C24-09 (Reapproved 2013) PDF

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Designation: C24 − 09 (Reapproved 2013)

Standard Test Method for


Pyrometric Cone Equivalent (PCE) of Fireclay and High
Alumina Refractory Materials1
This standard is issued under the fixed designation C24; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope 3. Terminology
1.1 This test method covers the determination of the Pyro- 3.1 Definitions—For definitions of terms used in this test
metric Cone Equivalent (PCE) of fire clay, fireclay brick, high method, see Terminology C71.
alumina brick, and silica fire clay refractory mortar by com-
parison of test cones with standard pyrometric cones under the 4. Summary of Test Method
conditions prescribed in this test method. 4.1 This test method consists of preparing a test cone from
1.2 Units—The values stated in inch-pound units are to be a refractory material and comparing its deformation end point
regarded as standard. The values given in parentheses are to that of a standard pyrometric cone. The resultant PCE value
mathematical conversions to SI units that are provided for is a measure of the refractoriness of the material.
information only and are not considered standard. 4.2 Temperature equivalent tables for the standard cones
1.2.1 Exceptions—Certain weights are in SI units with have been determined by the National Institute of Standards
inch-pound in parenthesis. Also, certain figures have SI units and Technology when subjected to both slow and rapid heating
without parenthesis. These SI units are to be regarded as rates.
standard.
1.3 This standard does not purport to address all of the 5. Significance and Use
safety concerns, if any, associated with its use. It is the 5.1 The deformation and end point of a cone corresponds to
responsibility of the user of this standard to establish appro- a certain heat-work condition due to the effects of time,
priate safety and health practices and determine the applica- temperature, and atmosphere.
bility of regulatory limitations prior to use. 5.2 The precision of this test method is subject to many
variables that are difficult to control. Therefore, an experienced
2. Referenced Documents operator may be necessary where PCE values are being utilized
2.1 ASTM Standards:2 for specification purposes.
C71 Terminology Relating to Refractories 5.3 PCE values are used to classify fireclay and high
E11 Specification for Woven Wire Test Sieve Cloth and Test alumina refractories.
Sieves
E220 Test Method for Calibration of Thermocouples By 5.4 This is an effective method of identifying fireclay
Comparison Techniques variations, mining control, and developing raw material speci-
E691 Practice for Conducting an Interlaboratory Study to fications.
Determine the Precision of a Test Method 5.5 Although not recommended, this test method is some-
times applied to materials other than fireclay and high alumina.
Such practice should be limited to in-house laboratories and
1
never be used for specification purposes.
This test method is under the jurisdiction of ASTM Committee C08 on
Refractories and is the direct responsibility of Subcommittee C08.02 on Thermal
Properties. 6. Procedure
Current edition approved Sept. 1, 2013. Published September 2013. Originally
approved in 1919. Last previous edition approved in 2009 as C24 – 09. DOI: 6.1 Preparation of Sample:
10.1520/C0024-09R13.
2
6.1.1 Clay or Brick—Crush the entire sample of fire clay or
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
fireclay brick, in case the amount is small, by means of rolls or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on a jaw crusher to produce a particle size not larger than 1⁄4 in. (6
the ASTM website. mm). If the amount is large, treat a representative sample

