ASTM C1022-17(2022)

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

• Status: Published
• Publication Date: 30-Jun-2022
• ICS: 27.120.30 - Fissile materials and nuclear fuel technology
• Technical Committee: C26 - Nuclear Fuel Cycle
• Drafting Committee: C26.05 - Methods of Test

Relations

• Refers: ASTM C859-24 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jan-2024
• Refers: ASTM C967-20 - Standard Specification for Uranium Ore Concentrate
• Effective Date: 01-Feb-2020
• Refers: ASTM C1254-18 - Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence
• Effective Date: 01-Oct-2018
• Refers: ASTM C761-18 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 01-Feb-2018
• Refers: ASTM C1287-18 - Standard Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry
• Effective Date: 01-Jan-2018
• Refers: ASTM C859-14a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jun-2014
• Refers: ASTM C859-14 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 15-Jan-2014
• Refers: ASTM C859-13a - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Jun-2013
• Refers: ASTM C859-13 - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-May-2013
• Refers: ASTM C967-13 - Standard Specification for Uranium Ore Concentrate
• Effective Date: 01-Jan-2013
• Refers: ASTM C1254-13 - Standard Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence
• Effective Date: 01-Jan-2013
• Refers: ASTM C967-12 - Standard Specification for Uranium Ore Concentrate
• Effective Date: 01-Jun-2012
• Refers: ASTM C1267-11 - Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
• Effective Date: 01-Jun-2011
• Refers: ASTM C761-11 - Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
• Effective Date: 15-May-2011
• Refers: ASTM C859-10b - Standard Terminology Relating to Nuclear Materials
• Effective Date: 01-Nov-2010

Overview

ASTM C1022-17(2022): Standard Test Methods for Chemical and Atomic Absorption Analysis of Uranium-Ore Concentrate provides comprehensive procedures for analyzing the chemical composition and impurities in uranium-ore concentrates. These standardized test methods allow laboratories to determine whether uranium-ore concentrates meet the requirements defined in ASTM Specification C967, ensuring product quality and regulatory compliance across the nuclear materials industry.

The standard addresses the unique challenges posed by variable uranium-ore matrices and the often limited availability of suitable calibration materials. It emphasizes the need for each laboratory to establish and document its own precision and bias for these methods based on their specific equipment and reference materials.

Key Topics

• Test Methods and Analytical Procedures

  • Uranium determination via ferrous sulfate reduction and potassium dichromate titrimetry
  • Measurement of nitric acid-insoluble uranium
  • Detection of extractable organic materials
  • Quantitation of impurities such as arsenic, halides, carbonate, fluoride, phosphorus, silicon, thorium, calcium, iron, magnesium, molybdenum, titanium, vanadium, potassium, sodium, and boron

• Instrumental Techniques

  • Use of chemical and atomic absorption spectrophotometry for trace elements
  • Application of X-ray fluorescence and emission spectroscopy where available
  • Procedures utilizing photometric and gravimetric analysis

• Lab-Specific Precision and Bias

  • Laboratories must validate method performance with their own reference materials
  • Provided precision and bias values are to be used as guidelines

• Safety and Regulatory Compliance

  • Emphasis on establishing and following appropriate safety, health, and environmental practices
  • Compliance with international standardization principles and WTO Technical Barriers to Trade (TBT) guidelines

Applications

The ASTM C1022-17(2022) standard is crucial in the following fields:

• Nuclear Fuel Processing: Ensures that uranium-ore concentrates used as feed for conversion and enrichment facilities meet stringent quality specifications.
• Quality Control: Supports manufacturers and testing laboratories in verifying the elemental composition and impurity levels of uranium-ore concentrates.
• Regulatory Reporting: Facilitates compliance with national and international regulations governing the nuclear fuel cycle.
• Reference Analysis: Provides methodologies to laboratories developing or validating internal chemical, atomic absorption, and instrumental analysis protocols for uranium compounds.
• Research & Development: Serves as a reference for analytical chemistry R&D involving uranium-ore concentrates and associated materials.

Related Standards

For a complete quality assurance program for uranium materials and their analysis, laboratories and industry professionals often refer to other ASTM standards, including:

• ASTM C967: Specification for Uranium Ore Concentrate – Defines the required chemical and physical properties for uranium-ore concentrates.
• ASTM C859: Terminology Relating to Nuclear Materials – Clarifies definitions and nomenclature.
• ASTM C761: Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride.
• ASTM C1254: Test Method for Determination of Uranium in Mineral Acids by X-Ray Fluorescence.
• ASTM C1267: Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium.
• ASTM C1287: Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by ICP-MS.
• ASTM C1347: Practice for Preparation and Dissolution of Uranium Materials for Analysis.
• ASTM D1193: Specification for Reagent Water.
• ASTM E60: Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry.

