ASTM D6247-18
(Test Method)Standard Test Method for Determination of Elemental Content of Polyolefins by Wavelength Dispersive X-ray Fluorescence Spectrometry
Standard Test Method for Determination of Elemental Content of Polyolefins by Wavelength Dispersive X-ray Fluorescence Spectrometry
SIGNIFICANCE AND USE
5.1 Elemental analysis serves as a quality control measure for post-reactor studies, for additive levels in formulated resins, and for finished products. X-ray fluorescence spectrometry is an accurate and relatively fast method to determine mass fractions of multiple elements in polyethylene and polypropylene materials.
SCOPE
1.1 This test method covers a general procedure for the determination of elemental content in polyolefins by wavelength-dispersive X-ray fluorescence (WDXRF) spectrometry, in mass fraction ranges typical of those contributed by additives, catalysts, and reactor processes. The elements covered by this test method include fluorine, sodium, magnesium, aluminum, silicon, phosphorus, sulfur, calcium, titanium, chromium, and zinc in the composition ranges given in Table 1.
1.1.1 This test method does not apply to polymers specifically formulated to contain flame retardants including brominated compounds and antimony trioxide.
1.1.2 This test method does not apply to polymers formulated to contain high levels of compounds of vanadium, molybdenum, cadmium, tin, barium, lead, and mercury because the performance can be strongly influenced by spectral interferences or interelement effects due to these elements.
Note 1: Specific methods and capabilities of users may vary with differences in interelement effects and sensitivities, instrumentation and applications software, and practices between laboratories. Development and use of test procedures to measure particular elements, mass fraction ranges or matrices is the responsibility of individual users.
Note 2: One general method is outlined herein; alternative analytical practices can be followed, and are attached in notes, where appropriate.
1.2 The values stated in SI units are to be regarded as the 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. Specific precautionary statements are given in Section 10.
Note 3: There is no known ISO equivalent to this standard.
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.
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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:D6247 −18
Standard Test Method for
Determination of Elemental Content of Polyolefins by
1
Wavelength Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D6247; 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* 1.2 The values stated in SI units are to be regarded as the
standard.
1.1 This test method covers a general procedure for the
1.3 This standard does not purport to address all of the
determination of elemental content in polyolefins by
safety concerns, if any, associated with its use. It is the
wavelength-dispersive X-ray fluorescence (WDXRF)
responsibility of the user of this standard to establish appro-
spectrometry, in mass fraction ranges typical of those contrib-
priate safety, health, and environmental practices and deter-
uted by additives, catalysts, and reactor processes. The ele-
mine the applicability of regulatory limitations prior to use.
ments covered by this test method include fluorine, sodium,
Specific precautionary statements are given in Section 10.
magnesium, aluminum, silicon, phosphorus, sulfur, calcium,
titanium, chromium, and zinc in the composition ranges given
NOTE 3—There is no known ISO equivalent to this standard.
in Table 1.
1.4 This international standard was developed in accor-
TABLE 1 Mass Fraction Ranges for Additive and Trace Elements
dance with internationally recognized principles on standard-
in Polyolefins
ization established in the Decision on Principles for the
Element Lower Upper
Development of International Standards, Guides and Recom-
Limit Limit
(mg/kg) (mg/kg)
mendations issued by the World Trade Organization Technical
Fluorine 100 300
Barriers to Trade (TBT) Committee.
Sodium 25 200
Magnesium 10 600
Aluminum 40 500 2. Referenced Documents
Silicon 30 1000
2
2.1 ASTM Standards:
Phosphorus 5 200
Sulfur 20 200
C1118 Guide for Selecting Components for Wavelength-
Calcium 10 300
Dispersive X-Ray Fluorescence (XRF) Systems (With-
Titanium 5 200
3
drawn 2011)
Chromium 5 100
Zinc 10 1000
D883 Terminology Relating to Plastics
D4703 Practice for Compression Molding Thermoplastic
1.1.1 This test method does not apply to polymers specifi-
Materials into Test Specimens, Plaques, or Sheets
cally formulated to contain flame retardants including bromi-
D6247 Test Method for Determination of Elemental Content
nated compounds and antimony trioxide.
of Polyolefins by Wavelength Dispersive X-ray Fluores-
1.1.2 This test method does not apply to polymers formu-
cence Spectrometry
lated to contain high levels of compounds of vanadium,
E29 Practice for Using Significant Digits in Test Data to
molybdenum, cadmium, tin, barium, lead, and mercury be-
Determine Conformance with Specifications
cause the performance can be strongly influenced by spectral
E135 Terminology Relating to Analytical Chemistry for
interferences or interelement effects due to these elements.
