1、Designation: C1099 07 (Reapproved 2012)Standard Test Method forModulus of Rupture of Carbon-Containing RefractoryMaterials at Elevated Temperatures1This standard is issued under the fixed designation C1099; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the modu-lus of rupture of carbon-con
3、taining refractories at elevatedtemperatures in air.1.2 The values stated in inch-pound units and degreesFahrenheit are to be regarded as standard. The values given inparentheses are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with
4、 its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 5.2. Referenced Documents2.1 ASTM Standards:2C583 Test Method for M
5、odulus of Rupture of RefractoryMaterials at Elevated TemperaturesE220 Test Method for Calibration of Thermocouples ByComparison Techniques2.2 ISO Standard:ISO Recommendation 5013 Determination of the HotModulus of Rupture of Shaped and Unshaped Dense andInsulating Refractory Products33. Significance
6、 and Use3.1 The modulus of rupture of carbon-containing refracto-ries at elevated temperatures has become accepted as a usefulmeasurement in quality control testing and in research anddevelopment. These measurements are also used to determinethe suitability of particular products for various applica
7、tionsand to develop specifications. The sample may undergo someoxidation during the test.3.2 In 1988, ruggedness testing was conducted on this testprocedure. The following variables were studied:3.2.1 Testing temperature (2525 (1385) versus 2575F(1413C),3.2.2 Air atmosphere versus argon atmosphere i
8、n thefurnace,3.2.3 Hold time prior to breaking the sample (12 versus 18min), and3.2.4 Loading rate on the sample (175 (778) versus 350lb/min (1556 N/min).3.3 Resin bonded magnesia-carbon brick containing ap-proximately 17 % carbon after coking where tested in twoseparate ruggedness tests. Metal-free
9、 brick were tested in thefirst ruggedness test, while aluminum-containing brick weretested in the second. Results were analyzed at a 95 % confi-dence level.3.4 For the metal-free brick, the presence of an argonatmosphere and hold time had statistically significant effects onthe modulus of rupture at
10、 2550F (1400C). The argon atmo-sphere yielded a lower modulus of rupture. The samples testedin air had a well-sintered decarburized zone on the exteriorsurfaces, possibly explaining the higher moduli of rupture. Thelonger hold time caused a lower result for the metal-free brick.3.5 For the aluminum-
11、containing brick, testing temperature,the presence of an argon atmosphere, and loading rate hadstatistically significant effects on the modulus of rupture at2550F (1400C). The higher testing temperature increased themeasured result, the presence of an argon atmosphere loweredthe result, and the high
12、er loading rate increased the result.4. Apparatus4.1 Electrically-Heated FurnaceAn electrically heatedfurnace should be used. The furnace will contain an airatmosphere.4.2 Lower Bearing Edges, at least one pair, made fromvolume-stable refractory material (Note 1) shall be installed inthe furnace on
13、5-in. (127-mm) centers.4.3 Thrust Column, containing the top bearing edge that ismade from the same volume-stable refractory material used for1This test method is under the jurisdiction of ASTM Committee C08 onRefractories and is the direct responsibility of Subcommittee C08.01 on Strength.Current e
14、dition approved Oct. 1, 2012. Published November 2012. Originallyapproved in 1992. Previous edition approved in 2007 as C1099 07. DOI:10.1520/C1099-07R12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS
15、tandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohoc
16、ken, PA 19428-2959. United States1the lower bearing edges, shall extend outside the furnace wheremeans are provided for applying a load.4.3.1 The lower bearing edges and the bearing end of thesupport column shall have rounded bearing surfaces havingabout a14-in. (6 mm) radius (Note 2). The lower bea
17、ringsurfaces may be made adjustable, but must attain the standardspan of 5 6332 in. (1276 2 mm). The length of the lowerbearing surfaces shall exceed the specimen width by about14in. The load shall be applied to the upper bearing edge by anysuitable means. Instrumentation for measuring the load shal
18、l beaccurate to 1 %.4.3.2 The thrust column shall be maintained in verticalalignment and all bearing surfaces shall be parallel in bothhorizontal directions.NOTE 1A minimum of 90 % alumina content is recommended as asuitable refractory.NOTE 2All bearing surfaces should be checked periodically tomain
19、tain a round surface.4.4 It is recommended that the furnace temperature becontrolled with calibrated platinum-rhodium/platinum thermo-couples connected to a program-controller recorder (seeMethod E220). A thermocouple protection tube is advisable.Temperature differential within the furnace shall not
20、 be morethan 620F (11C), but the controlling thermocouple shall beplaced within12 in. (13 mm) of the geometric center of a sideface of the test specimen when positioned on the bearing edges.5. Hazards5.1 Standard safety precautions that are used in high tem-perature testing should be followed for th
21、is test method. Thiswould include use of protective clothing and eyeglasses whenhandling hot samples. In addition, these tests should be run inan area that has adequate ventilation since there is potential foroxidation of carbon to form carbon monoxide. There may alsobe organic volatiles present fro
22、m pyrolysis of pitch and resin.6. Sampling6.1 The sample shall consist of five specimens, each takenfrom five brick or shapes.7. Test Specimens7.1 The standard test specimen shall be 1 6132 by 1 6132by approximately 6 in. (25 6 0.8 by 25 6 0.8 by approxi-mately 152 mm). Specimens cut from brick shal