Practical Value

Adhering to ASTM C1022-17(2022) promotes uniformity, reliability, and comparability in uranium-ore concentrate analysis. This standard enables testing laboratories, nuclear fuel producers, and regulators to maintain high standards of safety, operational efficiency, and product integrity throughout the nuclear supply chain. By following these internationally recognized methods, stakeholders ensure robust data for quality control, certification, and regulatory documentation of uranium-ore concentrate products.

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 [e-mail]. 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 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
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.
FIG. 1 Hexane Extraction Unit
20. Summary of Test Method
20.1 This test method consists of a dual extraction using
22. Apparatus
n-hexane on the solid uranium-ore concentrate sample and
chloroform on a subsequent nitric acid solution of the sample. 22.1 Soxhlet Extraction Apparatus—The n-hexane extrac-
Each of the extractants is evaporated to measure the amount of tion is done in a Soxhlet extraction apparatus. Construct as
organic material extracted. follows (see Fig. 1):
22.1.1 Modify a medium Soxhlet extraction tube so that the
21. Interferences
sidearm siphon is about 2 cm high, therefore, reducing the
21.1 At the specification limit for extractable organic mate- volume of solvent needed. Insert a 3 cm to 4 cm long, 25 mm
rial established for uranium-ore concentrations, and within the outside diameter glass tube upright into the extraction tube in
scope of this test method, interferences are insignificant. such a manner that an extraction thimble may be placed on it.
C1022 − 17 (2022)
22.1.2 Connect a 250 mL Florence flask, that has a 24/40 24.4 Add a piece of sintered glass or several glass boiling
ground-glass joint on the lower end to the top of the extraction beads and then 120 mL to 125 mL n-hexane to the 250 mL
tube. A 250 mL heating mantle connected to a 7.5 A variable Florence flask. Attach the flask to the Soxhlet extraction tube.
transformer shall be used to heat this.
24.5 Place the heating mantle below the Florence flask,
22.1.3 Connect a Friedrichs condenser, that has a 45/50
connect to the variable transformer set at 55 V to 60 V, and
ground-glass joint on the lower end, to the top of the extraction 1
allow the reagent to reflux rapidly for 3 ⁄2to4h.
tube.Turnthissideofthecondenserupward,andfusetheouter
24.6 Pour the refluxed reagent into a weighed (W in grams)
member of a 24/40 ground-glass joint to it.
platinumdish,andevaporateinahood.Aninfraredlamporhot
22.1.4 Connect a Graham condenser, that has a 24/40
air stream from a heat gun may be used.
ground-glass joint on the lower end, to the modified sidearm of
NOTE 6—Exercise care in this evaporation. If a heat source is used,
the Friedrichs condenser. Unless the relative humidity is low,
adjust the rate of heat input and velocity of air across the dish so that no
insulate the Graham condenser to prevent the condensation of
sample will be mechanically lost. If a heat gun is used, the amount and
water on the outside surface that might seep through the joint
temperature of the air directed against the sample are especially critical
totheFriedrichscondenser.Foaminsulation1cmthickmaybe
because the high rate of evaporation is likely to lower the temperature of
the solution to the point where water will condense in the dish.
used for this purpose. The Graham condenser is cooled with
coldwaterfromawaterbathcooler,andmayberequiredwhen
24.7 Allow the dish to come to room temperature while
n-hexane is used for the extraction.
tilting and rotating it to spread the last few drops of solvent
uniformly over the bottom.
22.2 Heat gun (hot-air electric dryer), may be used to
evaporate the solvent in procedure 24.6 or 24.15.
NOTE 7—Do not allow the temperature of the dish to go below the
dewpoint.
22.3 Extraction Thimbles, with 33 mm I.D., length 94 mm,
24.8 Weigh in open air at intervals on an analytical balance,
and 1.5 mm thick has been found to be suitable.
recording the weight of the dish 5 min after the rate of loss has
