ASTM D5604-1996(2006) Standard Test Methods for Precipitated Silica-Surface Area by Single Point B E T Nitrogen Adsorption《沉淀二氧化硅的标准试验方法 用单点B E T 氮的吸附法沉淀的硅表面积》.pdf
《ASTM D5604-1996(2006) Standard Test Methods for Precipitated Silica-Surface Area by Single Point B E T Nitrogen Adsorption《沉淀二氧化硅的标准试验方法 用单点B E T 氮的吸附法沉淀的硅表面积》.pdf》由会员分享,可在线阅读,更多相关《ASTM D5604-1996(2006) Standard Test Methods for Precipitated Silica-Surface Area by Single Point B E T Nitrogen Adsorption《沉淀二氧化硅的标准试验方法 用单点B E T 氮的吸附法沉淀的硅表面积》.pdf(5页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 5604 96 (Reapproved 2006)Standard Test Methods forPrecipitated SilicaSurface Area by Single Point B.E.T.Nitrogen Adsorption1This standard is issued under the fixed designation D 5604; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se of revision, 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.1. Scope1.1 These test methods cover a procedure to measure thesurface area of precipitated hydrated
3、silicas by, a single pointapproximation of the Brunauer, Emmett, and Teller (B.E.T.)2theory of multilayer gas adsorption. These test methods specifythe sample preparation and treatment, instrument calibrations,required accuracy and precision of experimental data, andcalculations of the surface area
4、results from the obtained data.1.2 These test methods are used to determine the singlepoint nitrogen surface areas in the range of 10 to 50 hm2kg (10to 500 m2/g).1.3 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.4 This standard
5、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. The minimumsafety equipment shou
6、ld include protective gloves, sturdy eyeand face protection.2. Referenced Documents2.1 ASTM Standards:3D 1799 Practice for Carbon BlackSampling PackagedShipmentsD 1900 Practice for Carbon BlackSampling Bulk Ship-mentsD 1993 Test Method for Precipitated Silica-SurfaceArea byMultipoint BET Nitrogen Ad
7、sorption3. Summary of Test Methods3.1 Solids adsorb nitrogen and, under specific conditions,the adsorbed molecules approach a monomolecular layer. Thequantity of gas in this hypothetical monomolecular layer iscalculated using an approximation of the B.E.T. equation.Combining this with the area occup
8、ied by the nitrogen mol-ecule yields an approximation of the total surface area of thesolid.3.2 These test methods measure the estimated quantity ofnitrogen in the monomolecular layer formed by adsorption atliquid nitrogen temperature and at a fractional saturationpressure of 0.30 6 0.01.3.3 Before
9、a surface area determination can be made it isnecessary that any material which may already be adsorbed onthe surface of the silica be removed. Removal of adsorbedforeign material (by heating under vacuum or in a steam ofnon-adsorbing gas) eliminates two potential errors. The firsterror is due to th
10、e mass of the foreign material. The seconderror is due to interference by the foreign material to access bynitrogen the silica surface.4. Significance and Use4.1 These test methods measure the approximate surfacearea of precipitated hydrated silicas that is available to thenitrogen molecule using an
11、 approximation of the B.E.T.method. While the multi-point version of the B.E.T. method isgenerally accepted as being less prone to errors arising fromthe varying surface properties of individual samples, thesingle-point approximation is often adequate due to the shortertime per test and relative sim
12、plicity of the instrumentationneeded. Quality control applications and comparative tests onnear-identical samples of close chemical and micro-structuralcomposition are likely to be the applications of greatest value.5. ASTM D11 Standard Reference Silicas5.1 None RequiredThis test method is used to d
13、eterminesurface area of candidate silicas. Reference silicas are avail-able4for determining agreement with data obtained in theinterlaboratory test used for multi-point procedure Test MethodD 1993.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct respon
14、sibility of Subcommittee D11.20 on CompoundingMaterials and Procedures.Current edition approved Oct. 1, 2006. Published November 2006. Originallyapproved in 1994. Last previous edition approved in 2001 as D 5604 96 (2001).2Brunauer, Emmett, and Teller, Journal of the American Chemical Society,Vol60,
15、 1938, p. 309.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.4The sole source of supply of precipitated samp
16、les known to the committee atthis time is Forcoven Products, P.O. Box 1556, Humble, TX 77338. (Samples areavailable in three surface areas: A138; B.57; and C.168 X103m2/kg.) If you areaware of alternative suppliers, please provide this information to ASTM Interna-tional Headquarters. Your comments w
17、ill receive careful consideration at a meetingof the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.TEST METHOD A SURFACE AREA BYSTATIC VOLUMETRIC APPARATUS6. Apparatus6.1 Static
18、-Volumetric Gas Adsorption Apparatus, withdewar flasks and all other accessories required for operation.6.2 Oven, vacuum-type, capable of temperature-regulationto 65C at 110C. Pressure should be less than 13.5 Pa (0.1mmHg).6.3 Sample Cells, which, when attached to the adsorptionapparatus, will maint
19、ain isolation of the sample from theatmospheric pressure equivalent to a helium leak rate of#105standard cubic centimeters per minute, per atmosphere ofpressure difference.6.4 McCleod Gage, or equivalent means to measure thepressure. (May be part of the adsorption apparatus.)6.5 Pressure Gage or Tra
20、nsducer, known to be accurate to60.25 % of reading or 60.067 kPa (60.5 mmHg), whicheveris greater and covering the 0 to 101.3 kPa (760 mmHg)pressure range. (May be part of the adsorption apparatus.)6.6 Analytical Balance, with 0.1 mg sensitivity.6.7 Glass Vials, small (30 cm3) glass vials with caps
21、foroven drying samples.6.8 Heating Mantle, or equivalent, capable of maintaining atemperature of 160 6 5C.6.9 Volumetric Calibration Apparatus, with valve or stop-cock and 6.4 mm tubing adapter to gas adsorption sampleconnector. See Fig. 1.7. Reagents7.1 Purity of ReagentsReagent grade chemicals sha
22、ll beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused, provided it is established that they are
23、 of sufficiently highpurity to use without lessening the accuracy of the determina-tion.7.2 Purity of WaterUnless otherwise indicated, referencesto water (and ice prepared from it) shall be understood to meandistilled water or water of equal purity.7.3 Liquid Nitrogen, 98 % or higher purity.7.4 Ultr
24、a-High Purity Nitrogen Gas, cylinder, or othersource of prepurified nitrogen gas.7.5 Ultra-High Purity Helium Gas, cylinder, or other sourceof prepurified helium gas.8. Sampling8.1 No separate practice for sampling silicas is available.However, samples may be taken in accordance with PracticesD 1799
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