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ASTM C1163-98

(Test Method)

Standard Test Method for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride

Standard Test Method for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride

SCOPE
1.1 This test method covers the preparation of separated fractions of actinides for alpha spectrometry as an alternate to electrodeposition. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples of applicable samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction separation.  
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see Section 8.

General Information

Status
Historical
Publication Date
09-Jul-1998
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
C26 - Nuclear Fuel Cycle
Drafting Committee
C26.05 - Methods of Test
Current Stage
Ref Project

Relations

Replaced By
ASTM C1163-03 - Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
Effective Date
10-Jul-2003

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ASTM C1163-98 - Standard Test Method for Mounting Actinides for Alpha Spectrometry Using Neodymium FluorideASTM C1163-98 - Standard Test Method for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
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ASTM C1163-98 - Standard Test Method for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact
ASTM International (www.astm.org) for the latest information.
Designation: C 1163 – 98
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Mounting Actinides for Alpha Spectrometry Using
1
Neodymium Fluoride
This standard is issued under the fixed designation C 1163; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope problems can be minimized using the neodymium fluoride
method.
1.1 This test method covers the preparation of separated
4.2 The sample mounting technique described in this test
fractions of actinides for alpha spectrometry as an alternate to
method is rapid, adds an additional purification step, since only
electrodeposition. It is applicable to any of the actinides that
those elements that form insoluble fluorides are mounted, and
can be dissolved in dilute hydrochloric acid. Examples of
the sample and filter media can be dissolved and remounted if
applicable samples would be the final elution from an ion
problems occur. The recoveries are better and resolution
exchange separation or the final strip from a solvent extraction
2
approaches normal electrodeposited samples. Recoveries are
separation.
sufficiently high that for survey work, if quantitative recoveries
1.2 This standard does not purport to address all of the
are not necessary, tracers can be omitted. Drawbacks to this
safety concerns, if any, associated with its use. It is the
technique include use of very hazardous hydrofluoric acid and
responsibility of the user of this standard to establish appro-
the possibility of a non-reproducible and ill-defined counting
priate safety and health practices and determine the applica-
geometry from filters that are not flat. Also, although the total
bility of regulatory limitations prior to use. For a specific
turn around time for coprecipitation may be less than for
hazard statement, see Section 8.
electrodeposition, coprecipitation required more time and at-
2. Referenced Documents tention from the analyst.
2.1 ASTM Standards:
5. Interferences
3
D 1193 Specification for Reagent Water
5.1 Calculation of a result from a sample that gives poor
3. Summary of Test Method
resolution should not be attempted since it probably implies an
error in performing the separation procedure.
3.1 Guidance is provided for the sample mounting of
separated actinides using coprecipitation with neodymium
6. Apparatus
fluoride. The purified samples are prepared and mounted on a
6.1 Alpha Spectrometry—A system should be assembled
membrane filter to produce a deposit that yields alpha spectra
that is capable of 60 to 70 keV resolution on an actual sample
equal to electrodeposited samples. Samples can be prepared
prepared by this test method, have a counting efficiency of
more rapidly than by electrodeposition and have comparable
greater than 20 %, and a background of less than 0.005 cpm
resolution.
over each designated energy region. Resolution is defined as
4. Significance and Use the full-width at half-maximum (FWHM) in keV, or the
distance between those points on either side of the alpha energy
4.1 The determination of actinides by alpha spectrometry is
peak where the count is equal to one-half the maximum count.
an essential portion of many environmental programs. Alpha
6.2 Filter—25-mm Metricel (0.1 μm pore) membrane filter
spectrometry allows the identification and quantification of
4
or equivalent.
most alpha-emitting actinides. Although numerous separation
6.3 Vacuum Funnel—Polysulfone twist-lock with stainless
methods are used, the final sample preparation technique is
4
steel screen for filter mounting.
usually by electrodeposition. However, electrodeposition may
6.4 Ultrasonic Bath.
have some drawbacks, such as time required, incompatibility
with prior chemistry, thick deposits, and low recoveries. These
7. Reagents
7.1 Purity of Reagents—Reagent-grade chemicals must be
1
This test method is under the jurisdiction of ASTM Committee C-26 on the used in all procedures. Unless otherwise indicated, all reagents
Nuclear Fuel Cycle.
should conform to the specifications of the Committee on
Current edition approved July 10, 1998. Published October 1998. Originally
Analytical Reagents of the American Chemical Society, if such
published as C 1163 – 92. Last previous edition C 1163 – 93.
2
Hindman, F. D., “Actinide Separations for Alpha Spectrometry Using Neody-
mium Fluoride Coprecipitation,” Analytical Chemistry, 58, 1986, pp. 1236–1241.
3 4
Annual Book of ASTM Standards, Vol 11.01. Available from Gelman Sciences, Ann Arbor, MI.
1

