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ASTM C1647-20

(Practice)

Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials

Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials

SIGNIFICANCE AND USE
5.1 This practice can be used to separate uranium or plutonium, or both, prior to the impurity analysis by various techniques. The removal of uranium and plutonium prior to quantification can improve the detection limits by minimizing the signal suppression caused by uranium or plutonium when using ICP techniques. Detection limits of ~1–10 part-per-billion (PPB) may be obtainable by matrix removal. Also, removal of the uranium and plutonium may allow the impurities analysis to be performed on a non-glove box enclosed instrument.  
5.2 Other test methods exist to determine impurities in uranium or plutonium. Test Method C1517 is able to determine many impurities in uranium at detection levels of ~1–10 part-per-million (ppm) by DC-Arc Spectrometry. Test Method C1287 is able to determine impurities in uranium at detection levels of ~100 ppb by ICP-MS. Test Method C1432 provides an alternative technique to remove plutonium by ion exchange prior to analysis of the impurities by ICP-AES.  
5.3 This practice can be used to demonstrate compliance with nuclear fuel specifications, for example, Specifications C753, C757, C776, C787, C788, and C996.
SCOPE
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.)  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
1.4 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-Nov-2020
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

Refers
ASTM C787-20 - Standard Specification for Uranium Hexafluoride for Enrichment
Effective Date
01-Mar-2020
Refers
ASTM C996-20 - Standard Specification for Uranium Hexafluoride Enriched to Less Than 5&#x2009;%&#x2009;<sup > 235</sup>U
Effective Date
01-Mar-2020

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ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium MaterialsASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
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ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
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REDLINE ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium MaterialsREDLINE ASTM C1647-20 - Standard Practice for Removal of Uranium or Plutonium, or both, for Impurity Assay in Uranium or Plutonium Materials
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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: C1647 − 20
Standard Practice for
Removal of Uranium or Plutonium, or both, for Impurity
1
Assay in Uranium or Plutonium Materials
This standard is issued under the fixed designation C1647; 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 C787 Specification for Uranium Hexafluoride for Enrich-
ment
1.1 This practice covers instructions for using an extraction
C788 Specification for Nuclear-Grade Uranyl Nitrate Solu-
chromatography column method for the removal of plutonium
tion or Crystals
or uranium, or both, from liquid or digested oxides or metals
C859 Terminology Relating to Nuclear Materials
prior to impurity measurements. Quantification of impurities
C996 Specification for Uranium Hexafluoride Enriched to
can be made by techniques such as inductively coupled plasma
235
Less Than 5 % U
mass spectrometry (ICP-MS), inductively coupled plasma
C1168 PracticeforPreparationandDissolutionofPlutonium
atomic emission spectrometry (ICP-AES), or atomic absorp-
Materials for Analysis
tion spectrometry (AAS.)
C1287 Test Method for Determination of Impurities in
1.2 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
1.3 This standard does not purport to address all of the Materials for Analysis
safety concerns, if any, associated with its use. It is the
C1432 Test Method for Determination of Impurities in
responsibility of the user of this standard to establish appro- Plutonium: Acid Dissolution, Ion Exchange Matrix
priate safety, health, and environmental practices and deter-
Separation, and Inductively Coupled Plasma-Atomic
mine the applicability of regulatory limitations prior to use. Emission Spectroscopic (ICP/AES) Analysis
1.4 This international standard was developed in accor-
C1517 TestMethodforDeterminationofMetallicImpurities
dance with internationally recognized principles on standard- in Uranium Metal or Compounds by DC-Arc Emission
ization established in the Decision on Principles for the
Spectroscopy
Development of International Standards, Guides and Recom-
D1193 Specification for Reagent Water
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
3. Terminology
3.1 Definitions:
2. Referenced Documents
3.1.1 For definitions of terms used in this test method but
2
2.1 ASTM Standards:
not defined herein, refer to Terminology C859.
C753 Specification for Nuclear-Grade, Sinterable Uranium
Dioxide Powder
4. Summary of Practice
C757 Specification for Nuclear-Grade Plutonium Dioxide
4.1 An aliquot of liquid sample or dissolved solid sample is
Powder for Light Water Reactors
adjusted as needed to 8M nitric acid for plutonium/uranium
C776 Specification for Sintered Uranium Dioxide Pellets for
removal using extraction chromatography. Uranium and pluto-
Light Water Reactors
niumareretainedontheresinandtraceimpuritiesarecollected
in the column effluent. The impurities can be measured by a
variety of techniques.
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear
Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of
Test.
5. Significance and Use
Current edition approved Dec. 1, 2020. Published January 2021. Originally
5.1 This practice can be used to separate uranium or
approved in 2006. Last previous edition approved in 2013 as C1647 – 13. DOI:
10.1520/C1647-20.
plutonium, or both, prior to the impurity analysis by various
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
techniques. The removal of uranium and plutonium prior to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
quantification can improve the detection limits by minimizing
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the signal suppression caused by uranium or plutonium when
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1647 − 20
using ICP techniques. Detection limits of ~1–10 part-per- 8.2 Purity of Water—Unless otherwise indicated, references
billion (PPB) may be obtainable by matrix removal. Also, to water shall be understood to mean reagent water as defin
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1647 − 13 C1647 − 20
Standard Practice for
Removal of Uranium or Plutonium, or both, for Impurity
1
Assay in Uranium or Plutonium Materials
This standard is issued under the fixed designation C1647; 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
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)(ICP-AES), or atomic absorption spectrometry (AAS.)
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.4 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.
2. Referenced Documents
2
2.1 ASTM Standards:
C753 Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder
C757 Specification for Nuclear-Grade Plutonium Dioxide Powder for Light Water Reactors
C776 Specification for Sintered Uranium Dioxide Pellets for Light Water Reactors
C787 Specification for Uranium Hexafluoride for Enrichment
C788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Crystals
C859 Terminology Relating to Nuclear Materials
235
C996 Specification for Uranium Hexafluoride Enriched to Less Than 5 % U
C1168 Practice for Preparation and Dissolution of Plutonium Materials for Analysis
C1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma
Mass Spectrometry
C1347 Practice for Preparation and Dissolution of Uranium Materials for Analysis
C1432 Test Method for Determination of Impurities in Plutonium: Acid Dissolution, Ion Exchange Matrix Separation, and
Inductively Coupled Plasma-Atomic Emission Spectroscopic (ICP/AES) Analysis
1
This practice is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.
Current edition approved Jan. 1, 2013Dec. 1, 2020. Published January 2013January 2021. Originally approved in 2006. Last previous edition approved in 20062013 as
C1647 – 06.13. DOI: 10.1520/C1647-13.10.1520/C1647-20.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1647 − 20
C1517 Test Method for Determination of Metallic Impurities in Uranium Metal or Compounds by DC-Arc Emission
Spectroscopy
D1193 Specification for Reagent Water
3. Terminology
3.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.
3.1 Definitions:
3.1.1 For definitions of terms used in this test method but not defined herein, refer to Terminology C859.
4. Summary of Practice
4.1 An aliquot of liquid sample or dissolved solid sample is adjusted as needed to 8M nitric acid for plutonium/uranium removal
using extraction chromatography. Uranium and plutonium are retained on the resin and trace impurities are collected in the column
effluent. The impurities can be measured by a variety of techniques.
5. Significance and Use
5.1 This practice can be used to separate uranium or plutonium, or both, prior to the impurity analysis by various techniques. The
removal of uranium and plutonium prior to quantification can improve the detection li
...

