Designation: C 914 – 95 (Reapproved 2004)
Standard Test Method for
Bulk Density and Volume of Solid Refractories by Wax
Immersion1
This standard is issued under the fixed designation C 914; 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.
1. Scope should be heated to only slightly above the melting point to
1.1 This test method covers the basic procedure for deter- avoid flashing of the wax vapors and to permit quickly forming
mining bulk density and volume of refractory shapes. This test a uniform surface coating of wax.
is applicable to all refractory shapes or monoliths, burned or NOTE 2—Caution: Vapors given off by molten wax ignite spontane-
unburned, independent of composition or forming method, ously at above 400°F (205°C) and should not be allowed to come in
including materials that slake and hydrate. It is particularly contact with the heating element or open flame.
suitable for determining bulk density and volume of complex 3.3 Balance, capable of determining the weights of the
shapes after forming, since results may be obtained in a matter specimens to four significant figures. Thus, specimens weigh-
of minutes. ing from 100 to 999 g should be weighed to one decimal place,
1.2 This standard does not purport to address all of the those from 10 to 99 g should be weighed to two decimal places,
safety concerns, if any, associated with its use. It is the and so forth.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 4. Sampling
bility of regulatory limitations prior to use. For a specific 4.1 At least five representative specimens should be chosen
hazard statement, see Note 2. of the refractory to be characterized. These may be whole
shapes or broken pieces, depending on the purpose of the test.
2. Significance and Use
2.1 This test method may be used to quickly determine 5. Procedure
volume and bulk density of a refractory of any shape, provided 5.1 Preparation of Specimens—The test specimens shall be
it has sufficient structural integrity to permit handling. Thus it dried to a constant weight by heating to 220 to 230°F (105 to
may be used on unfired or fired, strong or friable shapes. 110°C) to remove entrapped moisture, which would affect the
2.2 Since the test may be performed quickly, it has found bulk density determination. This drying process may be omit-
application as manufacturing in-process control as well as in ted when specimens are known to be dry or when it is desired
characterizing finished refractory products. Also it may be used to make density determinations on moisture-containing speci-
to examine specimens after other test or service exposure. mens, such as brick shapes, immediately after forming.
5.2 Initial Weight,W—Determine the initial weight, W, of
3. Apparatus
each test specimen in grams to four significant figures.
3.1 Paraffın Wax, fully refined, that has a known constant 5.3 Coating the Test Specimen:
density, K, that does not change after repeated melting and 5.3.1 Coat the specimen with wax by dipping the specimen
cooling cycles. into the container of melted wax. The coating is easily applied
NOTE 1—The paraffin waxes generally used are commercially available by holding one end of the specimen and immersing one half to
and have density values in the range 0.87 to 0.91 g/cm3. Also, these waxes two thirds of it. Then, hold the waxed end, and immerse the
melt at approximately 135°F (57°C). unwaxed portion plus a small overlap into the wax to provide
3.2 Wax-Melting Container, used to melt the wax but should a complete coating.
not allow the wax to overheat. A container heated by hot water, 5.3.2 Take care not to entrap air bubbles under the wax. If
preferably thermostatically controlled, is satisfactory. The wax found, press these bubbles out so the wax conforms exactly to
the surface of the specimen. Close holes in the wax coating by
additional dipping in wax so the surface can be completely
1
This test method is under the jurisdiction of ASTM Committee C08 on sealed.
Refractories and is the direct responsibility of Subcommittee C08.03 on Physical 5.4 Wax-Coated Weight,P—Determine the weight of the
Tests and Properties.
Current edition approved Sept. 1, 2004. Published October 2004. Originally wax-coated specimen, P, in grams to four significant figures.
approved in 1979. Last previous edition approved in 1999 as C 914 – 95 (1999). 5.5 Suspended Weight, S:
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
C 914 – 95 (2004)
TABLE 1 Volume Measurement
Precision
Standard Deviation
Material Average Within Laboratories, Sr Between Laboratories, SL Repeatability Interval, Ir Reproducibility Interval, IR
A 397.17 0.695 0.377 1.965 1.066
B 408.51 0.592 0.245 1.674 0.693
C 408.82 0.859 0.307 2.429 0.868
D 410.56 0.801 0.370 2.265 1.046
E 411.80 0.885 0.494 2.503 1.397
Grand Average 407.37 0.766 0.359 2.167 2.933
Relative Precision
Coefficient of Variance
Material Average Within Laboratories, Between Laboratories, Relative Repeatability Relative Reproducibility
% Vr % VL Interval, % Ir Interval, % IR
A 397.17 0.175 0.095 0.495 0.269
B 408.51 0.145 0.060 0.410 0.170
C 408.82 0.210 0.075 0.594 0.212
D 410.56 0.195 0.090 0.552 0.255
E 411.80 0.215 0.120 0.608 0.339
Grand Average 407.37 0.188 0.088 0.532 0.249
5.5.1 Determine the weight of the wax-coated specimen 7. Report
suspended in water, S, in grams to four significant figures. 7.1 For each property, report the average of the values
5.5.2 Previously counterbalance the balance with the wire obtained with at least five specimens, and preferably, the
or other device used to suspend the specimen in place, and individual values as well.
immerse in water to the same depth as used when the refractory 7.2 Report the bulk density results to two decimal places.
specimen is in place. This weighing may be accomplished by
suspending the specimen in a loop or halter of AWG Gage 22 8. Precision and Bias
(0.643-mm) copper wire hung from one arm of the balance.