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5.1 The determination of actinides by alpha spectrometry is an essential function of many environmental and other programs. Alpha spectrometry allows the identification and quantification of most alpha-emitting actinides. Although numerous separation methods are used, the final sample preparation technique has historically been by electrodeposition (Practice C1284). However, electrodeposition may have some drawbacks, such as time required, incompatibility with prior chemistry, thick deposits, and low recoveries. These problems may be minimized by using the neodymium fluoride coprecipitation method whose performance is well documented (1-6).4 To a lesser extent cerium fluoride has been used (7) but is not addressed in this practice.  
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SCOPE
1.1 This practice covers the preparation of separated fractions of actinides for alpha spectrometry. It is applicable to any of the actinides that can be dissolved in dilute hydrochloric acid. Examples of applicable samples would be the final elution from an ion exchange separation or the final strip from a solvent extraction separation.2  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM C1909-21(Test Method)
Standard Test Method for Moisture Analysis of Plutonium Dioxide (PuO2) by Thermogravimetric Mass Spectrometry (TGA-MS)

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5.1 This test method is intended for use in quality control laboratories where a quantitative analysis of adsorbed moisture on a PuO2 sample is desired.  
5.2 The parameters described should be considered as guidelines. They may be altered to suit a particular analysis or type of analyzer, provided the changes are validated by the laboratory and noted in the report.  
5.3 The quantity of an adsorbed gas on a given PuO2 sample may indicate specific quality or end use performance characteristics. Specific limits on moisture content, for example, are required in cases where PuO2 will be packaged and stored for extended periods of time.
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1.1 This test method provides necessary information to determine the total amount of moisture (physisorbed and chemisorbed water molecules) in a plutonium dioxide (PuO2) sample using a combination of thermogravimetric and mass spectrometric analyses. This test method is useful when performing analysis in cases where a maximum amount of moisture content in PuO2 samples has been agreed upon by interested parties. For example this method can be used to determine the moisture content of some types of PuO2 packaged to meet the requirements of DOE-STD-3013 (1),2 “Stabilization, Packaging, and Storage of Plutonium-Bearing Materials,” when such PuO2 meets the specifications given in this test method (2).  
1.2 This test method is applicable to PuO2 samples having the following characteristics: Plutonium mass fraction ≥ 83 % (the plutonium in the sample should be close to stoichiometric PuO2 which is approximately 88 wt% plutonium depending on the isotopic composition of the plutonium, but can have several weight percent impurities), moisture ≤1 %.  
1.3 The temperature range of test is typically room temperature to greater than 1000 °C. Typically the PuO2 is heated to 1100 °C.  
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1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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ASTM C1590-21(Practice)
Standard Practice for Alternate Actinide Calibration for Inductively Coupled Plasma-Mass Spectrometry

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5.1 One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities (that is,  232Th and 238U). Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest.  
5.2 The degree of actual mass bias is variable and is dependent upon instrument tune parameters. This standard practice uses universal interference equations to derive a mass bias correction that is specific to the instrument parameters and tune used for sample data acquisition and not based on a historical average.  
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5.4 The methodology that this standard practice is based on has been used for the determination of 232Th and  237Np in enriched uranium solutions and the determination of  241Am in plutonium and uranium legacy oxides following dissolution and ion extraction chromatography separation.  
5.5 Data presented in Section 12 were developed using a quadrupole ICP-MS. This practice can also be applied to high resolution ICP-MS with appropriate validation.
SCOPE
1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest.  
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Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry

