariablenature;therefore,
mined using Test Method C1254. The user’s laboratory must
all interferences are very difficult to predict. The individual
establish and document method performance.
user should verify the applicability of each procedure for
NOTE 1—Dissolution of UOC samples may be achieved using the
specific ore concentrates.
techniques or combination of techniques described in C1347 The labora-
tory must validate the performance of C1347 using characterized UOC
6. Reagents
samples. If C1347 methods are not suitable for UOC sample dissolution,
the user may establish and document applicable dissolution methods.
6.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
NITRIC ACID-INSOLUBLE URANIUM
all reagents shall conform to the specifications of the Commit-
tee onAnalytical Reagents of theAmerican Chemical Society,
10. Scope
where such specifications are available. Other grades may be
10.1 This test method covers the determination of that
used, provided it is first ascertained that the reagent is of
quantity of uranium in uranium-ore concentrate that is not
sufficiently high purity to permit its use without lessening the
soluble in nitric acid.
accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references
11. Summary of Test Method
towatershallbeunderstoodtomeanreagentwaterconforming
11.1 A sample of ore concentrate is digested in 10 M nitric
to Specification D1193.
acidat95to100°Cfor1h.Theslurryisfilteredandtheresidue
7. Precautions washed with 1 M nitric acid until the filtrate gives a negative
test for uranium. The washed residue is then dried and ignited
7.1 Properprecautionsshouldbetakentopreventinhalation
at 1000 6 25°C for 1 h. The uranium content is determined on
or ingestion of uranium during sample preparation and any
the ignited residue by spectrophotometry.
subsequent sample analysis.
7.2 Hydrofluoric acid is a highly corrosive acid that can
12. Interference
severely burn skin, eyes, and mucous membranes. Hydroflu-
12.1 At the specification limit for nitric acid insoluble
oric acid is similar to other acids in that the initial extent of a
uranium usually established for uranium-ore concentrates,
burn depends on the concentration, the temperature, and the
interference effects are insignificant.
duration of contact with the acid. Hydrofluoric acid differs
from other acids because the fluoride ion readily penetrates the
13. Apparatus
13.1 Digestion Flask, 500-mL, with side entry tube and
Reagent Chemicals, American Chemical Society Specifications, American
attached reservoir.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory 13.2 Stirring Apparatus, with sleeve-type stirrer.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
13.3 Heating Mantle, 250-W, controlled by a variable trans-
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. former.
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C1022 − 05 (2010)
13.4 Büchner Funnel. 15.11 Turn off the stirrer, then lower the flask and mantle.
13.5 Porcelain Crucibles, 40-mL. 15.12 Carefully wash the slurry that adheres to the stirrer
shaft and blades into the flask with water.
13.6 Muffle Furnace.
15.13 Wipe the shaft and blades with one fourth of a circle
13.7 Filter Paper, of medium porosity.
of filter paper and transfer the filter paper to the Büchner
13.8 Spectrophotometer, with 1-cm cells that are in accor-
funnel.
dance with Practice E60.
15.14 Filter the slurry through the Büchner funnel and wash
14. Reagents
contents of the flask into the funnel.
14.1 Nitric Acid (10 M)—Dilute 62.5 mL of HNO (sp gr
15.15 Wash the residue with 1 M nitric acid until a 10-mL
1.42) to 100 mL with distilled water.
portion of the filtrate shows no detectable yellow color when
made basic with sodium hydroxide and after a few drops of
14.2 Nitric Acid (1 M)—Dilute 62.5 mL of HNO (sp gr
1.42) to 1 L with distilled water. H O (30 %) have been added as a color developer.
2 2
14.3 Sodium Hydroxide (100 g/L)—Dissolve 10 g of NaOH
15.16 Wash the residue several times with water after a
in 100 mL of water. negative test is obtained.
14.4 Hydrogen Peroxide (H O , 30 %).
15.17 Draw air through the filter until the residue and filter
2 2
pad are dry.
14.5 Hydrochloric Acid (HCl, sp gr 1.19).
15.18 Scrape the residue and paper into a preignited
14.6 Hydrofluoric Acid (HF, 48 %).
(1000°C) tared 40-mLcrucible, place on a hot plate and slowly
14.7 Sulfuric Acid (9 M)—Add 500 mL H SO (sp gr 1.84)
2 4
char off the organic material.
to 500 mLof iced water with constant stirring. Cool and dilute
15.19 Ignite the residue for1hat 1000°C in a muffle
to 1 L with water.
furnace.