22.4 Phase Separator Paper, treated with silicon and about
decreased to 0.5 mg/min.
90 mm in diameter.
NOTE 8—This weight is in grams as W .
24.9 Add a plastic-covered magnetic stirring bar and
23. Reagents
100 mL of (1 + 1) nitric acid to a 400 mL beaker.
23.1 n-hexane—Whenever a new supply is used, it should
24.10 While magnetically stirring the acid, cautiously add
be checked for nonvolatile residue. Evaporate 100.0 mLjust to
the extracted sample from the extraction thimble. Stir until the
drynessinaweightedplatinumdish,cooltoroomtemperature,
sample is dissolved or until it is apparent that practically no
and reweigh the dish. If there is any residue, either make the
more sample will dissolve.
appropriate blank correction or distill the solvent before use to
remove the nonvolatile impurities.
24.11 Cool to about room temperature and transfer to a
500 mL separatory funnel. Add 100.0 mL of chloroform,
23.2 Nitric Acid (1 + 1)—Mix equal volumes of concen-
stopper tightly, and shake as vigorously as possible for 60 s.
trated (sp gr 1.42) reagent grade HNO and water.
24.12 Allow the phases to separate.
23.3 Chloroform—Whenever a new supply of chloroform is
to be used, it should be checked for nonvolatile residue as NOTE 9—If emulsions form, transfer to centrifuge tubes and centrifuge
to separate the phases.
described in 23.1.
24.13 Drain off the lower phase. If the lower phase is the
24. Procedure chloroform layer, filter through a phase-separator filter paper
into a graduated cylinder or narrow-neck flask. If the lower
24.1 Weigh 50.0 g of well-mixed, undried uranium-
phase is the aqueous phase, drain and discard. Then filter the
concentrate sample and transfer to an extraction thimble while
upper phase through a phase-separator filter paper into a
tapping the thimble on a table top to compact and level the
graduated cylinder or narrow-neck flask.
sample.
24.14 Transfer 50.0 mL of the filtered chloroform into an
24.2 Place a plug of glass wool in the thimble above the
ignited (900 °C) platinum dish.
sample. Support the thimble on the glass tube in the Soxhlet
24.15 Place the platinum dish in a hood and evaporate until
extractiontubesothatwhensolventcondensesonthelowertip
about 1 mL of chloroform remains. This evaporation may be
of the Friedrichs condenser, it will drop into the thimble.
done as described in 24.6.
24.3 Connect the extraction tube to the bottom of the
24.16 Allow the dish to cool to room temperature while
Friedrichs condenser that is in series with the Graham con-
tilting and rotating it to spread the last few drops uniformly
denser. Turn on the tap water coolant to the condensers.
over the bottom.
NOTE 5—Tap water may be used in cooling both condensers if the
24.17 Weigh in open air on a recording balance or at
amount of reagent lost during the refluxing (see 24.5) is not greater than
intervals on an analytical balance, recording the weight of the
10 % of the volume added in 24.4. If the tap water is too warm, then the
dish 5 min after the rate of weight loss has decreased to
Graham condenser must be cooled by the refrigerated water cooler, or an
ice-cooled condenser may be used in place of the Graham condenser. 0.5 mg⁄min.
C1022 − 17 (2022)
FIG. 2 Carbonate Apparatus
NOTE 10—This weight is in grams as W .
the C1022 – 02 version can be obtained by visiting
www.astm.org and entering C1022 – 02 into the search.
24.18 Ignite the platinum dish at 900 °C for a minimum of
30 min, cool to room temperature, and weigh.
27.2 With appropriate sample preparation, Atomic Absorp-
tion Spectrometry as described in Test Methods C1219 may be
NOTE 11—This weight is in grams as W .
used for arsenic determination.
25. Calculation
27.3 As an alternative and with appropriate sample
25.1 Calculate the percentage of extractable organic preparation, ICP-MS as described in Test Method C1287 may
material, O , as follows: be used for arsenic determination.
m
100 @~W 2 W !12 ~W 2 W !#
2 1 3 4
CARBONATE BY CO GRAVIMETRY
O 5 (4) 2
m
S
w
28. Scope
where:
W = weight of platinum dish in 24.8,g,
28.1 This test method covers the determination of 0.1 % to
W = weight of platinum dish in 24.6,g,
3 % carbonate in uranium-ore concentrate.
W = weight of platinum dish in 24.17,g,