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Standard Practice for Mounting Actinides for Alpha Spectrometry Using Neodymium Fluoride

SIGNIFICANCE AND USE
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  
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Standard Test Method for Moisture Analysis of Plutonium Dioxide (PuO2) by Thermogravimetric Mass Spectrometry (TGA-MS)

SIGNIFICANCE AND USE
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.
SCOPE
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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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.  
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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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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.
SCOPE
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FIG. 1 Activity/Industry that may be Sources of PFAS Use and Release
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SCOPE
1.1 Per- and polyfluoroalkyl substances (PFAS) are a group of over 7,000 manmade compounds consisting of polymeric chains of carbon bonded to fluorine atoms, usually with a polar functional group at the head. This guide recognizes that PFAS can be categorized as polymeric or nonpolymeric, collectively amounting to more than 4,700 Chemical Abstracts Service (CAS)-registered substances. Environmental concerns pertaining to PFAS are centered primarily on the perfluoroalkyl acids (PFAA), a subclass of per-and polyfluoroalkyl substances, which display extreme persistence and chain-length dependent bioaccumulation and adverse effects in biota.  
1.2 The regulatory framework for PFAS continues to evolve, both domestically and internationally. The United States Environmental Protection Agency (EPA) is proceeding with a wide-ranging set of PFAS regulatory actions (EPA, 2021). While the Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA) does not currently recognize PFAS as hazardous substances, the statute does require actions to protect public health and the environment from contaminants and pollutants released to the environment. Other federal regulatory programs, such as the Safe Drinking Water Act are being used to address drinking water supplies adversely impacted by releases of PFAS. The Clean Water Act’s National Pollutant Discharge Elimination System (NPDES) permitting program is tool that both federal and state regulators are using to regulate the inflows of PFAS-impacted wastewaters at both publicly-owned treatment works (POTW) and federally-owned wastewater treatment plants and the concentration of PFAS in permitted effluent. EPA continues to add additional per-and polyfluoroalkyl substances to the list of substances reportable under the federal Toxic Release Inventory (TRI) reporting program. International efforts to address per-and polyfluoroalkyl substances include Australia’s PFAS Nation...

