ASTM C1022-17(2022)
(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
4.1 The test methods in this standard are designed to show whether a given material meets the specifications prescribed in Specification C967.
4.2 Because of the variability of matrices of uranium-ore concentrate and the limited availability 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.
4.3 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.
1.2 The analytical procedures appear in the following order:
Sections
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
Titrimetry
9
Nitric Acid-Insoluble Uranium
10 to 18
Extractable Organic Material
19 to 26
Determination of Arsenic
27
Carbonate by CO2 Gravimetry
28 to 34
Fluoride by Ion-Selective Electrode
35 to 42
Halides by Volhard Titration
43 to 50
Phosphorus by Spectrophotometry
52 to 60
Determination of Silicon
61
Determination of Thorium
62
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
dium by Atomic Absorption Spectrophotometry
63 to 72
Potassium and Sodium by Atomic Absorption
Spectrophotometry
73 to 82
Boron by Spectrophotometry
83 to 92
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. A specific precautionary statement is given in Section 7.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1022 − 17 (Reapproved 2022)
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 2. Referenced Documents
2.1 ASTM Standards:
1.1 These test methods cover procedures for the chemical
and atomic absorption analysis of uranium-ore concentrates to C761 Test Methods for Chemical, Mass Spectrometric,
Spectrochemical, Nuclear, and RadiochemicalAnalysis of
determine compliance with the requirements prescribed in
Specification C967. Uranium Hexafluoride
C859 Terminology Relating to Nuclear Materials
1.2 The analytical procedures appear in the following order:
C967 Specification for Uranium Ore Concentrate
Sections
C1110 Test Method for Determining Elements in Waste
Uranium by Ferrous Sulfate Reduction—Potassium Dichromate
StreamsbyInductivelyCoupledPlasma-AtomicEmission
Titrimetry 9
Spectroscopy (Withdrawn 2014)
Nitric Acid-Insoluble Uranium 10 to 18
Extractable Organic Material 19 to 26
C1219 Test Methods for Arsenic in Uranium Hexafluoride
Determination of Arsenic 27
(Withdrawn 2015)
Carbonate by CO Gravimetry 28 to 34
Fluoride by Ion-Selective Electrode 35 to 42 C1254 Test Method for Determination of Uranium in Min-
Halides by Volhard Titration 43 to 50
eral Acids by X-Ray Fluorescence
Phosphorus by Spectrophotometry 52 to 60
C1267 Test Method for Uranium by Iron (II) Reduction in
Determination of Silicon 61
Determination of Thorium 62 PhosphoricAcid Followed by Chromium (VI) Titration in
Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-
the Presence of Vanadium
dium by Atomic Absorption Spectrophotometry 63 to 72
C1287 Test Method for Determination of Impurities in
Potassium and Sodium by Atomic Absorption
Spectrophotometry 73 to 82 Nuclear Grade Uranium Compounds by Inductively
Boron by Spectrophotometry 83 to 92
Coupled Plasma Mass Spectrometry
1.3 The values stated in SI units are to be regarded as C1347 Practice for Preparation and Dissolution of Uranium
standard. The values given in parentheses are for information Materials for Analysis
only. C1843 Test Method for Determining Moisture Content in
Uranium-Ore Concentrate
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, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. A
3. Terminology
specific precautionary statement is given in Section 7.
3.1 Definitions—For definitions of terms used in these test
1.5 This international standard was developed in accor-
methods, refer to Terminology C859.
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
4. Significance and Use
Development of International Standards, Guides and Recom-
4.1 The test methods in this standard are designed to show
mendations issued by the World Trade Organization Technical
whether a given material meets the specifications prescribed in
Barriers to Trade (TBT) Committee.
Specification C967.
