Astm C1039

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An American National Standard

Designation: C1039 – 85 (Reapproved 2005)

Standard Test Methods for


Apparent Porosity, Apparent Specific Gravity, and Bulk
Density of Graphite Electrodes1
This standard is issued under the fixed designation C1039; 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 4.3.1 The pressure vessel shall be provided with an opentop


1.1 These test methods cover the determination of apparent container to hold the specimens and a means of introducing
porosity, apparent specific gravity, and bulk density of cores water around the specimens while specimens are being held at
taken from graphite electrodes manufactured for use in electric low pressure.
arc furnaces. (See also C559 and C838.) 4.4 Vacuum Pump.
1.2 This standard does not purport to address the safety 4.5 Wire Loop, Halter or Stirrup, fabricated with 22 AWG
concerns, if any, associated with its use. It is the responsibility (9.643 mm) copper wire shall be provided for determining
of the user of this standard to establish appropriate safety and suspended weight.
health practices and determine the applicability of regulatory 4.6 Smooth Linen or Cotton Cloth.
limitations prior to use. 5. Test Specimens and Sampling
2. Referenced Documents 5.1 Electrodes can be sampled using Practice C783 that
2.1 ASTM Standards:2 result in a specimen with approximately 50 mm (2 in.)
C559 Test Method for Bulk Density by Physical Measure- diameter and 191 mm (71⁄2 in.) long or a specimen of
ments of Manufactured Carbon and Graphite Articles equivalent volume.
C783 Practice for Core Sampling of Graphite Electrodes 5.2 If sizes and shapes which are different from those
C838 Test Method for Bulk Density of As-Manufactured described in 5.1, these shall be included in the report.
Carbon and Graphite Shapes 5.3 For each test, select at least five electrodes, at random,
to represent a lot. The lot size will be determined by agreement
3. Significance and Use of the parties desiring the tests.
3.1 The results of these test methods can be used as a quality
6. Calibration
control or quality assurance check of electrodes either during
their manufacture or at the user’s location. The results of these 6.1 Prior to obtaining the suspended weights of the speci-
methods tend to be operator-sensitive, therefore, care must be mens, the balance shall be adjusted to zero with the wire stirrup
taken in the execution of the test in order to obtain reproducible suspended from the balance and immersed into a container of
results. the liquid to the same depth in the liquid as occurs when a
specimen is in place.
4. Apparatus
7. Procedure
4.1 Drying Oven.
4.2 Analytical Balance, capable of weighing to 0.1 g. 7.1 Determinations of Dry Weight, D:
4.3 Autoclave or Pressure Vessel, capable of withstanding 7.1.1 Dry the test specimens to constant weight by heating
one atmosphere externally and designed to withstand at least to 100 to 110°C (212 to 230°F). Cool and determine the dry
448 to 483 kPa (65 to 70 psi) internal pressure. weight, D, in grams to the nearest 0.1 g. If the time between
drying and weighing exceeds 8 h, the specimens must be stored
in a desiccator.
1
These test methods are under the jurisdiction of ASTM Committee D02 on 7.1.2 The determination of dry weight may be done either
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.F0 on Manufactured Carbon and Graphite Products.
before or after the saturation operation. If the specimen is
Current edition approved June 1, 2005. Published August 2005. Originally friable or there is evidence that particles have broken loose
approved in 1985. Last previous edition approved in 2000 as C1039–85(2000). DOI: during the saturation operation, the dry weight shall be
10.1520/C1039-85R05. obtained after the suspended and saturated weights have been
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM determined. Drying as described in 7.1.1 must be carried out.
Standards volume information, refer to the standard’s Document Summary page on 7.2 Saturation:
the ASTM website.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
C1039 – 85 (2005)
7.2.1 Using the pressure vessel described in 4.3, place the 8.3 Volume of Impervious Portion—Obtain the volume of
specimens in the open-top container inside the vessel. Close impervious portion by subtracting the suspended weight, S,
and seal the vessel and pump down at least to 133 Pa (1 mm from the dry weight, D.
Hg) and maintain this pressure for 30 min. Volume of impervious portion, cm3 5 D 2 S (3)
7.2.2 Slowly introduce water (preferably distilled water)
until the specimens are covered with at least 40 mm (1.5 in.) of 8.4 Apparent Porosity, P—The apparent porosity, P, is
