Standard Test Method for Ash Content in Thermoplastics

SCOPE
1.1 This test method was developed to determine the inorganic content of plastics by destructive ashing procedures. Ash levels of 0.01 % or above are covered by this test method.
1.2 These ashing procedures are used only to quantify the residual solids in the polymer and can not be used to identify the individual chemical components of the ash, qualitatively.
1.3 This test method is limited to those materials (including glass) that are stable to 900°C. Test Method D 2584 is recommended for unknown samples, and in instances where fusion of the inorganic portions may be of concern.
1.4 Fluorinated polymers and polymers containing halogenated components have not been included in these procedures.
1.5 Two procedures for determining the inorganic residue in plastics are listed as follows:
1.5.1 Procedure A Muffle-Furnace Technique— For 5 - 50 gram samples. Samples are flamed over a burner prior to being ashed in a muffle furnace.
1.5.2 Procedure B Rapid-Ash Muffle-Furnace Technique— For 5 - 50 gram samples. Samples are ignited and ashed in a muffle furnace.
Note 1—For more efficient ashing, the plastic sample should be in the form of powder or pellet.
Note 2—Procedure B is similar to ISO 3451/1-1981(E).
1.6 The values stated in SI units are to be regarded as the standard.
1.7 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. See Section 9 for specific precautionary statements.

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Status
Historical
Publication Date
09-Sep-2001
Technical Committee
Drafting Committee
Current Stage
Ref Project

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D5630–01
Standard Test Method for
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Ash Content in Plastics
This standard is issued under the fixed designation D 5630; 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* D 2584 Test Method for Ignition Loss of Cured Reinforced
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Resins
1.1 This test method was developed to determine the inor-
E 691 Practice for Conducting an Interlaboratory Study to
ganic content of plastics by destructive ashing procedures.Ash
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Determine the Precision of a Test Method
levels of 0.01 % or above are covered by this test method.
2.2 ISO Standard:
1.2 These ashing procedures are used only to quantify the
ISO3451/1-1981(E) Plastics—DeterminationofAsh—Part
residual solids in the polymer and can not be used to identify
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1, General Methods, 5.3 Method A—Direct Calcination
the individual chemical components of the ash, qualitatively.
1.3 This test method is limited to those materials (including
3. Terminology
glass) that are stable to 900°C. Test Method D 2584 is
3.1 Definitions—For definitions of plastics terms, see Ter-
recommended for unknown samples, and in instances where
minologies D 883 and D 1600. There are no terms in this test
fusion of the inorganic portions may be of concern.
method that require new or other than dictionary definitions.
1.4 Fluorinated polymers and polymers containing haloge-
nated components have not been included in these procedures.
4. Summary of Test Method
1.5 Two procedures for determining the inorganic residue in
4.1 This test method is based on a loss in weight of a plastic
plastics are listed as follows:
sample when combusted to oxidize all organic matter.
1.5.1 Procedure A, Muffle-Furnace Technique—For5–50
gram samples. Samples are flamed over a burner prior to being
5. Significance and Use
ashed in a muffle furnace.
5.1 Inorganic residues from plastics ashing may be anti-
1.5.2 Procedure B, Rapid-Ash Muffle-Furnace Technique—
block, fillers, reinforcements, catalyst residues, colorants, etc.
For5–50 gram samples. Samples are ignited and ashed in a
Thequantitativeamountsofeachareimportantvariablesofthe
muffle furnace.
manufacturing process.
NOTE 1—For more efficient ashing, the plastic sample should be in the
form of powder or pellet. 6. Interferences
NOTE 2—Procedure B is similar to ISO 3451/1-1981(E).
6.1 Aflame height of over 2.5 cm is likely to cause a loss of
1.6 The values stated in SI units are to be regarded as the
fine particles.
standard.
6.2 Largesamplesizes(Note5)couldresultintheevolution
1.7 This standard does not purport to address all of the
of pyrolysis products that could affect the ash recovery.
safety concerns, if any, associated with its use. It is the
6.3 Furnace doors must be in the closed position during the
responsibility of the user of this standard to establish appro-
ignition period to prevent too-rapid oxidation and combustion
priate safety and health practices and determine the applica-
of the sample (Note 7).
bility of regulatory limitations prior to use. See Section 9 for
6.4 Ensure that all crucibles are cooled to ambient tempera-
specific precautionary statements.
ture before weighing.
2. Referenced Documents
7. Apparatus
2.1 ASTM Standards:
7.1 Balance—A balance having the capability to weigh the
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D 883 Terminology Relating to Plastics
sample to the nearest 0.0001 g.The balance should be checked
D 1600 Terminology for Abbreviated Terms Relating to
periodically to ensure accuracy.
2
Plastics
7.2 Crucibles—Porcelain or quartz-fiber, of sufficient size.
NOTE 3—Coors porcelain crucibles, or CEM quartz-fiber crucibles No.
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This test method is under the jurisdiction ofASTM Committee D20 on Plastics
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and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Annual Book of ASTM Standards, Vol 08.02
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Current edition approved September 10, 2001. Published November 2001. Annual Book of ASTM Standards, Vol 14.02.
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Originally published as D 5630 – 94. Last previous edition D 5630 – 94. Available from American National Standards Institute, 25 W. 43rd St., 4th
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Annual Book of ASTM Standards, Vol 08.01. Floor, New York, NY 10036.
*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.
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D5630–01
9.2 Exercise all normal safety precautions when working
with open flames and high temperatures. Use insulated gloves
and long crucible tongs when transferring crucibles.
9.3 Always work with an appropriately vented muffle fur-
nace or under a fume hood when
...

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