ASTM C1069-1986(2004)e1 Standard Test Method for Specific Surface Area of Alumina or Quartz by Nitrogen Adsorption《用氮吸附法测定氧化铝和石英表面特性的试验方法》.pdf

1、Designation: C 1069 86 (Reapproved 2004)e1Standard Test Method forSpecific Surface Area of Alumina or Quartz by NitrogenAdsorption1This standard is issued under the fixed designation C 1069; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re

2、vision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEThe address in footnote 3 was changed in May 2004.1. Scope1.1 This test method covers the determination

3、 of the specificsurface area of aluminas and silicas used in the manufacture ofceramics. The test method is a general one, permitting the useof any modern commercial nitrogen adsorption apparatus butstrictly defining the outgassing procedure. Calculations arebased on the Brunauer-Emmett-Teller (BET)

4、 equation.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with 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.2. Re

5、ferenced Documents2.1 ASTM Standards:2E 173 Practice for Conducting Interlaboratory Studies ofMethods for Chemical Analysis of Metals3. Summary3.1 An appropriate size sample is degassed for1hat423Kbefore proceeding with the analysis as prescribed by themanufacturer of the instrument used. The sample

6、 is accuratelyweighed after analysis.3.2 Calculations are based on the BET equations, adaptedwhere necessary for the equipment being used. The cross-sectional area of the nitrogen molecule is taken as 0.162 nm2.4. Significance and Use4.1 Both sellers and purchasers of alumina and quartz willfind the

7、 test method useful to determine the specific surfacearea and indirectly as a measure of the particle size for materialspecifications, manufacturing control, and research and devel-opment.5. Apparatus5.1 Specific Surface Area Analyzer, recently (after 1970)manufactured commercial equipment employing

8、 low-temperature (77 K) nitrogen adsorption. This test method maybe dynamic or static.5.2 Degassing Equipment, suitable to the instrument used.5.3 Analytical Balance, having a sensitivity of 1.0 mg.6. Reagents and Materials6.1 Liquid Nitrogen.6.2 Cylinder of compressed nitrogen gas, high purity assp

9、ecified by manufacturer, with pressure regulator.6.3 Cylinder of compressed helium gas, high purity asspecified by manufacturer, with pressure regulator, for staticinstruments or for dynamic instruments having gas mixingability and employing the multipoint procedure or,6.4 Cylinder of compressed, ap

10、proximately 0.30 mol frac-tion, nitrogen in helium with pressure regulator, for otherdynamic instruments employing the single point procedure.7. Procedure7.1 Sample PreparationBlend the gross sample very well.For non-free-flowing materials mechanical agitation is neces-sary (for example, V-type blen

11、der with intensifier). If samplesplitting of free-flowing materials is necessary, use a spinningriffler.37.2 Sample Degassing7.2.1 Sample size is related to the equipment being used andshall conform to the equipment manufacturers recommenda-tions for highest precision.7.2.2 The degassing technique (

12、for example, vacuum, no-vacuum) shall conform to the equipment manufacturers rec-ommendations.7.2.3 The degassing temperature shall be1hat423K.7.2.4 Samples must be analyzed immediately after degas-sing.1This test method is under the jurisdiction of ASTM Committee C21 on CeramicWhitewares and Relate

13、d Prodcuts and is the direct responsibility of SubcommitteeC21.04 on Raw Materials.Current edition approved April 1, 2004. Published May 2004. Originallyapproved in 1986. Last previous edition approved in 1997 as C 1069 86 (1997)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org

14、, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Spinning rifflers manufactured by Quantachrome Corp., 1900 Corporate Drive,Boynton Beach, FL 33426 or by Gilson Company, Inc., P

15、.O. Box 200, Lewis Center,OH 43035-0200, which has been found suitable for this purpose.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 AnalysisThe analysis procedure recommended by themanufacturer as their most precise shall be

16、followed.8. Calculations8.1 The procedure recommended by the manufacturer asbeing the most complete shall be followed.9. Report9.1 Report the following information:9.1.1 ResultsIn units of m2/g.9.1.2 Specific surface area as the average of two determi-nations, each made on separately degassed sample

17、s. If theresults do not agree within 5 % the procedure should bereviewed, the equipment checked, and the test repeated a thirdtime.9.1.3 From a practical standpoint it is recommended that thefollowing guidelines be used in reporting data:9.1.3.1 From 1 to 99 m2/gno more than two significantfigures.9

18、.1.3.2 From 100 to 200 m2/gto the nearest 1 m2/g.9.1.3.3 From 200 m2/g and aboveto the nearest 5 m2/g.10. Precision and Bias10.1 PrecisionSix laboratories cooperated in a testingprogram involving various materials having specific surfaceareas ranging from 1 to 200 m2/g. The determinations weremade i

19、n duplicate on separate samples and days. Practice E 173was used to obtain the analyses of variance in Table 1.10.2 BiasNo absolute method for surface area determina-tions is recognized and, therefore, it is not possible to discussbias of results obtained.11. Keywords11.1 alumina; nitrogen adsorptio

20、n; particle size; quartzASTM 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 infringe

21、ment 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 standard o

22、r 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 views k

23、nown 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 contacting A

24、STM 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).TABLE 1 Analyses of VarianceSurfaceArea,m2/gARepeatabilityInterval,R1,m2/gReproducibilityInterval,R2,m2/g1.1 0.05 0.191.3 0.12 0.268.4 0.40 2.079.3 0.44 0.8625 0.63 5.2101 4.8 11.0205 8.2 33.2AAverages from round-robin study.C 1069 86 (2004)e12