ASTM D3516-89(2011)
(Test Method)Standard Test Methods for Ashing Cellulose
Standard Test Methods for Ashing Cellulose
SIGNIFICANCE AND USE
Ash content gives an estimation of the inorganic content of cellulose samples. The presence of high levels of ash can be expected to be detrimental to the process of making cellulose derivatives. It also provides a rough estimate of silica content which can have a significant effect on the performance of filters in cellulose derivative manufacturing facilities.
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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3516 − 89 (Reapproved 2011)
Standard Test Methods for
1
Ashing Cellulose
This standard is issued under the fixed designation D3516; 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 and it should not be considered as a standard preparative
procedure for elemental analysis.
1.1 These test methods cover four ashing methods for
cellulose. These are intended for use on unbleached and
NOTE 1—The ash content at this ignition temperature is a reasonable
bleached cellulose in sheeted or bulk fiber form. Each one of
measure of the mineral salts and inorganic foreign matter in the cellulose.
the test methods has advantages, so that preference applica- The weight of ash obtained varies with the temperature of ignition. Higher
temperatures(850°C)willconvertcalciumcarbonateandothercarbonates
tions exist for all four.
to the oxides and thus give lower values for ash. The composition of ash
1.2 The test methods appear as follows:
may vary with the pulping process employed for manufacture, which
limits the significance of the ash determination in absolute terms.
Sections
Test Method A—Ash in Cellulose at 575°C 6 to 11
3.2 Test Method B, Sulfated Ash in Cellulose at 575°C—In
Test Method B—Sulfated Ash in Cellulose at 575°C 12 to 17
Test Method C—Ashing Cellulose by Schoniger Oxidation 18 to 22
this ashing procedure the metal salts are converted to sulfates
Test Method D—Wet Ashing of Cellulose for Inorganics 23 to 29
by treatment with sulfuric acid and ignition at 575 6 25°C to
1.3 The values stated in SI units are to be regarded as the
overcome limitations of Test Method A. It should not be
standard. The values given in parentheses are for information
considered as a standard preparative test method for elemental
only.
analysis.
1.4 This standard does not purport to address all of the
NOTE 2—Conventional dry ashing at high temperature (over 850°C)
safety concerns, if any, associated with its use. It is the
results in loss of carbon dioxide from metal carbonates, decomposition of
responsibility of the user of this standard to establish appro-
magnesiumsulfate,andlossofsodiumsalts.Ashingatlowertemperatures
priate safety and health practices and determine the applica-
(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
bility of regulatory limitations prior to use. For a specific
by the burning pulp can raise the temperature far above 575°C for a short
hazard statement, see 20.6.1.
period of time, converting calcium carbonate to the oxide in varying
amounts. The sulfated ash method overcomes these objectionable features
2. Referenced Documents
and has additional advantages. It is relatively insensitive to ignition time.
2
Ash weight remains constant during weighing, and because the ash does
2.1 ASTM Standards:
not melt it will not attack the crucible.
D1193 Specification for Reagent Water
D1348 Test Methods for Moisture in Cellulose 3.3 Test Method C, Ashing Cellulose by Schoniger
Oxidation—This test method is generally applicable to ashing
3. Summary of Test Methods
cellulose for subsequent analysis of inorganic constituents.The
procedure utilizes the Schoniger technique in which the cellu-
3.1 Test Method A, Ash in Cellulose at 575°C—This test
lose is burned in a combustion flask and all combustion
method measures the ash content of cellulose, which is defined
products are dissolved in an aqueous medium, thus avoiding
for this test as the residue remaining after ignition at 575 6
the possibility of physical loss of sample such as can occur in
25°C until all carbon has been burned off. It is the simplest of
dry ashing (Test Methods A and B). A limitation is the
the four test methods for the determination of ash content only,
relatively small sample of 1 g, which can be ashed without
excessively large apparatus in which to carry out the oxidation
step. Small specimens may not be adequately representative
1
These test methods are under the jurisdiction of ASTM Committee D01 on
where a particulate contaminate is involved.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.
3.4 Test Method D, Wet Ashing of Cellulose for Inorganics—
Current edition approved June 1, 2011. Published June 2011. Originally
This test method is recommended for ashing cellulose for
approved in 1976. Last previous edition approved in 2006 as D3516 – 89 (2006).
DOI: 10.1520/D3516-89R11.
subsequent analysis of inorganic constituents. The pr
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