Ash in A Graphite Sample: Standard Test Method For

An American National Standard
Designation: C 561 – 91 (Reapproved 2005)
Standard Test Method for

Ash in a Graphite Sample1
This standard is issued under the fixed designation C 561; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope crucibles, and (2) the possible chemical combination of trace

1.1 This test method provides a practical determination for elements with the ceramic crucible.
the ash content in a graphite sample. 4.2 Any ash or trace elements introduced to the sample will
1.2 This standard does not purport to address all of the influence results. Contamination can occur during drilling to
safety concerns, if any, associated with its use. It is the obtain the sample and during pulverization. (See 6.1.)
responsibility of the user of this standard to establish appro- 5. Apparatus
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 5.1 Alumina Ceramic or Platinum Crucible or Dish, suit-
able for holding sample (subsequently called sample holder).
2. Referenced Documents 5.2 Analytical Balance, capable of weighing to 60.0002 g.
2.1 ASTM Standards: 2 5.3 Muffle Furnace, capable of reaching 950°C (1742°F)
C 562 Test Method for Moisture in a Graphite Sample with controller capable of maintaining a temperature of 950° 6
20°C (1742 6 68°F).
3. Significance and Use 5.4 Platinum or Stainless Steel Wire.
3.1 This test method provides a practical estimate of non- 5.5 Desiccator, charged with indicating desiccant.
burnable residues in commercially available graphite materials. 5.6 Drying Oven, air convection type, capable of being
The ash values determined by this test method are of use in controlled to 110 6 2°C (230 6 4°F).
comparing the relative purity of various grades of graphite. To
6. Sampling
facilitate use, this test method institutes simplifications that
preclude the ability to determine absolutely the ash values of 6.1 Samples may be solid or particulate. Solid bodies may
the test graphite material due to uncontrolled sources of trace be sampled by removing one or more solid pieces from the
contamination. body by, for example, sawing, turning, milling, or fracturing.
3.2 This test method is not intended for use in determining Particulate samples may be generated from solid bodies by
the ash content of purified graphites, for example, nuclear drilling, using a carbide drill to minimize contamination, or by
materials. The relationship between the mineral content of a other crushing and grinding methods.
graphite sample and the ash content of that sample is unknown
7. Procedure
and is not determined by the application of this test method.
7.1 Dry the sample in accordance with Test Method C 562,
4. Interferences or for a minimum of 16 h in a drying oven at 110 6 2°C (230
4.1 Although permitted within the scope of this test method, 6 4°F), and allow the sample to cool to room temperature in
the use of alumina ceramic crucibles may affect results due to the desiccator.
difficulties in obtaining repeatable or proper weights, or both, 7.2 Tare a dried sample holder using an analytical balance to
because of (1) the hygroscopic nature of some ceramic 60.002 g. As soon as the sample has cooled to room
temperature, remove it from the desiccator and weigh a 25- to
50-g sample into the tared sample holder. Reweigh the sample
1
This test method is under the jurisdiction of ASTM Committee D02 on and sample holder to 60.002 g.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 7.3 Introduce a slow stream of air into the muffle furnace
D02.F0 on Manufactured Carbon and Graphite Products.
Current edition approved June 1, 2005. Published August 2005. Originally
(Note 1). Place the sample holder containing the sample into
approved in 1965. Last previous edition approved in 2000 as C 561–91(2000). the furnace, then heat the furnace so that the sample reaches
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 500°C (932°F) in 1 h and 750°C (1382°F) in 2 h.
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on NOTE 1—The stream of air into the furnace should be carefully adjusted
the ASTM website. so that the sample or ash will not be blown from the dish. The air stream
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
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C 561 – 91 (2005)
may be admitted by leaving the door of the furnace open a slight amount. 9.1.2 Results obtained from at least two ash determinations
Exercise care when placing a sample into a warm furnace so that no and their averages.
sample material will be lost due to drafts.
7.4 To aid in oxidation, stir the sample periodically with the 10. Precision and Bias 3
wire. The absence of black flecks indicates that ashing is 10.1 The precision of this test method was determined
complete; at that time raise the furnace temperature to 950°C during a round-robin test among four laboratories testing
(1742°F) for 1 h. samples split from a common sample which was ground to pass
7.5 Remove the dish containing the ash from the furnace, a No. 60 (250-µm) sieve. This sampling method was used for
(see Note 1) and cool to room temperature in the desiccator. the round-robin to minimize variations among samples pro-
Following removal from the desiccator, weigh the dish with the vided to participating laboratories.
ash as rapidly as possible. 10.2 On this sample the mean, standard deviation between
7.6 Replace the sample in the furnace at 950°C (1742°F) for laboratories and standard deviation within laboratories were,
30 min and repeat the procedure prescribed in 7.5 until a respectively:
constant weight is obtained to 60.002 g. Mean 0.7286
Between laboratories 0.0159
8. Calculation Within laboratories 0.0127
8.1 Calculate the percentage of ash as follows: 10.3 No bias was noted during this round-robin test; how-
Ash, % 5 [~ C 2 A!/~B 2 A!# 3 100 (1) ever, the method is empirical and there is no suitable reference
material that can be used to determine the bias of this test
where: method.
A = weight of the sample holder,
B = weight of the sample holder and dried sample, 11. Keywords
C = weight of the sample holder and ash. 11.1 ash; carbon; graphite
9. Report
9.1 The report shall include the following: 3
Supporting data have been filed at ASTM International Headquarters and may
9.1.1 Proper identification of the sample, and be obtained by requesting Research Report RR:C05-1008.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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2
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An American National Standard

Designation: C 561 – 91 (Reapproved 2005)

Standard Test Method for

1. Scope crucibles, and (2) the possible chemical combination of trace

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