15. Procedure
15.20 Cool the crucible in a desiccator and weigh.
15.1 Weigh a 50.0 6 0.1-g sample directly into the diges-
15.21 Calculate the percentage of solids in accordance with
tion flask.
17.1.
15.2 Place the flask in the heating mantle and adjust the
NOTE 3—If the percentage of solids (insoluble residue) is greater than
support ring so that the joints of the flask and sleeve stirrer are
0.1 %, grind and mix the residue and determine the total milligrams of
engaged, and the stirrer blades turn freely but just clear the
uranium in the residue by the photometric procedure in 16.1 – 16.10.
bottom of the flask.
15.3 Transfer 95 mLof 10 M nitric acid to a 250-mLbeaker
16. Photometric Procedure for Uranium
and heat between 95 to 100°C.
16.1 Transfer the ground, blended residue from 15.20 to a
15.4 Slowly transfer the heated nitric acid solution to the
100-mL beaker.
digestion flask through the entry side tube with the stirrer
16.2 Add 10 mL of water and 10 mL of HCl (sp gr 1.19),
turning.
cover, and boil for 10 min.
NOTE 2—The stirrer is started before the acid is added to prevent
16.3 Add 5 mL of HNO (sp gr 1.42) and boil until fuming
material from sticking to the flask.
of NO ceases. Remove cover glass.
15.5 Alignathermometerinsuchamannerthatthemercury
chamber of the thermometer is immersed in the stirring slurry, 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
but adequately clears the turning stirrer blades.
H SO and cool.
2 4
15.6 Quickly bring the sample to 97°C and digest between
95 to 100°C for 1 h while stirring. (Measure the 1-h digestion 16.5 Wash down sides of beaker with water and add 5 mL
time after the temperature of the slurry has reached 97°C.)
of HNO .
15.7 Turn off the variable transformer, but allow the stirrer
16.6 Cover with a watchglass and digest for approximately
to continue turning.
10 min near the boiling point.
15.8 Remove the thermometer and carefully rinse with
16.7 Quantitatively transfer the solution to a 250-mL volu-
water all slurry that adheres to it.
metric flask.Add 25 mL of NaOH solution and a few drops of
H O . Make up to mark with water and mix.
15.9 Wipe the immersed portion of the thermometer with 2 2
one fourth of a circle of filter paper and transfer the paper to a
NOTE 4—The solution must be basic for yellow sodium peruranate
prepared Büchner funnel fitted with a filter paper.
color to develop.
15.10 Add 10 mL of paper pulp to the slurry and continue
16.8 Measure the absorbance of the solution in a spectro-
stirring for about 5 min.
photometerat425nmina1-cmcellusingablankasreference.
The blank is prepared by diluting 25 mL of NaOH, plus a few
Whatman brand No. 40 or its equivalent has been found suitable. drops of H O , to 250 mL with water.
2 2
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C1022 − 05 (2010)
16.9 Prepare a calibration curve covering the range from 0
to 50 mg of uranium from aliquots of a standard uranium
solution. Proceed as in 16.5 – 16.8. Plot the milligrams of
uranium against absorbance readings.
16.10 Determine the total milligrams of uranium in the
sample solution from the calibration curve.
NOTE 5—If the sample solution falls outside the calibration range,
dilute a portion with the reference-blank solution and read again.
17. Calculation
17.1 Calculate the percentage of insoluble residue, R, pres-
ent as follows:
R 3100
w
R 5 (1)
S
w
where:
R = weight of residue (see 15.20), g, and
w
S = weight of samples, g.
w
17.2 If the insoluble residue exceeds 0.1 %, calculate the
percentage of nitric acid-insoluble uranium, U , and present as
N
follows:
U
U 5 (2)
N
S 310
w
where:
U = uranium content calculated in 16.10, mg, and
S = weight of sample, g.
w
17.3 Calculate the percentage of nitric acid-insoluble
uranium, U , on a uranium basis as follows:
u
U 3100
N
U 5 (3)
u
U
s
where:
U = nitric acid-insoluble residue present (see 17.2), %, and
N
U = uranium in sample, %.
s
18. Precision and Bias
18.1 Precision—A relative standard deviation for this test
methodhasbeenreportedas10 %atthe0.2 %HNO insoluble
uranium level (see 4.2).
18.2 Bias—For information on the bias of this test method
see 4.2.
EXTRACTABLE ORGANIC MATERIAL
FIG. 1 Hexane E
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