water. Continue to pump for an additional 5 min. expressed as a percentage of the volume of open pores to the
exterior volume, and may be calculated as follows:
NOTE 1—Sufficient water must be provided above the specimens to
supply enough water to fill the open pores of the specimens during P, % 5 [~ W 2 D!/V# 3 100 5 [~ W 2 D!/~W 2 S!#3 100 (4)
pressurization. If after pressurization, one or more specimens are exposed 8.5 Bulk Density, B—The bulk density of a specimen, B, in
to air above the water, these specimens must be dried and process repeated grams per cubic centimetre, is its mass per unit volume,
(7.1.1).
including pores. Calculate as follows:
7.2.3 After the evacuation process is completed, close the
B, g/cm3 5 D/V 5 D/~W 2 S! (5)
vacuum line and introduce air pressure. Pressurize to 207 6 7
kPa (30 6 1 psi) gage pressure and hold for 4 h. Following this If bulk density in pounds per cubic foot is desired, multiply
period of time return the vessel to atmospheric pressure. by 62.4.
7.3 Determination of Suspended Weight, S: 8.6 Apparent Specific Gravity, T—Calculate the apparent
7.3.1 Within 1 h of the time the vessel returns to atmo- specific gravity, T, of that portion of the specimen which is
spheric pressure, the suspended weights and saturated weights impervious to water under these test conditions as follows:
must be obtained. T 5 D/~D 2 S! (6)
7.3.2 Place the container used in the vacuum-pressure
vessel near the immersion container to facilitate rapid transfer 9. Report
to the weighing stirrup (see 4.5). 9.1 Report sizes of specimens tested.
7.3.3 Obtain the suspended weight, S, to the nearest 0.1 g, of 9.2 Report the values of all properties for individual speci-
each specimen. The specimens can be transferred through air mens and the averages.
but the transfer must be made quickly. Following the weighing, 9.3 Calculate apparent porosity values to one decimal place.
each specimen should be returned to a separate container of 9.4 Calculate bulk density and apparent specific gravity
water or the saturated weight, W, should be obtained immedi- values to two decimal places.
ately according to 7.4.
7.4 Determination of Saturated Weight, W: 10. Precision and Bias
7.4.1 After determining the suspended weight, blot each
10.1 Interlaboratory Tests—An interlaboratory study using
specimen lightly with a moistened smooth linen or cotton cloth
the vacuum-pressure method, was conducted among six labo-
to remove all drops of water from the surface and weigh in air,
ratories who tested three specimens of each of three graphite
to the nearest 0.1 g, to obtain the saturated weight, W. The cloth
materials representing a range of apparent porosities and bulk
must be prepared by previously saturating it with water and
densities. The three materials were chosen from premium
then pressing only enough to remove the water which would
grade electrodes, regular grade electrodes, and connecting
drip from the cloth. Avoid excessive blotting or rubbing which
nipples.
will remove water from the pores of the specimen.
10.2 Precision—Tables 1-3 show the applicable data for
8. Calculation precision in terms of percent apparent porosity (Table 1),
grams per cubic centimetre of bulk density (Table 2) and
8.1 Exterior Volume—Obtain the exterior volume by sub-
apparent specific gravity (Table 3).
tracting the suspended weight from the saturated weight.
10.3 Bias—A bias statement is not possible because no
V, cm3 5 W 2 S (1) standard reference materials are available.
where: 11. Keywords
V = exterior volume, cm3,
W = saturated weight, g, and 11.1 bulk; carbon; density; electrodes; graphite; physical;
S = suspended weight, g. porosity; specific gravity
NOTE 2—This assumes that one cubic centimetre of water weighs 1 g.
This is true within about 3 parts in 1000 for water at 20 to 25°C (68 to TABLE 1 Precision of Apparent Porosity, Percent
77°F). Standard Deviations
8.2 Volume of Open Pores—Obtain the volume of open Material Average Within Labs Between Labs
pores by subtracting the dry weight, D, from the saturated 1 23.1 0.70 0.71
weight, W. 2 18.6 1.21 0.91
3 13.1 1.37 0.33
Volume of open pores, cm3 5 W 2 D (2)

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C1039 – 85 (2005)
TABLE 2 Precision of Bulk Density, Grams per Cubic
Centimetre
Standard Deviations
Material Average Within Labs Between Labs
1 1.61 0.011 0.005
2 1.70 0.018 0.010
3 1.81 0.025 0.014

TABLE 3 Precision of Apparent Specific Gravity


Standard Deviations
Material Average Within Labs Between Labs
1 2.10 0.008 0.018
2 2.09 0.019 0.026
3 2.09 0.011 0.018

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