28.2 The concentration range can be extended by taking
W = weight of platinum dish in 24.18,g,and
smaller sample weights.
S = weight of sample.
w
29. Summary of Test Method
26. Precision and Bias
29.1 The carbonate in the sample is decomposed with
26.1 Precision—A relative standard deviation for this test
hydrochloric acid and evolved as carbon dioxide. The incom-
method has been reported as 18 % at the 0.1 % extractable
ing air is dried and the CO is removed by passing it through
organic level (see 4.2).
NaOH and anhydrous calcium sulfate (CaSO ). The evolved
26.2 Bias—For information on the bias of this test method
gases are scrubbed in H SO to remove moisture and passed
2 4
see 4.2.
through a tower of manganese dioxide and zinc metal to
remove any SO or H S formed. The evolved gas is then
DETERMINATION OF ARSENIC 2 2
absorbed by NaOH in a Nesbitt bulb and determined gravi-
metrically (1).
27. Scope
27.1 The determination of Arsenic by diethyldithiocarbam-
30. Apparatus
ate photometric method has been discontinued. Interested
personscanobtainacopyintheC1022 – 02version.Acopyof 30.1 Carbonate Apparatus, (see Fig. 2).
C1022 − 17 (2022)
A, A'—Heating jacket controlled by variable transformer. Nominal temperature 80 °C to 85 °C for water.
B—One-liter three-necked with gas diffuser and thermometer 0 °C to 110 °C. Water used meeting specification D1193.
C—Tube furnace, controlled by variable transformer with thermocouple. Operating temperature 850 °C 6 25 °C.
D—Sample boat.
E—Pyrohydrolytic tube.
F—Collection system; 10 mL of 0.2 N sodium hydroxide in first tube, 10 mL to 15 mL of water in second tube.
FIG. 3 Pyrohydrolysis Apparatus
31. Reagents 32.7 Boil for 15 min, then shut off the flame.
31.1 Sodium Hydroxide Coated Non-Fibrous Silicate. 32.8 Continue to pass air through the apparatus for an
additional 10 min.
31.2 Anhydrous Calcium Sulfate.
32.9 Remove the Nesbitt bulb and close the stopper imme-
31.3 Glass Wool.
diately.
31.4 Manganese Dioxide, granular.
32.10 Reweigh the Nesbitt bulb to the nearest 0.1 mg.
31.5 Zinc Metal, granular.
32.11 Remove the Erlenmeyer flask from the apparatus
31.6 Sulfuric Acid (H SO , sp gr 1.84).
2 4
while air is still flowing. Leave the air on until the flask is
31.7 Hydrochloric Acid (5.5 M)—Dilute 50 mL of HCl (sp removed to prevent suck-back of the H SO .
2 4
gr 1.19) to 100 mL with water.
32.12 Repeat the procedure in 32.1 – 32.10, without a
sample, to obtain a blank.
32. Procedure
32.1 Weigh a sample (maximum of 5 g) to the nearest
33. Calculation
0.01 g. The sample should contain approximately 20 mg CO .
33.1 Calculate the percentage of carbonate, C , for the
a
Transfer to an Erlenmeyer flask and add enough water to cover
sample and the blank as follows:
the inlet tube.
136.36 ~B 2 C!
32.2 Attach the Nesbitt bulb, open the stopper and pass air
C 5 (5)
a
A
through the apparatus for 10 to 15 min at the rate of 2 to 3
bubbles/s.
where:
32.2.1 Measure the flow rate at the H SO moisture trap.
2 4
A = sample weight, g, (step 32.1),
32.3 Remove the Nesbitt bulb without altering the air flow. B = weight of Nesbitt bulb after absorption of CO , g, (step
32.10), and
Close the stopper and weigh the bulb to nearest 0.1 mg.
C = weight of Nesbitt bulb before absorption of CO,g
32.4 Open the stopper of the bulb and replace it on the
(step 32.3).
apparatus.
33.2 Correct the percentage of CO obtained on the sample
32.5 Evaluate the type of uranium ore concentrate.
for a blank.
32.5.1 If the UOC was produced as any type other than
33.3 Calculate the weight percentage of carbonate, C,on
uranium peroxide, then place 25 mL of 5.5 M HCl in the
u
a uranium basis as follows:
dropping funnel and force it into the flask by replacing the air
inlet tube.
C 3100
c
C 5 (6)
32.5.2 If the uranium-ore concentrate was produced as a u
U
uranium peroxide, replace 25 mL of 5.5 M HCl with 25 mL of
where:
5.5 M H SO to prevent the release of chlorine.
2 4
C = corrected percentage of carbonate in the sample (see
c
32.6 Heat the Erlenmeyer flask with a small burner until the
33.2), and
acid boils and adjust the burner to maintain gentle boiling.
C1022 − 17 (2022)
38.12 Fluoride-Ion Selective Electrode.
U = uranium in the sample, %. This is obtained from a
