ASTM D6247-10
(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
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.
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Designation:D6247 −10
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
determination of elemental content in polyolefins by 1.3 This standard does not purport to address all of the
wavelength-dispersive X-ray fluorescence (WDXRF) safety concerns, if any, associated with its use. It is the
spectrometry, in mass fraction ranges typical of those contrib- responsibility of the user of this standard to establish appro-
uted by additives, catalysts, and reactor processes. The ele- priate safety and health practices and determine the applica-
ments covered by this test method include fluorine, sodium, bility of regulatory limitations prior to use. Specific precau-
magnesium, aluminum, silicon, phosphorus, sulfur, calcium, tionary statements are given in Section 10.
titanium, chromium, and zinc in the composition ranges given
NOTE 3—There is no known ISO equivalent to this standard.
in Table 1.
TABLE 1 Mass Fraction Ranges for Additive and Trace Elements
2. Referenced Documents
in Polyolefins
2
2.1 ASTM Standards:
Element Lower Upper
Limit Limit
C1118 Guide for Selecting Components for Wavelength-
(mg/kg) (mg/kg)
Dispersive X-Ray Fluorescence (XRF) Systems (With-
Fluorine 100 300
3
drawn 2011)
Sodium 25 200
Magnesium 10 600
D883 Terminology Relating to Plastics
Aluminum 40 500
D4703 Practice for Compression Molding Thermoplastic
Silicon 30 1000
Phosphorus 5 200 Materials into Test Specimens, Plaques, or Sheets
Sulfur 20 200
D6247 Test Method for Determination of Elemental Content
Calcium 10 300
of Polyolefins by Wavelength Dispersive X-ray Fluores-
Titanium 5 200
Chromium 5 100 cence Spectrometry
Zinc 10 1000
E29 Practice for Using Significant Digits in Test Data to
Determine Conformance with Specifications
1.1.1 This test method does not apply to polymers specifi-
E135 Terminology Relating to Analytical Chemistry for
cally formulated to contain flame retardants including bromi-
Metals, Ores, and Related Materials
nated compounds and antimony trioxide.
E1361 Guide for Correction of Interelement Effects in
1.1.2 This test method does not apply to polymers formu-
lated to contain high levels of compounds of vanadium, X-Ray Spectrometric Analysis
E1601 Practice for Conducting an Interlaboratory Study to
molybdenum, cadmium, tin, barium, lead, and mercury be-
cause the performance may be strongly influenced by spectral Evaluate the Performance of an Analytical Method
E1621 Guide for ElementalAnalysis by Wavelength Disper-
interferences or interelement effects due to these elements.
NOTE 1—Specific methods and capabilities of users may vary with
sive X-Ray Fluorescence Spectrometry
differences in interelement effects and sensitivities, instrumentation and
applications software, and practices between laboratories. Development
3. Terminology
and use of test procedures to measure particular elements, mass fraction
ranges or matrices is the responsibility of individual users.
3.1 Definitions:
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 Aug. 1, 2010. Published September 2010. Originally the ASTM website.
3
approved in 1998. Last previous edition approved in 2004 as D6247 - 98(2004). The last approved version of this historical standard is referenced on
DOI: 10.1520/D6247-10. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6247−10
3.1.1 Definitions of terms applying to XRF and plastics by the limited resolution of the detection subsystem. The
appear in Terminology E135 and Terminology D883, respec- degreeoflineoverlapandthebestmethodtoaccountorcorrect
tively.
for it must be ascertained on an individual basis and must be
considered when calibrating the instrument.
3.2 Defini
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:D6247–98 (Reapproved 2004) Designation: D6247 – 10
Standard Test Method for
Analysis of Elemental Content in Polyolefins By X-ray
Fluorescence SpectrometryDetermination of Elemental
Content of Polyolefins by Wavelength Dispersive X-ray
1
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
1.1This test method covers a general procedure for the determination of elemental content in polyolefins by X-ray fluorescence
spectrometry, in concentration levels typical of those contributed by additives and reactor processes.
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 may be strongly influenced by spectral interferences or
interelement effects due to these elements.
NOTE 1—Specificmethodsandcapabilitiesofusersmayvarywithdifferencesininterelementeffectsandsensitivities,instrumentationandapplications
software, and practices between laboratories. Development and use of test procedures to measure particular elements, concentrationmass 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.
1.2The values stated in SI units are to be regarded as the standard. The inch-pound units given in brackets are for information
only.
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 10.
NOTE3—There is no similar or equivalent ISO standard. 3—There is no known ISO equivalent to this standard.
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 JulyAug. 1, 2004.2010. Published July 2004.September 2010. Originally approved in 1998. Last previous edition approved in 19982004 as
D6247 - 98(2004). DOI: 10.1520/D6247-98R04.10.1520/D6247-10.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D6247 – 10
2. Referenced Documents
2
2.1 ASTM Standards:
C1118 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence (XRF) Systems
D883 Terminology Relating to Plastics
D4703 Practice for Compression Molding Thermoplastic Materials into Test Specimens, Plaques, or Sheets
D6247 Test Method for Analysis of Elemental Content in Polyolefins By 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 E691Practice for Conducting an
Interlaboratory Study to De-
termine the Precision of aTest
Method
E1361 Guide for Correction of Interelement Effects in X-Ray Spectrometric Analysis
E1601 Practice for Conducting a
...
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