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 July 1, 2022. Published July 2022. Originally approved the ASTM website.
in 1984. Last previous edition approved in 2017 as C1022 – 17. DOI: 10.1520/ The last approved version of this historical standard is referenced on
C1022-17R22. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1022 − 17 (2022)
4.2 Because of the variability of matrices of uranium-ore 8. Sampling
concentrate and the limited availability of suitable reference or
8.1 Collect samples in accordance with Specification C967.
calibration materials, the precision and bias of these test
8.2 Special requirements for subsampling are given in the
methods should be established by each individual laboratory
individual test methods.
that will use them. The precision and bias statements given for
each test method are those reported by various laboratories and
URANIUM BY FERROUS SULFATE
can be used as a 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.
techniquesorcombinationoftechniquesdescribedinPracticeC1347.The
laboratory must validate the performance of Practice C1347 using
6. Reagents characterized UOC samples. If Practice C1347 methods are not suitable
for UOC sample dissolution, the user may establish and document
6.1 Purity of Reagents—Reagent grade chemicals shall be
applicable dissolution methods.
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,
where such specifications are available. Other grades may be 10. Scope
used, provided it is first ascertained that the reagent is of
10.1 This test method covers the determination of that
sufficiently high purity to permit its use without lessening the
quantity of uranium in uranium-ore concentrate that is not
accuracy of the determination.
soluble in nitric acid.
6.2 Purity of Water—Unless otherwise indicated, references
11. Summary of Test Method
towatershallbeunderstoodtomeanreagentwaterconforming
to type I water in Specification D1193.
11.1 A sample of ore concentrate is digested in 10 M nitric
acid at 95 °C to 100 °C for 1 h. The slurry is filtered and the
7. Precautions
residue washed with 1 M nitric acid until the filtrate gives a
7.1 Properprecautionsshouldbetakentopreventinhalation negativetestforuranium.Thewashedresidueisthendriedand
or ingestion of uranium during sample preparation and any ignited at 1000 °C 6 25 °C for 1 h. The uranium content is
subsequent sample analysis. determined on the ignited residue by spectrophotometry.
7.2 Hydrofluoric acid is a highly corrosive acid that can
12. Interference
severely burn skin, eyes, and mucous membranes. Hydroflu-
oric acid differs from other acids because the fluoride ion 12.1 At the specification limit for nitric acid insoluble
readily penetrates the skin, causing destruction of deep tissue uranium usually established for uranium-ore concentrates,
layers. Unlike other acids that are rapidly neutralized, hydro- interference effects are insignificant.
fluoric acid reactions with tissue may continue for days if left
untreated.FamiliarizationandcompliancewiththeSafetyData 13. Apparatus
Sheet is essential.
13.1 Digestion Flask, 500 mL, with side entry tube and
7.3 Chloroform is a dangerous chemical causing acute
attached reservoir.
toxicity with repeated inhalation, dermal, or oral exposure.
13.2 Stirring Apparatus, with sleeve-type stirrer.
Many health hazards are associated with exposure to chloro-
13.3 Heating Mantle, 250 W, controlled by a variable trans-
form including its potential to cause cancer. Familiarization
former.
and compliance with the Safety Data Sheet is essential.
13.4 Büchner Funnel.
13.5 Porcelain Crucibles, 40 mL.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
13.6 Muffle Furnace.
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
13.7 Filter Paper, ashless of medium porosity, and a me-
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
dium flow rate with a particle retention of 8 µm has been found
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD. to be suitable.
C1022 − 17 (2022)
13.8 Spectrophotometer, with 1 cm cells that are in accor- 15.13 Wipe the shaft and blades with one fourth of a circle
dance with Practice E60. of filter paper and transfer the filter paper to the Büchner
funnel.
14. Reagents
15.14 Filter the slurry through the Büchner funnel and wash
contents of the flask into the funnel.
14.1 Nitric Acid (10 M)—Dilute 62.5 mL of HNO (sp gr
1.42) to 100 mL with distilled water.
15.15 Wash the residue with 1 M nitric acid until a 10 mL
portion of the filtrate shows no detectable yellow color when
14.2 Nitric Acid (1 M)—Dilute 62.5 mL of HNO (sp gr
made basic with sodium hydroxide and after a few drops of
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 %).