uranium assay method, for example: C1267 Test
38.13 Millivolt Meter, with saturated calomel reference
Method for Uranium by Iron (II) Reduction in Phos-
electrode capable of reading to 1 mV.
phoric Acid Followed by Chromium (VI) Titration in
38.14 Magnetic Stirrer.
the Presence of Vanadium.
39. Reagents
34. Precision and Bias
39.1 Accelerator—Fluoride-free uranium oxide (U O ).
3 8
34.1 Precision—A relative standard deviation for this test
39.2 Sodium Hydroxide Solution (NaOH, 0.2 N)—Dissolve
method has been reported at 5 % at 1.0 % carbonate level (see
8 g of NaOH in distilled water and dilute to 1 L.
4.2).
39.3 Buffer Solution (0.001 N)—Dissolve 0.1 g of potas-
34.2 Bias—For information about the bias of this test
sium acetate (KC H O ) in water.Add 0.050 mLof acetic acid
method see 4.2.
2 3 2
(sp gr 1.05) and dilute to 1 L.
FLUORIDE BY ION-SELECTIVE ELECTRODE
39.4 Fluoride Solution, Standard (1 mL=10µgF)—
Dissolve in water 0.221 g of sodium fluoride (NaF) previously
35. Scope
dried at 110 °C and dilute to 1 L in a volumetric flask. Pipet
35.1 This test method covers the determination of fluoride
10.0 mL of this solution into a 100 mL volumetric flask and
in uranium-ore concentrates.
dilute to volume with water. Mix and transfer the solution to a
plastic container.
36. Summary of Test Method
36.1 The fluoride is separated pyrohydrolytically by passing 40. Procedure
a stream of moist oxygen over a mixture of sample and
40.1 Adjust the pyrohydrolysis system to operating condi-
fluoride-free uranium oxide (U O ) in a reactor tube at 850 °C.
3 8
tions as follows:
(The U O acts as an accelerator in the presence of high
3 8
40.1.1 Placethereactortubeinthefurnacewiththedelivery
concentrations of sodium, calcium, or magnesium.) The HF
tube as close as possible to the end (5 mm to 10 mm).
formed is absorbed in a dilute solution of sodium hydroxide
40.1.2 Turn on the furnace and allow it to reach 850 °C.
and the fluoride ion concentration is measured with an ion-
Adjust the controls to maintain this temperature within
selective electrode (2, 3, 4).
625 °C.
40.1.3 Fill the three-necked flask half full with water.
37. Interferences
40.1.4 Place the flask on the heating mantle, then connect
37.1 At the specification limit for fluoride, interference
the gas diffuser to the flowmeter and the female socket to the
effects are insignificant.
reactor tube with a spring clamp.
40.1.5 Adjust the control on the heating mantle to bring the
38. Apparatus
temperature of the water to 80 °C to 85 °C.
40.1.6 Turn on the oxygen and adjust the flow to
38.1 Pyrohydrolysis Apparatus, (see Fig. 3).
500 mL⁄min. Flush the apparatus in this manner for 10 to 15
38.2 Gas-Flow Regulator and Flowmeter.
min.
38.3 Three-Necked 1 L Flask.
40.2 Weigh 4 g 6 0.01 g of powdered sample, mix thor-
38.4 Gas Diffuser.
oughly with8gofU O accelerator, and place in a sample
3 8
boat.
38.5 Thermometer.
38.6 Male Ball-Joint Connector. NOTE 12—A blank of8gU O is run in a separate boat.
3 8
40.3 Connect the collection system. The collection system
38.7 Heating Mantle, for 1 L flask, controlled by variable
consists of two 50 mL test tubes in series. The first tube
transformer.
contains 10 mL of 0.2 N NaOH. The second tube contains
38.8 Furnace—A tube furnace capable of maintaining a
10 mL to 15 mL of water. The first tube is fitted with a
temperature of 850 °C. The bore of the furnace should be a
two-holed stopper through which is passed the quartz delivery
minimum of 32 mm (1 ⁄4 in.) in diameter and 330 mm (13 in.)
tube from the pyrohydrolysis apparatus and a glass inverted
in length.
U-tube leading to the second tube. The gas stream escaping
38.9 Reactor Tube, made from clear silica about 30 mm
from the first tube during pyrohydrolysis is carried through the
(1 ⁄8 in.) in diameter and 460 mm (18 in.) in length having a
inverted U-tube into the water in the second test tube. Suffi-
female ball-joint connector at the entrance end and a delivery
cient back pressure is created to ensure that all the fluoride is
tube 9.5 mm ( ⁄8 in.) in diameter and 150 mm in length fused
absorbed in the first tube.
at right angles to the exit end.
NOTE 13—The delivery tube tip should be immersed to a depth of 15