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ASTM
ASTM D7169-23(Test Method)
Standard Test Method for Boiling Point Distribution of Samples with Residues Such as Crude Oils and Atmospheric and Vacuum Residues by High Temperature Gas Chromatography

SIGNIFICANCE AND USE
5.1 The determination of the boiling point distribution of crude oils and vacuum residues, as well as other petroleum fractions, yields important information for refinery operation. These boiling point distributions provide information as to the potential mass percent yield of products. This test method may provide useful information that can aid in establishing operational conditions in the refinery. Knowledge of the amount of residue produced is important in determining the economics of the refining process.
SCOPE
1.1 This test method covers the determination of the boiling point distribution and cut point intervals of crude oils and residues by using high temperature gas chromatography. The amount of residue (or sample recovery) is determined using an external standard.  
1.2 This test method extends the applicability of simulated distillation to samples that do not elute completely from the chromatographic system. This test method is used to determine the boiling point distribution through a temperature of 720 °C. This temperature corresponds to the elution of n-C100.  
1.3 This test method is used for the determination of boiling point distribution of crude oils. This test method uses capillary columns with thin films, which results in the incomplete separation of C4-C8 in the presence of large amounts of carbon disulfide, and thus yields an unreliable boiling point distribution corresponding to this elution interval. In addition, quenching of the response of the detector employed to hydrocarbons eluting during carbon disulfide elution, results in unreliable quantitative analysis of the boiling distribution in the C4-C8 region. Since the detector does not quantitatively measure the carbon disulfide, its subtraction from the sample using a solvent-only injection and corrections to this region via quenching factors, results in an approximate determination of the net chromatographic area. A separate, higher resolution gas chromatograph (GC) analysis of the light end portion of the sample may be necessary in order to obtain a more accurate description of the boiling point curve in the interval in question as described in Test Method D7900 (see Appendix X1).  
1.4 This test method is also designed to obtain the boiling point distribution of other incompletely eluting samples such as atmospheric residues, vacuum residues, etc., that are characterized by the fact that the sample components are resolved from the solvent.  
1.5 A correlation between boiling range distribution results from Test Method D2892, and the weight percentage data determined via this method, is presented in Appendix X2.  
1.6 This test method is not applicable for the analysis of materials containing a heterogeneous component such as polyesters and polyolefins.  
1.7 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.8 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. Specific warning statements are given in Section 8.  
1.9 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.

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ASTM
ASTM D5399-09(2023)(Test Method)
Standard Test Method for Boiling Point Distribution of Hydrocarbon Solvents by Gas Chromatography

SIGNIFICANCE AND USE
5.1 The gas chromatographic determination of the boiling point distribution of hydrocarbon solvents can be used as an alternative to conventional distillation methods for control of solvents quality during manufacture, and specification testing.  
5.2 Boiling point distribution data can be used to monitor the presence of product contaminants and compositional variation during the manufacture of hydrocarbon solvents.  
5.3 Boiling point distribution data obtained by this test method are not equivalent to those obtained by Test Methods D86, D850, D1078, D2887, D2892, and D3710.
SCOPE
1.1 This test method covers the determination of the boiling point distribution of hydrocarbon solvents by capillary gas chromatography. This test method is limited to samples having a minimum initial boiling point of 37 °C (99 °F), a maximum final boiling point of 285 °C (545 °F), and a boiling range of 5 °C to 150 °C (9 °F to 270 °F) as measured by this test method.  
1.2 For purposes of determining conformance of an observed or calculated value using this test method to relevant specifications, test result(s) shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing the specification limit, in accordance with the rounding-off method of Practice E29.  
1.3 The values stated in SI units are standard. The values given in parentheses are for information purposes 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.  
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.

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ASTM
ASTM G136-03(2023)e1(Practice)
Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction

SIGNIFICANCE AND USE
5.1 This practice is suitable for the determination of extractable substances that may be found in materials used in systems or components requiring a high level of cleanliness, such as oxygen systems. Soft goods, such as seals and valve seats, may be tested as received. Gloves and wipes, or samples thereof, to be used in cleaning operations may be evaluated prior to use to ensure that the proposed extracting agent does not extract or deposit chemicals, or both, on the surface to be cleaned.  
5.2 Wipes or other cleaning equipment may be tested after use to determine the amount of contaminant removed from a surface.
Note 1: The amount of material extracted may be dependent upon the frequency and power density of the ultrasonic unit.  
5.3 The extraction efficiency has been shown to vary with the frequency and power density of the ultrasonic unit. The unit, therefore, must be carefully evaluated to optimize the extraction conditions.
SCOPE
1.1 This practice may be used to extract nonvolatile and semivolatile residues from materials such as new and used gloves, new and used wipes, component soft goods, and so forth. When used with proposed cleaning materials (wipes, gloves, and so forth), this practice may be used to determine the potential of the proposed solvent or other fluids to extract contaminants (plasticizers, residual detergents, brighteners, and so forth) and deposit them on the surface being cleaned.  
1.2 This practice is not suitable for the evaluation of particulate contamination.  
1.3 The values stated in SI units are to be regarded standard. No other units of measurement are included in this standard.  
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.  
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.

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