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

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C24 − 09 (2013)
obtained by approved methods. Then mix the sample thor-
oughly and reduce the amount to about 250 g (0.5 lb) by
quartering (see Note 1). Then grind this portion in an agate,
porcelain, or hard steel mortar and reduce the amount again by
quartering. The final size of the sample shall be 50 g and the
fineness capable of passing an ASTM No. 70 (212-µm) sieve3
(equivalent to a 65-mesh Tyler Standard Series). In order to
avoid excessive reduction to fines, remove them frequently
during the process of reduction by throwing the sample on the
sieve and continuing the grinding of the coarser particles until
all the sample passes through the sieve (see Note 2). Take
precautions to prevent contamination of the sample by steel
particles from the sampling equipment during crushing or
grinding.
NOTE 1—Take care during the crushing and grinding of the sample to
prevent the introduction of magnetic material.
NOTE 2—The requirement to grind the coarser particles is particularly
important for highly siliceous products; excessively fine grinding may
reduce their PCE by as much as two cones.
6.1.2 Silica Fire Clay (see 3.1)—In the case of silica fire
clay, test the sample obtained by approved methods as received
without grinding or other treatment.
6.2 Preparation of Test Cones:
NOTE 1—Dimensions are in inches.
6.2.1 After preparing samples of unfired clays (Note 3), or
SI Equivalents
of mixes containing appreciable proportions of raw clay, in
in. mm
accordance with 6.1.1, heat them in an oxidizing atmosphere in
the temperature range from 1700 to 1800°F (925 to 980°C) for 0.075 1.90
not less than 30 min. 0.272 6.91
0.281 7.14
NOTE 3—Some unfired clays bloat when they are formed into cones and 1.081 27.46
are carried through the high-temperature heat treatment prescribed in 5.4.1 1.125 28.58
without preliminary calcining. The substances that cause bloating can, in
most cases, be expelled by heating the clay samples before testing. FIG. 1 Standard Pyrometric Test Cone
6.2.2 The clay sample may be given the heat treatment
prescribed in 6.2.1 after it has been formed into a cone (see
6.2.3), but this procedure has been found not as effective as the the test cones with the PCE cones in so far as is practical (see
treatment of the powdered material. If cones so prepared bloat Note 5). The plaque may be any convenient size and shape and
during the PCE test, heat a portion of the original sample in its may be biscuited before using, if desired.
powdered condition as prescribed in 6.2.1 and then retest it. NOTE 4—A satisfactory cone plaque mix consists of 85 % fused
6.2.3 Thoroughly mix the dried sample, and after the alumina and 15 % plastic refractory clay. For tests that will not go above
addition of sufficient dextrine, glue, gum tragacanth, or other Cone 34, the plastic refractory clay may be increased to 25 % and the
alkali-free organic binder and water, form it in a metal mold alumina may be replaced with brick grog containing over 70 % alumina.
into test cones in the shape of a truncated trigonal pyramid with The alumina or grog should be ground to pass an ASTM No. 60 (250-µm)
sieve (equivalent to a 60-mesh Tyler Standard Series), and the PCE of the
its base at a small angle to the trigonal axis, and in accordance refractory plastic clay should be not lower than Cone 32.
with dimensions shown in Fig. 1. In forming the test cone use NOTE 5—The number of cones and their mounting facing inward as
the mold shown in Fig. 2. shown in Fig. 3 is typical for gas-fired furnaces of relatively large
dimensions and gases moving at high velocity. The practical bore of the
6.3 Mounting: muffle tubes in most electric furnaces does not permit cone pats of this
6.3.1 Mount both the test cones and the Standard Pyromet- size. The static atmosphere prevailing permits the cones being mounted to
ric Cones on plaques of refractory material that have a face outward, if so desired.
composition that will not affect the fusibility of the cones (see 6.4 Heating:
Note 4). Mount both test and PCE cones with the base 6.4.1 Perform the heating in a suitable furnace, operating
embedded so that the length of the sloping face of the cone with an oxidizing atmosphere, at rates to conform to the
above the plaque shall be 15⁄16 in. (24 mm) and the face of the following requirements (see Note 6 and Note 7). It is advisable,
cone (about which bending takes place) shall be inclined at an but not mandatory that the furnace temperature be controlled
angle of 82° with the horizontal. Arrange the test cones with with a calibrated4 thermocouple or radiation pyrometer con-
respect to the PCE cones as shown in Fig. 3, that is, alternate nected to a program-controlled recorder.

3 4
Detailed requirements for this sieve are given in Specification E11. Test Method E220 specifies calibration procedures for thermocouples.

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C24 − 09 (2013)
TABLE 1 Heating Rates Up to Cone 26
Cold Test Furnace Time inter- Cumulative
to Cone No. val, min Time, h:min

12 45 0:45
13 5 0:50
14 19 1:09
15 13 1:22
16 24 1:46
17 9 1:55
18 4 1:59
19 8 2:07
20 9 2:16
23 16 2:32
26 7 2:39