38.10 Absorption Vessels—50 mL glass test tubes.
mm below the surface of the NaOH solution.
38.11 CombustionBoat—Aquartzboatwith10 mLcapacity 40.4 Position the sample boat in the middle of the reactor
and dimensions (100 mm long, 15 mm wide, and 10 mm deep. tube and immediately close the tube.
C1022 − 17 (2022)
40.5 Pyrohydrolyze for 60 min. 44. Summary of Test Method
40.6 Remove the first test tube containing NaOH solution
44.1 Asample of ore concentrate is digested in dilute HNO
and rinse the delivery tube with water into the tube.
without boiling. A known amount of standard silver nitrate
solution is added and the silver halide precipitates that are
40.7 Transfer the contents of the test tube to a 25 mL
formed are filtered. The excess silver nitrate in the filtrate is
volumetric flask. Dilute to mark and mix.
titrated with a standard potassium thiocyanate solution using
40.8 Pipet 1 mLinto a 100 mLplastic beaker, add 24 mLof
ferric ammonium sulfate as indicator.The halide content of the
water and 25 mL of buffer solution.
sample is expressed as a chloride equivalent.
40.9 Place in a magnetic stirrer and insert the electrode pair.
40.10 Set the meter at the millivolt setting and stir the
45. Apparatus
sample solution until a stable reading is reached. Record the
45.1 Filter Paper, ashless with a particle retention of
millivolt reading.
2.5 µm.
40.11 Rinse electrodes with water and dry with absorbent
tissue.
46. Reagents
40.12 Read all samples and blank.
46.1 Silver Nitrate Solution, Standard (0.0500 N)—Weigh
40.13 Prepare a calibration curve by adding, to separate
approximately 8.494 g of finely powdered silver nitrate
100 mL plastic beakers, the following amounts of fluoride
(AgNO ), dried at 110 °C, into a 250 mL beaker. Dissolve the
standard solution (1 mL = 10 µg of fluoride): 0 mL, 0.1 mL,
salt in water and dilute to exactly 1 L. Store the reagent in an
0.5 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL, and 5.0 mL. Dilute
amber-colored bottle.
to25mLwithdistilledwater.Add25mLofbuffersolutionjust
46.2 Potassium Thiocyanate Solution, Standard
prior to measuring each standard individually as in 56.15 and
(0.025 N)—Dissolve 2.43 g of potassium thiocyanate (KSCN)
56.16. Plot mV readings against micrograms of fluoride using
in 1 L of water.
log/linear graph paper.
46.3 Nitric Acid (HNO , sp gr 1.42).
41. Calculation
46.4 Nitric Acid Solution (1 + 4)—Add 200 mL of HNO
41.1 Calculate the percentage of fluoride, F, as follows:
(sp gr 1.42) to 500 mL of water and boil to remove oxides of
C 2 C
~ !
s B
F 5 (7) nitrogen. Dilute the cooled solution to 1 L with water.
W 3400
46.5 Ferric Ammonium Sulfate Indicator Solution—Add
where:
50 g of ferric ammonium sulfate to 200 mL of water and heat
C = fluoride from the calibration curve for the sample, µg,
s
gently to dissolve. Add HNO (sp gr 1.42) dropwise, while
C = fluoride from the calibration curve for the blank, µg,
B
stirring, until the color of the solution changes from brown to
and
pale yellow.
W = sample weight, g.
41.2 Calculate the percentage of fluoride, F , on a uranium
u 47. Standardization of Potassium Thiocyanate Solution
basis as follows:
47.1 Pipet individual 10 mL aliquots of the 0.0500 N silver
F 3100
nitrate solution into two 250 mL beakers.
F 5 (8)
u
U
47.2 Add 25 mL of HNO (1 + 4) solution and 10 mL of
where:
ferric ammonium sulfate indicator solution to each beaker.
F = fluoride (see 41.1), %, and
47.3 Titrate with the potassium thiocyanate solution to the
U = uranium in sample, %. This is obtained from a uranium
first permanent reddish-brown end point.
assay method, for example: C1267 Test Method for
Uranium by Iron (II) Reduction in Phosphoric Acid
0.5
Normality of KSCN 5 (9)
FollowedbyChromium(VI)TitrationinthePresenceof
mean titre ~mL!
Vanadium.
48. Procedure
42. Precision and Bias
48.1 Add 25 mLof boiled nitric acid solution to a 2.00 g 6
42.1 Precision—A relative standard deviation has been
0.01 g sample without cooling and heat for 20 min at low heat.
reported as 7 % at the 0.05 % fluoride level (see 4.2).
Do not boil. (If insoluble residue is evident, filter through filter
42.2 Bias—For information on the bias of this test method
paper using a small amount of paper pulp.)
see 4.2.
