ASTM D5630-94
(Test Method)Standard Test Method for Ash Content in Thermoplastics
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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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5630 – 94 An American National Standard
Standard Test Method for
Ash Content in Thermoplastics
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 Determine the Precision of a Test Method
2.2
1.1 This test method was developed to determine the inor-
ISO Standard:
ganic content of thermoplastics by destructive testing tech-
ISO 3451/1-1981(E) Plastics—Determination of Ash— Part
niques. Ash levels of 0.01 % or above are covered by this test
1, General Methods, 5.3 Method A—Direct Calcination
method.
1.2 These ashing procedures are used only to quantify the
3. Terminology
residual solids in the polymer and are not used to identify the
3.1 Definitions—For definitions of plastics terms, see Ter-
individual chemical components of the ash qualitatively.
minologies D 883 and D 1600. There are no terms in this test
1.3 This test method is limited to those materials (including
method that require new or other than dictionary definitions.
glass) that are stable to 900°C.
1.4 Fluorinated polymers or any polymers containing halo-
4. Summary of Test Method
genated components have not been included in these proce-
4.1 This test method is based on a loss in weight of a
dures.
thermoplastic sample that is heated and combusted to oxidize
1.5 Two different techniques for determining the inorganic
all organic matter.
residue in plastics are listed as follows:
1.5.1 Procedure A, Muffle-Furnace Technique—Samples to
5. Significance and Use
be ashed may be in powder or pellet form. This technique uses
5.1 Inorganic residues from thermoplastics ashing may be
large sample sizes. Samples are flamed over a burner prior to
antiblock, fillers, or catalyst residues. The quantitative amounts
being ashed in a muffle furnace.
of each are important variables of the manufacturing process.
1.5.2 Procedure B, Rapid-Ash Muffle-Furnace Technique—
Samples to be ashed may be in a powder or pellet form. This
6. Interferences
technique uses sample sizes of 2 to 8 g. Samples are ignited
6.1 A flame height of over 2.5 cm is likely to cause a loss of
and ashed in a muffle furnace.
fine particles.
NOTE 1—This test method is similar to ISO 3451/1-1981(E).
6.2 Large sample sizes (Note 4) could result in the evolution
of pyrolysis products that could affect the ash recovery.
1.6 The values stated in SI units are to be regarded as the
6.3 Furnace doors must be in the closed position during the
standard.
ignition period to prevent too-rapid oxidation and combustion
1.7 This standard does not purport to address all of the
of the sample (Note 6).
safety concerns, if any, associated with its use. It is the
6.4 Ensure that all crucibles are cooled to ambient tempera-
responsibility of the user of this standard to establish appro-
ture before weighing.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See Section 9 for
7. Apparatus
specific precautionary statements.
7.1 Balance—This shall be a laboratory balance having the
2. Referenced Documents
capability to weigh the sample to the nearest 0.0001 g. The
balance should be checked periodically to ensure accuracy.
2.1 ASTM Standards:
7.2 Crucibles—Porcelain or quartz-fiber, of sufficient size.
D 883 Terminology Relating to Plastics
D 1600 Terminology for Abbreviated Terms Relating to
NOTE 2—Coors porcelain crucibles, or CEM quartz-fiber crucibles No.
Plastics
303040, or equivalents, may be used.
E 691 Practice for Conducting an Interlaboratory Study to
7.3 Muffle Furnace—Electric-resistance-heated or
Annual Book of ASTM Standards, Vol 14.02.
1 4
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics Available from American National Standards Institute, 11 W. 42nd St., 13th
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. Floor, New York, NY 10036.
Current edition approved Oct. 15, 1994. Published December 1994. Porcelain crucibles are available from catalogs such as Fisher. CEM quartz-
Annual Book of ASTM Standards, Vol 08.01. fiber crucibles are available from CEM Corp., Matthews, NC.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5630
microwave-heated furnace, capable of maintaining a tempera- 9.3 Always work with an appropriately vented muffle fur-
ture of 900 6 25°C. nace or under a fume hood when ashing. Irritant fumes are
given off by the polymer during ashing.
NOTE 3—If an electric muffle furnace is used, it should be positioned in
a well-ventilated hood. If a microwave furnace is used, it should be
10. Sampling, Test Specimens, and Test Units
positioned adjacent to the hood and the exhaust tube vented into the hood
10.1 For hygroscopic materials such as nylons, etc., dry
to prevent breathing of the byproducts of the combustion. A microwave
sample specimens to constant weight before testing. (See Table
furnace should be capable of providing an air flow of 2.8 m /min to be
moved through the microwave cavity. and Table )
7.4 Cooling Assembly—A nichrome triangle is positioned
11. Preparation and Apparatus
over a polypropylene funnel connected to a dry compressed-air
11.1 Crucible Preparation—Clean the porcelain crucibles
source, or equivalent. See Fig. 1, Procedure B. Calibrate the air
with tap water and an abrasive detergent. Ensure that any
flow with a wet test meter or bubblemeter to yield a flow rate
baked-in residue is removed from the crucibles completely.
of approximately 30 L/min.
Quartz-fiber crucibles are disposable items and do not require
7.5 Burner.
cleaning.
7.6 Desiccator.
11.2 Fire (condition) the clean crucibles in a muffle furnace
at the set operating temperature for 5 min to burn off any
8. Reagents and Materials
residue in the crucibles.
8.1 Desiccant—Materials suitable for use in the desiccator
11.3 After firing (conditioning) the crucibles, place them in
may be chosen from the following:
a desiccator to cool for 20 to 30 min (porcelain crucibles) or 2
8.1.1 Anhydrous Calcium Sulfate.
min (quartz-fiber crucibles). Handle the crucibles with tongs
8.1.2 Silica Gel.
only. Do not use gloves or cloth to hold the crucibles at any
time.
9. Safety Precautions
12. Calibration and Standardization
9.1 Always wear safety glasses when working in the labo-
12.1 Calibrate the analytical balances in accordance with
ratory.
the manufacturer’s procedure.
9.2 Exercise all normal safety precautions when working
with open flames and high temperatures. Use insulated gloves
13. Procedure A—Muffle Furnace Technique
and long crucible tongs when taking samples out of a muffle
13.1 Sample Type—Determine the type of polymer and
furnace or putting them into it.
anticipated amount of inorganics in the polymer to be ashed.
Determine the ashing temperature, ashing time, and sample
size required to perform the ash analysis in accordance with
Table X1.1.
13.2 Preashing Procedure—Weigh a clean, dry porcelain
crucible to the nearest 0.0001 g. Record the resulting value as
W .
13.2.1 Weigh approximately the amount of material in
accordance with Table X1.1 into the preweighed crucible.
Record the resulting value as W .
13.2.2 Place the crucible on a burner. (The diameter of the
flame equals 2.5 cm, and the height of the flame equals just
enough to touch the wire gauze holding the crucible.) Ensure
that the material does not overflow the crucible. When the flash
point of the polymer is attained (which is approximately 600°C
for most thermoplastics), the polymer begins to burn. To
prevent the loss of fine particles, ensure that the flame intensity
appearing from the crucible is low and that the flame height is
not over 2.5 cm. Continue flaming until there are no visible
flames appearing from the crucible.
13.3 Muffle Furnace—Remove the sample from the burner,
and place it in the muffle furnace (electric or microwave) set at
the desired temperature in accordance with Table X1.1.
13.4 After the pres
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