23、l have at leastone original brick surface perpendicular to the pressed direc-tion. This original brick surface will be the surface in tensionduring testing. If cut from shapes, the specimens shall be takenparallel to the longest dimension. For irregular shapes, all fourlong surfaces of the specimen
24、may be cut faces. Note this in thereport.7.2 The test specimens shall be prepared from brick as theyare to be used. They shall not be coked prior to testing.7.3 Opposite faces of the specimen shall be parallel, andadjacent faces shall be perpendicular.7.4 Measure the width and depth of the test spec
25、imen atmidspan to the nearest 0.01 in. (0.3 mm).8. Procedure8.1 Preheat the furnace to the test temperature and allow itto soak until thermal equilibrium is established.8.2 Specify the test temperature as 2550 6 10F (1400 66C). Note any deviation from 2550F in the report.8.3 Once thermal equilibrium
26、 is established, open the fur-nace door, place one specimen on the lower bearing edgeskeeping the original brick surface as the tension surface, andclose the door as quickly as possible.8.4 Hold the sample for 15 min 6 30 s. Bring the topbearing edge to bear at mid-span on the specimen, ensureproper
27、 alignment of the bearing surfaces, and apply pressurethrough the loading mechanism until failure of the specimenoccurs. The rate of application of the load on the sample shallbe 175 6 17.5 lbf (778.8 N)/min. The resulting rate of increasein bending stress for the standard 1 by 1 by 6 in. (25 by 25
28、by152 mm) specimen is 1312.5 6 131 psi (9.05 6 0.9 MPa)/min.48.5 Since opening the furnace door as the specimen isinserted will lower the temperature of the furnace, note theamount of temperature loss, as well as the time it takes for thefurnace to reestablish its equilibrium temperature.8.6 Once th
29、e sample has been broken, open the furnacedoor, remove the broken sample from the lower bearing edges,and place another sample on the lower bearing edges for testingin an identical manner.9. Calculation9.1 Calculate the modulus of rupture (MOR) for eachrectangular specimen as follows:MOR 5 3PL/2bd2w
30、here:MOR = modulus of rupture, psi or MPa,P = concentrated load at rupture, lbf or N,L = span between supports, in. or mm,b = breadth or width of specimen, in. or mm, andd = depth of specimen, in. or mm.10. Report10.1 Report the following information:10.1.1 The test temperature,10.1.2 The five indiv
31、idual test results,10.1.3 The average modulus of rupture and standard devia-tion in pounds-force per square inch (or megapascals) for thefive specimens, and10.1.4 List of deviations.11. Precision and Bias511.1 PrecisionInterlaboratory Study: An interlaboratorytest program between four laboratories w
32、as completed in 1989.4This rate is 0.151 MPa/s, which is in agreement with the stress rate in ISORecommendation 5013.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting RR:CO8-1010.C1099 07 (2012)2Each laboratory received five brick measuring 9 by 4.5
33、 by 3 in.for each of four different materials. The four materials were:tar-bonded magnesia brick containing about 5 % residualcarbon with no metallic additives; resin-bonded magnesite-carbon brick containing about 20 % residual carbon and nometallic additives; resin-bonded magnesite-carbon brick con
34、-taining about 20 % residual carbon and an addition of poweredaluminum; and resin-bonded magnesite-carbon brick contain-ing about 10 % residual carbon and no metallic additives.11.2 RepeatabilityThe maximum permissible differencedue to test error between two test results obtained by oneoperator on t
35、he same material is given by the repeatabilityinterval and the relative repeatability interval (coefficient ofvariation). The 95 % repeatability intervals are given in Table1. Two test results that do not differ by more than therepeatability interval will be considered to be from the samepopulation,
36、 and, conversely, two test results that do differ bymore than the repeatability interval will be considered to befrom different populations.11.3 ReproducibilityThe maximum permissible differencedue to test error between two test results obtained by twooperators in different laboratories on the same
37、type of materialusing the same type of test equipment is given by thereproducibility interval and relative reproducibility interval(coefficient of variation). The 95 % reproducibility intervalsare given in Table 1. Two test results that do not differ by morethan the reproducibility interval will be
38、considered to be fromthe same population and, conversely, two test results that dodiffer by more than the reproducibility interval will be consid-ered to be from different populations.11.4 BiasThis test method does not lend itself to astatement of bias.12. Keywords12.1 carbon-containing; modulus of
39、rupture; refractories;strengthASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof in
40、fringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this stan
41、dard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your v
42、iews known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contac
43、ting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).TABLE 1 Relative PrecisionMaterialNumb
44、erAverageX, psiStandardWithin,Sr, psiDeviationBetween,SR, psiRepeat-abilityIntervalr, psiReproduc-ibilityIntervalR, psiCoefficient of VariationRelativeRepeat-ability, r ,%RelativeReproduc-ibility, R,%WithinLab,Vr,%BetweenLabs,VR,%1 343 60.4 63.8 169 179 17.6 18.6 49.3 52.22 522 33.8 46.3 94.6 130 6.48 8.87 18.1 24.93 1400 122 109 341 341 8.71 7.79 24.4 24.44 390 81.9 81.9 229 229 21.0 21.0 58.7 58.7C1099 07 (2012)3
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