48.2 Add 5.0 mL of the AgNO standard solution by pipet
HALIDES BY VOLHARD TITRATION
and stir thoroughly. Heat at low heat until the precipitate
coagulates.
43. Scope
43.1 This test method covers the determination of halides 48.3 Filter off the precipitated silver halides using filter
except fluoride in uranium-ore concentrates. paper. Wash the beaker and filter paper with water.
C1022 − 17 (2022)
48.4 Add 10 mL of ferric ammonium sulfate indicator 54. Interferences
solution to the filtrate and titrate the excess AgNO with the
54.1 There are no known interferences. A blank is run to
KSCN standard solution to the first permanent ferric thiocya-
compensate for any possible absorbance due to the uranyl ion.
nate color.
55. Apparatus
49. Calculation
55.1 Spectrophotometer, with 1 cm cells in accordance with
49.1 Calculate the percentage of halides (expressed as
Practice E60.
chloride), H, as follows:
55.2 Laboratory Shaker, with clamps to hold 250 mL sepa-
H 5 0.177 @A 2 ~B 3C!#
ratory funnels.
(10)
S
55.3 Centrifuge,equippedtohandle15 mLcentrifugetubes.
where:
55.4 Filter Paper, 22 µm ashless.
A = 0.0500 N AgNO added, mL,
56. Reagents
B = 0.025 N KSCN added, mL,
C = KSCN factor, the actual normality of KSCN (see
56.1 Potassium Permanganate Solution (1 %)—Dissolve
47.3) divided by 0.0500,
10 g of potassium permanganate (KMnO ) in water and dilute
0.177 = mg chloride/mL (0.0500 N) AgNO , and
to1L.
S = sample weight, g.
56.2 Sulfurous Acid (H SO )—Saturate water with SO .
2 3 2
49.2 Calculate the percentage of halides, H , on a uranium
u
56.3 Ammonium Vanadate Solution (0.25 %)—Dissolve
basis as follows:
2.5 g of ammonium metavanadate (NH VO ) in 500 mL of
4 3
H 3100
warm water, cool, add 20 mL of HNO (sp gr 1.42) and dilute
H 5 (11)
u
U
to 1 L with water.
where:
56.4 Ammonium Molybdate Solution (10 %)—Dissolve
H = halide from 49.1,%,and
100 g of ammonium molybdate ((NH ) Mo O ·4H O) in
4 6 7 24 2
U = uranium in the sample, %. This is obtained from a
about 800 mL of hot water, cool, and dilute to 1 L. Filter if
uranium assay method, for example: C1267 Test
necessary.
Method for Uranium by Iron (II) Reduction in Phos-
56.5 Isoamyl Alcohol.
phoric Acid Followed by Chromium (VI) Titration in
56.6 Phosphorus Solution, Standard (1 mL = 100 µg P)—
the Presence of Vanadium.
Weigh 4.2638 g of ammonium hydrogen phosphate
((NH ) HPO ). Dissolve in water and dilute to 1 L to produce
50. Precision and Bias 4 2 4
a solution containing 1 mg phosphorus/mL. Dilute 10 mL of
50.1 Precision—A relative standard deviation for this test
1 mg of phosphorus/mL solution to 100 mL to produce a
methodhasbeenreportedas25 %at0.10 %chloridelevel(see
solution containing 100 µg phosphorus/mL.
4.2).
57. Calibration
50.2 Bias—For information on the bias of this test method
see 4.2.
57.1 Prepare a calibration curve by adding 0 mL, 10 mL,
20 mL, 30 mL, 40 mL, and 50 mL of phosphorus standard
51. Determination of Moisture
solution (100 µg of phosphorus/mL) to separate 250 mL
beakers, each containing 0.5 g of pure U O .
51.1 Determination of moisture can be found in Test
3 8
Method C1843.
57.2 Follow 58.2 – 58.19 of the procedure.
57.3 Plot absorbancies corrected for the blank against mil-
PHOSPHORUS BY SPECTROPHOTOMETRY
ligrams of phosphorus.
52. Scope
58. Procedure
52.1 This test method covers the determination of phospho-
58.1 Weigh 0.5 g to 1 g of sample and a blank that is either
rus in uranium-ore concentrates.
nuclear grade UO or U O to the nearest 1 mg into separate
2 3 8
250 mL beakers. The blank and the sample will both follow
53. Summary of Test Method
steps 58.2 – 58.18.
53.1 The phosphorus compounds present in the sample are
58.2 Dissolve the sample in 10 mLof HNO (sp gr 1.42) by
oxidized by potassium permanganate to orthophosphates in
digesting on a hot plate until dissolution is complete.
dilutenitricacidsolution.Additionofammoniumvanadateand
58.3 Dilute the solution to approximately 50 mL to 75 mL
ammonium molybdate produces the colored phospho-
with water.
vanadomolybdate complex.This complex is extracted from the
sample matrix with isoamyl alcohol. The absorbance of the
NOTE 14—Some uranium-ore concentrates may produce an insoluble
extract is then measured spectrophotometrically at 400 nm (5