6.4.1.1 For PCE tests expected to have an end point of PCE


Cone 12 or above, but not exceeding Cone 26, heat at the rate
prescribed in Table 1.
6.4.1.2 For PCE tests expected to have an end point above
Cone 26, heat at the rate prescribed in Table 2.
NOTE 6—The heating rate through the cone series in both Table 1 and
2 is at 270°F (150°C)/h.
NOTE 7—Following a test run, the cone pat may be removed at 1830°F
(1000°C) and a new pat may be put in without cooling the furnace to
below red heat. The time interval to bring the furnace, using Table 1, up
to Cone 12 shall be not less than 20 min, and using Table 2, the time
interval up to Cone 20 shall be not less than 25 min.
6.4.2 The furnace atmosphere shall contain a minimum of
Table of Dimensions 0.5 % oxygen with 0 % combustibles. Make provisions to
in. mm in. mm prevent any external forces from being exerted on the cones or
cone plaque, such as from flames or gases. Test the furnace at
A 0.50 12.7 K 2.500 63.50 intervals to determine the uniformity of the distribution of the
B 0.75 19.0 L 2.75 69.8
C 2.510 63.75 M 1.00 25.4 heat.
D 1.084 27.53 N 0.12 3.0
E 1.015 25.78 O 0.62 15.7
6.5 Pyrometric Cone Equivalent:
F 0.229 5.82 P 0.75 19.0 6.5.1 The softening of the cone will be indicated by the top
G 0.75 19.0 Q 0.75 19.0 bending over and the tip touching the plaque. Always report the
H 0.460 11.68 R 1.50 38.1
I 0.399 10.13 S 0.75 19.0 bloating, squatting, or unequal fusion of small constituent
J 0.75 19.0 T 2.62 66.5 particles. Report the Pyrometric Cone Equivalent (PCE) in
terms of Standard Pyrometric Cones and the cone that most
FIG. 2 Split Mold for ASTM Pyrometric Test Cone nearly corresponds in time of softening with the test cone. If
the test cone softens later than one Standard Pyrometric Cone
but earlier than the next Standard Pyrometric Cone and
approximately midway between, report the PCE as Cone
33–34.
6.5.2 If the test cone starts bending at an early cone but is
not down until a later cone, report this fact.
6.5.3 The temperatures corresponding to the end points of
the Standard Pyrometric Cones are frequently of interest and
are shown in Appendix X1.

7. Precision and Bias


7.1 Precision—No justifiable statement of precision is pos-
sible since the results of the tests are descriptive and do not
produce a precise numeric value.
7.2 Bias—No justifiable statement on bias is possible since
FIG. 3 Method of Mounting Test Cones and Appearance After
Testing
the true physical property values of refractories cannot be
established by any acceptable reference material.

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TABLE 2 Heating Rates Above Cone 26 8. Keywords
Cold Test Furnace Time Inter- Cumulative
to Cone No. val, min Time, h:min
8.1 PCE; pyrometric cone; pyrometric cone equivalent;
refractories
20 45 0:45
23 16 1:01
26 7 1:08
27 7 1:15
28 3 1:18
29 5 1:23
30 3 1:26
31 7 1:33
311⁄2 6 1:39
32 7 1:46
321⁄2 3 1:49
33 7 1:56
34 9 2:05
35 9 2:14
36 7 2:21
37 7 2:28

APPENDIX

(Nonmandatory Information)

X1. TEMPERATURES CORRESPONDING TO STANDARD PYROMETRIC CONE END POINTS

X1.1 The approximate temperature equivalents correspond- X1.2 Heating Rate:


ing to the end points of those Standard Pyrometric Cones that X1.2.1 Cones 12 to 37, inclusive—270°F (150°C)/h.
are used in connection with refractory testing are as shown in
Table X1.1. X1.2.2 Cone 38—(100°C)/h.
X1.2.3 Cones 39 to 42, inclusive—1080°F (600°C)/h.
TABLE X1.1 Temperature Equivalents for Pyrometric Cones Used X1.3 Standard Pyrometric Cones 28 and 30 are manufac-
in Refractory Testing tured but are not used in the PCE test.
Cone No. End Point, °F (°C) Cone No. End Point, °F (°C)
X1.4 Temperatures for Cones 12 to 37 were reported at the
12 2439 (1337) 31 3061 (1683) National Institute of Standards and Technology.5Temperatures
13 2460 (1349) 311⁄2 3090 (1699) for Cones 38 to 42 were determined by C. O. Fairchild and M.
14 2548 (1398) 32 3123 (1717)
15 2606 (1430) 321⁄2 3135 (1724)
F. Peters.6 These temperatures apply satisfactorily for all the
16 2716 (1491) 33 3169 (1743) conditions of this test method, but do not apply to the
17 2754 (1512) 34 3205 (1763) conditions of commercial firing of kilns and use of refractory
18 2772 (1522) 35 3245 (1785)
19 2806 (1541) 36 3279 (1804)
materials.
20 2847 (1564) 37 3308 (1820)
23 2921 (1605) 38 3335 (1835) X1.5 Temperature values were determined in degrees Cel-
26 2950 (1621) 39 3389 (1865) sius; Fahrenheit temperature values were calculated.
27 2984 (1640) 40 3425 (1885)
28 2995 (1646) 41 3578 (1970) 5
29 3018 (1659) 42 3659 (2015) Beerman, H. P.,Journal of the American Ceramic Society, Vol. 39, No. 2H,
30 3029 (1665) 1956, pp. 47–53.
6
Fairchild, C. O., and Peters, M. F., “Characteristics of Pyrometric Cones,”
Journal of the American Ceramic Society, Vol. 9, No. 11, November 1976, p. 700.

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C24 − 09 (2013)
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