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5.1 This test method is designed to determine whether a given material meets the purchaser's specification for plutonium content. This method may also be used, with sufficient qualification, for process control or accountability measurements associated with nuclear materials processing.
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1.1 This test method describes the determination of total plutonium as plutonium(III) in nitrate and chloride solutions. The technique is applicable to solutions resulting from plutonium dioxide powders and pellets (Test Methods C697), nuclear grade mixed oxides (Test Methods C698), plutonium metal (Test Methods C758), and plutonium nitrate solutions (Test Methods C759). Solid samples are dissolved using the appropriate dissolution techniques described in Practice C1168. The use of this technique for other plutonium-bearing materials has been reported (1-6),2 but final determination of applicability must be made by the user. The applicable concentration range for plutonium sample solutions is 10 to 200 g Pu/L.
Note 1: As directly measured in the spectrophotometer, concentrations will be approximately 0.8 to 4.0 g Pu/L. Sample solutions are diluted to reach this target range. For solid samples, select the sample size and dissolved solution weight to yield sample solutions in the 10 to 30 g Pu/L range. With special preparation and spectral analysis techniques, the method has been applied to nitrate solutions in the 0.1 to 10 g Pu/L range.  
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1.1 This practice covers instructions for using an extraction chromatography column method for the removal of plutonium or uranium, or both, from liquid or digested oxides or metals prior to impurity measurements. Quantification of impurities can be made by techniques such as inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES), or atomic absorption spectrometry (AAS.)  
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5.1 The method is designed to show whether or not the tested materials meet the specifications as given in Specifications C787 and C788.
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1.1 This method covers the determination of bromine (Br) and chlorine (Cl) in uranium hexafluoride (UF6) and uranyl nitrate solution. The method as written covers the determination of bromine in UF6 over the concentration range of 0.2 to 8 µg/g, uranium basis. The chlorine in UF6 can be determined over the range of 4 to 160 µg/g, uranium basis. Higher concentrations may be covered by appropriate dilutions. The detection limit for Br is 0.2 µg/g uranium basis and for Cl is 4 µg/g uranium basis.  
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Standard Test Method for Nondestructive Assay of Special Nuclear Material in Low-Density Scrap and Waste by Segmented Passive Gamma-Ray Scanning

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5.1 Segmented gamma-ray scanning provides a nondestructive means of measuring the nuclide content of scrap and waste where the specific nature of the matrix and the chemical form and relationship between the nuclide and matrix may be unknown.  
5.2 The procedure can serve as a diagnostic tool that provides a vertical profile of transmission and nuclide concentration within the item.  
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SCOPE
1.1 This test method covers the transmission-corrected nondestructive assay (NDA) of gamma-ray emitting special nuclear materials (SNMs), most commonly 235U, 239Pu, and 241Am, in low-density scrap or waste, packaged in cylindrical containers. The method can also be applied to NDA of other gamma-emitting nuclides including fission products. High-resolution gamma-ray spectroscopy is used to detect and measure the nuclides of interest and to measure and correct for gamma-ray attenuation in a series of horizontal segments (collimated gamma detector views) of the container. Corrections are also made for counting losses occasioned by signal processing limitations  (1-3).2  
1.2 There are currently several systems in use or under development for determining the attenuation corrections for NDA of radioisotopic materials (4-8). A related technique, tomographic gamma-ray scanning (TGS), is not included in this test method (9, 10, 11).  
1.2.1 This test method will cover two implementations of the Segmented Gamma Scanning (SGS) procedure: (1) Isotope Specific (Mass) Calibration, the original SGS procedure, uses standards of known radionuclide masses to determine detector response in a mass versus corrected count rate calibration that applies only to those specific radionuclides for which it is calibrated, and (2) Efficiency Curve Calibration, an alternative method, typically uses non-SNM radionuclide sources to determine system detection efficiency vs. gamma energy and thereby calibrate for all gamma-emitting radionuclides of interest (12).  
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ASTM C1561-10(2016)(Guide)
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SCOPE
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