residueofsilica,inwhichcasethesolutionshouldbefilteredthroughfilter
and 6). paper, and the residue washed well with hot water. The washings should
C1022 − 17 (2022)
be added to the main filtrate. TABLE 1 Instrumental Conditions
Determination Range in
58.4 Transfer the solution to a 500 mL volumetric flask and
Wavelength,
Element Flame Solution Aspirated,
nm
dilute to volume with water. Pipet a 50 mL aliquot into a
µg/mL
250 mL Erlenmeyer flask.
Calcium 422.7 N O/C H 0.02–2
2 2 2
Iron 248.3 N O/C H 0.05–2
2 2 2
58.5 Add 5 mL of 1 % KMnO solution and boil for 3 min.
4 Magnesium 285.2 N O/C H 0.05–2
2 2 2
Molybdenum 313.3 N O/C H 0.2–2
2 2 2
58.6 Add H SO dropwise until the solution clears.
2 3
Titanium 365.3 N O/C H 0.2–2
2 2 2
Vanadium 318.4 N O/C H 0.1–2
2 2 2
58.7 Boil off the excess sulfur dioxide and evaporate the
solution to a volume of about 10 mL.
58.8 Cool the solution and transfer it to a 50 mL stoppered
graduated cylinder keeping the volume to about 30 mL after
three water washings. At this point, ensure that the separatory
U = uranium in the sample, %. This is obtained from a
funnelsarecleanandreadyforuseontheshaker.Proceedfrom
uranium assay method, for example: C1267 Test
this point as rapidly as possible.
Method for Uranium by Iron (II) Reduction in Phos-
phoric Acid Followed by Chromium (VI) Titration in
58.9 Add 5 mL 6 0.5 mL of HNO (sp gr 1.42).
the Presence of Vanadium.
58.10 Add 5 mL of ammonium vanadate solution and mix.
60. Precision and Bias
58.11 Add5mLofammoniummolybdatesolution,diluteto
50 mL, stopper the cylinder, and shake.
60.1 Precision—A relative standard deviation has been
reported as 6 % at 0.5 % phosphorus level, and 25 % at 0.05 %
58.12 Transfertoa250 mLseparatoryfunnelwithoutwash-
phosphorus level (see 4.2).
ing.
60.2 Bias—For information on the bias of this test method
58.13 Add 50 mL 6 0.5 mL of isoamyl alcohol.
see 4.2.
58.14 Shake for 5 min.
DETERMINATION OF SILICON
58.15 Discard the lower aqueous layer, and let a little
solvent run through the spout of the funnel to clean it.
61. Scope
58.16 Transfer a portion of the organic layer to a 15 mL
61.1 The determination of Silicon by gravimetric method
centrifuge tube.
has been discontinued. Interested persons can obtain a copy in
the C1022 – 02 version.Acopy of the C1022 – 02 version can
58.17 Centrifuge for about 1 min.
beobtainedbyvisitingwww.astm.organdenteringC1022 – 02
58.18 Measuretheabsorbanceoftheorganiclayerina1 cm
into the search.
cell at 400 nm using isoamyl alcohol as the reference.
61.2 Silicon may be determined by X-Ray Fluorescence
58.19 Measure the absorbance of the blank solution and
analysis following preparation as described in Practice C1110.
subtract the absorbance from all the sample readings.
DETERMINATION OF THORIUM
58.20 Using either the calibration curve (see 57.3)ora
factor, obtain the phosphorus content in milligrams of the
62. Scope
50 mL aliquot (see 58.4).
62.1 The determination of Thorium by the thorin photomet-
ric method has been discontinued. Interested persons can
59. Calculation
obtain a copy in the C1022-02 version.
59.1 Calculate the percentage of phosphorus, P, as follows:
62.2 With appropriate sample preparation, ICP-MS as de-
C
scribed in Test Method C1287 may be used for thorium
P 5 (12)
W
determination.
where:
CALCIUM, IRON, MAGNESIUM, MOLYBDENUM,
C = phosphorus in the aliquot (see 58.20), mg, and
TITANIUM, AND VANADIUM BY ATOMIC
W = weight of sample, g.
ABSORPTION SPECTROPHOTOMETRY
59.2 Calculate percentage of phosphorus, P , on a uranium
u
basis as follows: 63. Scope
100 C
63.1 This test method is suitable for the determination of
P 5 (13)
u
W 3U calcium, iron, magnesium, molybdenum, titanium, and vana-
dium in uranium-ore concentrates. The nominal determination
where:
ranges of the elements are given in Table 1. The range of
C = phosphorus in the aliquot, mg,
concentrations measured can be varied considerably by appro-
W = weight of sample, g, and
priate dilution of the sample solution (7).
C1022 − 17 (2022)
63.2 For simultaneous determination of metals by plasma 67.7 Iron Solution, Standard (1 mg/mL)—Dissolve 500 mg
emission spectroscopy refer to Test Methods C761, Sections 6 1 mg of pure iron (Fe) in 50 mL
...