8.1 Volume Measurement:
8.1.1 Interlaboratory Test Program—Interlaboratory study
6. Calculation
was conducted by five laboratories using three replications and
6.1 Volume, V: two duplicate runs on the same specimen. The specimen was
6.1.1 Obtain the volume, V 1, of the test specimens (includ- 21⁄2 in. (63.5 mm) series 9 in. (229 mm) straights of oxynitride
ing the wax) in cubic centimetres as follows: bonded silicon carbide cut into quarter bricks approximately
V1 5 P 2 S (1) 4.5 by 2.25 by 1.5 in. (114 by 57 by 38 mm).
8.1.2 Precision:
3
NOTE 3—This assumes that 1 cm of water weighs 1 g. This is true 8.1.2.1 Repeatability— Two test results, each composed of
within 3 parts in 1000 for water at room temperature.
five specimens from one laboratory, should be considered
6.1.2 Obtain the volume, V 2, of the wax coating on the test significantly different at the 95 % confidence level, if their
specimen in cubic centimetres as follows: difference exceeds the Repeatability Interval, Ir, for the grand
V2 5 ~P – W!/K (2)
average in Table 1.
8.1.2.2 Reproducibility— Two test results, each composed
where: of five specimens from two laboratories, should be considered
K = density of the wax, g/cm3. significantly different at the 95 % confidence level, if their
6.1.3 Obtain the volume, V, of the test specimen by sub- difference exceeds the Reproducibility Interval, IR, for the
tracting the volume of the wax coating from the total volume grand average in Table 1.
as calculated in 6.1.1 as follows: 8.1.3 Bias—No justifiable statement can be made since
V 5 V 1 2 V2 (3) there is no accepted reference material and the true values of
volume cannot be established by an accepted reference
6.2 Bulk Density,B—The bulk density, B, of a specimen in method.
grams per cubic centimetre is the quotient of its initial weight 8.2 Bulk Density Measurement:
divided by volume of the test specimen, excluding the volume 8.2.1 Interlaboratory Test Program—Interlaboratory study
of wax. Calculate B as follows: was conducted by five laboratories using three replications and
B 5 W/V (4) two duplicate runs on the same specimen. The specimen was
2
C 914 – 95 (2004)
TABLE 2 Bulk Density Measurement
Precision
Standard Deviation
Material Average Within Laboratories, Between Laboratories, Repeatability Reproducibility
Sr SL Interval, Ir Interval, IR
A 2.585 0.0033 0.0066 0.0094 0.0210
B 2.569 0.0033 0.0026 0.0094 0.0120
C 2.619 0.0041 0.0009 0.0115 0.0120
D 2.622 0.0033 0.0020 0.0094 0.0110
E 2.599 0.0024 0.0024 0.0067 0.0094
Grand Average 2.599 0.0033 0.0029 0.0093 0.0131
Relative Precision
Coefficient of Variance
Material Average Within Laboratories, Between Laboratories, Relative Repeatability Relative Reproducibility
% Vr % VL Interval, % Ir Interval, % IR
A 2.585 0.129 0.257 0.36 0.81
B 2.569 0.130 0.103 0.37 0.47
C 2.619 0.156 0.033 0.44 0.45
D 2.622 0.127 0.077 0.36 0.42
E 2.599 0.091 0.091 0.26 0.36
Grand Average 2.599 0.127 0.112 0.36 0.50
21⁄2 in. (63.5 mm) series 9 in. (229 mm) straights of oxynitride significantly different at the 95 % confidence level, if their
bonded silicon carbide cut into quarter bricks approximately difference exceeds the Reproducilibity Interval, IR, for the
4.5 by 2.25 by 1.5 in. (114 by 57 by 38 mm). grand average in Table 2.
8.2.2 Precision: 8.2.3 Bias—No justifiable statement can be made since
8.2.2.1 Repeatability— Two test results, each composed of there is no accepted reference material and the true values of
five specimens from one laboratory, should be considered bulk density cannot be established by an accepted reference
significantly different at the 95 % confidence level, if their method.
difference exceeds the Repeatability Interval, Ir, for the grand
average in Table 2. 9. Keywords
8.2.2.2 Reproducibility— Two test results, each composed 9.1 bulk density; refractory shapes; solid refractories; vol-
of five specimens from two laboratories, should be considered ume; wax immersion
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