Standard Test Methods for Ashing Cellulose

SCOPE
1.1 These test methods cover four ashing methods for cellulose. These are intended for use on unbleached and bleached cellulose in sheeted or bulk fiber form. Each one of the test methods has advantages, so that preference applications exist for all four.
1.2 The test methods appear as follows:SectionsTest Method A-Ash in Cellulose at 575oC6 to 11Test Method B-Sulfated Ash in Cellulose at 575oC12 to17Test Method C-Ashing Cellulose by Schoniger Oxidation18 to 22Test Method D-Wet Ashing of Cellulose for Inorganics23 to 29
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information 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 and health practices and determine the applicability of regulatory limitations prior to use. For a specific hazard statement, see 20.6.1.

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Publication Date
31-Dec-1999
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D3516–89(Reapproved 2000)
Standard Test Methods for
1
Ashing Cellulose
This standard is issued under the fixed designation D 3516; 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.
NOTE 1—The ash content at this ignition temperature is a reasonable
1. Scope
measure of the mineral salts and inorganic foreign matter in the cellulose.
1.1 These test methods cover four ashing methods for
The weight of ash obtained varies with the temperature of ignition. Higher
cellulose. These are intended for use on unbleached and
temperatures(850°C)willconvertcalciumcarbonateandothercarbonates
bleached cellulose in sheeted or bulk fiber form. Each one of
to the oxides and thus give lower values for ash. The composition of ash
the test methods has advantages, so that preference applica- may vary with the pulping process employed for manufacture, which
limits the significance of the ash determination in absolute terms.
tions exist for all four.
1.2 The test methods appear as follows:
3.2 Test Method B, Sulfated Ash in Cellulose at 575°C—In
Sections
this ashing procedure the metal salts are converted to sulfates
6to11
by treatment with sulfuric acid and ignition at 575 6 25°C to
Test Method A—Ash in Cellulose at 575°C
overcome limitations of Test Method A. It should not be
Test Method B—Sulfated Ash in Cellulose at 575°C 12 to 17
Test Method C—Ashing Cellulose by Schoniger Oxidation 18 to 22
considered as a standard preparative test method for elemental
Test Method D—WetAshing of Cellulose for Inorganics 23 to 29
analysis.
1.3 The values stated in SI units are to be regarded as the
NOTE 2—Conventional dry ashing at high temperature (over 850°C)
standard. The values given in parentheses are for information
results in loss of carbon dioxide from metal carbonates, decomposition of
only.
magnesiumsulfate,andlossofsodiumsalts.Ashingatlowertemperatures
1.4 This standard does not purport to address all of the
(575°C) gives a better estimate of the inorganic impurities, but has the
disadvantage of requiring a long ignition time and also the heat produced
safety concerns, if any, associated with its use. It is the
by the burning pulp can raise the temperature far above 575°C for a short
responsibility of the user of this standard to establish appro-
period of time, converting calcium carbonate to the oxide in varying
priate safety and health practices and determine the applica-
amounts. The sulfated ash method overcomes these objectionable features
bility of regulatory limitations prior to use. For a specific
and has additional advantages. It is relatively insensitive to ignition time.
hazard statement, see 20.6.1.
Ash weight remains constant during weighing, and because the ash does
not melt it will not attack the crucible.
2. Referenced Documents
3.3 Test Method C, Ashing Cellulose by Schoniger
2.1 ASTM Standards:
Oxidation—This test method is generally applicable to ashing
2
D 1193 Specification for Reagent Water
cellulose for subsequent analysis of inorganic constituents.The
3
D 1348 Test Methods for Moisture in Cellulose
procedure utilizes the Schoniger technique in which the cellu-
lose is burned in a combustion flask and all combustion
3. Summary of Test Methods
products are dissolved in an aqueous medium, thus avoiding
3.1 Test Method A, Ash in Cellulose at 575°C—This test
the possibility of physical loss of sample such as can occur in
method measures the ash content of cellulose, which is defined
dry ashing (Test Methods A and B). A limitation is the
for this test as the residue remaining after ignition at 575 6
relatively small sample of 1 g, which can be ashed without
25°C until all carbon has been burned off. It is the simplest of
excessively large apparatus in which to carry out the oxidation
the four test methods for the determination of ash content only,
step. Small specimens may not be adequately representative
and it should not be considered as a standard preparative
where a particulate contaminate is involved.
procedure for elemental analysis.
3.4 Test Method D, Wet Ashing of Cellulose for
Inorganics—This test method is recommended for ashing
cellulose for subsequent analysis of inorganic constituents.The
1
These test methods are under the jurisdiction of ASTM Committee D01 on
procedure employs saturation of the cellulose with a concen-
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
trated solution of hydrogen peroxide followed by incremental
Current edition approved Oct.
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