NOTE 1—Specific methods and capabilities of users may vary with Metals, Ores, and Related Materials
differences in interelement effects and sensitivities, instrumentation and
E1361 Guide for Correction of Interelement Effects in
applications software, and practices between laboratories. Development
X-Ray Spectrometric Analysis
and use of test procedures to measure particular elements, mass fraction
E1601 Practice for Conducting an Interlaboratory Study to
ranges or matrices is the responsibility of individual users.
Evaluate the Performance of an Analytical Method
NOTE 2—One general method is outlined herein; alternative analytical
practices can be followed, and are attached in notes, where appropriate.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2018. Published October 2018. Originally the ASTM website.
3
approved in 1998. Last previous edition approved in 2010 as D6247 - 10. DOI: The last approved version of this historical standard is referenced on
10.1520/D6247-18. www.astm.org.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
...
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: D6247 − 10 D6247 − 18
Standard Test Method for
Determination of Elemental Content of Polyolefins by
1
Wavelength Dispersive X-ray Fluorescence Spectrometry
This standard is issued under the fixed designation D6247; 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 Scope*
1.1 This test method covers a general procedure for the determination of elemental content in polyolefins by wavelength-
dispersive X-ray fluorescence (WDXRF) spectrometry, in mass fraction ranges typical of those contributed by additives, catalysts,
and reactor processes. The elements covered by this test method include fluorine, sodium, magnesium, aluminum, silicon,
phosphorus, sulfur, calcium, titanium, chromium, and zinc in the composition ranges given in Table 1.
TABLE 1 Mass Fraction Ranges for Additive and Trace Elements in Polyolefins
Element Lower Upper
Limit Limit
(mg/kg) (mg/kg)
Fluorine 100 300
Sodium 25 200
Magnesium 10 600
Aluminum 40 500
Silicon 30 1000
Phosphorus 5 200
Sulfur 20 200
Calcium 10 300
Titanium 5 200
Chromium 5 100
Zinc 10 1000
1.1.1 This test method does not apply to polymers specifically formulated to contain flame retardants including brominated
compounds and antimony trioxide.
1.1.2 This test method does not apply to polymers formulated to contain high levels of compounds of vanadium, molybdenum,
cadmium, tin, barium, lead, and mercury because the performance maycan be strongly influenced by spectral interferences or
interelement effects due to these elements.
NOTE 1—Specific methods and capabilities of users may vary with differences in interelement effects and sensitivities, instrumentation and applications
software, and practices between laboratories. Development and use of test procedures to measure particular elements, mass fraction ranges or matrices
is the responsibility of individual users.
NOTE 2—One general method is outlined herein; alternative analytical practices can be followed, and are attached in notes, where appropriate.
1.2 The values stated in SI units are to be regarded as the 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. Specific precautionary statements are given in Section 10.
NOTE 3—There is no known ISO equivalent to this standard.
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.
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Aug. 1, 2010Oct. 1, 2018. Published September 2010October 2018. Originally approved in 1998. Last previous edition approved in 20042010
as D6247 - 98D6247 - 10.(2004). DOI: 10.1520/D6247-10.10.1520/D6247-18.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6247 − 18
2. Referenced Documents
2
2.1 ASTM Standards:
3
C1118 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence (XRF) Systems (Withdrawn 2011)
D883 Terminology Relating to Plastics
D4703 Practice for Compression Molding Thermoplastic Materials into Test Specimens, Plaques, or Sheets
D6247 Test Method for Determination of Elemental Content of Polyolefins by Wavelength Dispersive X-ray Fluorescence
Spectrometry
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E1361 Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1621 Guide for Elemental Analysis by Wavelengt
...
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