2 2
15.17 Draw air through the filter until the residue and filter
14.5 Hydrochloric Acid (HCl, sp gr 1.19).
pad are dry.
14.6 Hydrofluoric Acid (HF, 48 %).
15.18 Scrape the residue and paper into a preignited
(1000 °C)tared40 mLcrucible,placeonahotplateandslowly
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
to 1 L with water.
15.19 Ignite the residue for1hat 1000 °C in a muffle
furnace.
15. Procedure
15.20 Cool the crucible in a desiccator and weigh.
15.1 Weigh a 50.0 g 6 0.1 g sample directly into the
15.21 Calculate the percentage of solids in accordance with
digestion flask.
17.1. If the percentage of solids (insoluble residue) is greater
15.2 Place the flask in the heating mantle and adjust the than 0.1 %, grind and mix the residue and determine the total
support ring so that the joints of the flask and sleeve stirrer are milligrams of uranium in the residue by the photometric
engaged, and the stirrer blades turn freely but just clear the procedure in 16.1 – 16.10.
bottom of the flask.
16. Photometric Procedure for Uranium
15.3 Transfer 95 mLof 10 M nitric acid to a 250 mLbeaker
and heat between 95 °C to 100 °C. 16.1 Transfer the ground, blended residue from 15.20 to a
100 mL beaker.
15.4 Slowly transfer the heated nitric acid solution to the
16.2 Add 10 mL of water and 10 mL of HCl (sp gr 1.19),
digestion flask through the entry side tube with the stirrer
turning. cover, and boil for 10 min.
16.3 Add 5 mL of HNO (sp gr 1.42) and boil until fuming
NOTE 2—The stirrer is started before the acid is added to prevent 3
of NO ceases. Remove cover glass.
material from sticking to the flask.
15.5 Adjust the thermometer so that the bulb of the ther- 16.4 Add 5 mL of 9M H SO and 2 mL of HF (48 %), then
2 4
mometer is immersed in the stirring slurry, but adequately heat to dryness on the hotplate. Bake to fume off remaining
clears the turning stirrer blades. H SO and cool.
2 4
16.5 Wash down sides of beaker with water and add 5 mL
15.6 Quickly bring the sample to 97 °C and digest between
95 °C to 100 °C for 1 h while stirring. (Measure the 1-h of HNO .
digestion time after the temperature of the slurry has reached
16.6 Cover with a watchglass and digest for approximately
97 °C.)
10 min near the boiling point.
15.7 Turn off the variable transformer, but allow the stirrer
16.7 Quantitatively transfer the solution to a 250 mL volu-
to continue turning.
metric flask.Add 25 mL of NaOH solution and a few drops of
H O . Make up to mark with water and mix.
15.8 Remove the thermometer and carefully rinse with 2 2
water all slurry that adheres to it.
NOTE 3—The solution must be basic for yellow sodium peruranate
color to develop.
15.9 Wipe the immersed portion of the thermometer with
16.8 Measure the absorbance of the solution in a spectro-
one fourth of a circle of filter paper and transfer the paper to a
prepared Büchner funnel fitted with a filter paper. photometer at 425 nmin a 1 cmcell using a blankasreference.
The blank is prepared by diluting 25 mL of a 100 g/L NaOH
15.10 Add 10 mL of paper pulp to the slurry and continue
solution, plus a few drops of H O , to 250 mL with water.
2 2
stirring for about 5 min.
16.9 Prepare a calibration curve covering the range from
15.11 Turn off the stirrer, then lower the flask and mantle.
0 mg to 50 mg of uranium from aliquots of a standard uranium
15.12 Carefully wash the slurry that adheres to the stirrer solution. Proceed as in 16.5 – 16.8. Plot the milligrams of
shaft and blades into the flask with water. uranium against absorbance readings.
C1022 − 17 (2022)
16.10 Determine the total milligrams of uranium in the
sample solution from the calibration curve.
NOTE 4—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 sam
...
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