ASTM C1365-2006(2011) Standard Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis《用X射线.pdf
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1、Designation: C1365 06 (Reapproved 2011)Standard Test Method forDetermination of the Proportion of Phases in PortlandCement and Portland-Cement Clinker Using X-Ray PowderDiffraction Analysis1This standard is issued under the fixed designation C1365; the number immediately following the designation in
2、dicates the year oforiginal adoption or, in 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. Scope*1.1 This test method covers direct determin
3、ation of theproportion by mass of individual phases in portland cement orportland-cement clinker using quantitative X-ray (QXRD)analysis. The following phases are covered by this standard:alite (tricalcium silicate), belite (dicalcium silicate), aluminate(tricalcium aluminate), ferrite (tetracalcium
4、 aluminoferrite),periclase (magnesium oxide), gypsum (calcium sulfate dihy-drate), bassanite (calcium sulfate hemihydrate), anhydrite (cal-cium sulfate), and calcite (calcium carbonate).1.2 This test method specifies certain general aspects of theanalytical procedure, but does not specify detailed a
5、spects.Recommended procedures are described, but not specified.Regardless of the procedure selected, the user shall demon-strate by analysis of certified reference materials (CRMs) thatthe particular analytical procedure selected for this purposequalifies (that is, provides acceptable precision and
6、bias) (seeNote 1). The recommended procedures are ones used in theround-robin analyses to determine the precision levels of thistest method.NOTE 1Asimilar approach was used in the performance requirementsfor alternative methods for chemical analysis in Test Methods C114.1.3 The values stated in SI u
7、nits shall be regarded as thestandard.1.4 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 li
8、mitations prior to use. For specifichazards, see Section 9.2. Referenced Documents2.1 ASTM Standards:2C114 Test Methods for Chemical Analysis of HydraulicCementC150 Specification for Portland CementC183 Practice for Sampling and the Amount of Testing ofHydraulic CementC219 Terminology Relating to Hy
9、draulic CementC670 Practice for Preparing Precision and Bias Statementsfor Test Methods for Construction MaterialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Tes
10、t Method3. Terminology3.1 Definitions are in accordance with Terminology C219.3.2 Phases (1):33.2.1 alite, ntricalcium silicate (C3S)4modified in com-position and crystal structure by incorporation of foreign ions;occurs typically between 30 to 70 % (by mass) of the portland-cement clinker; and is n
11、ormally either the M1or M3crystalpolymorph, each of which is monoclinic.3.2.2 alkali sulfates, narcanite (K2SO4) may accommo-date Na+, Ca2+, and CO3in solid solution, aphthitalite (K4-x,Nax)SO4with x usually 1 but up to 3), calcium langbeinite(K2Ca2SO43) may occur in clinkers high in K2O, andthenard
12、ite (Na2SO4) in clinkers with high Na/K ratios (1).1This test method is under the jurisdiction of ASTM Committee C01 on Cementand is the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.Current edition approved Dec. 1, 2011. Published May 2012. Originallyapproved in 1998. Last p
13、revious edition approved in 2006 as C1365 - 98 (2006).DOI: 10.1520/C1365-06R11.2For 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 o
14、nthe ASTM website.3The boldface numbers in parentheses refer to the list of references at the end ofthis standard.4When expressing chemical formulae,C=CaO,S=SiO2,A=Al2O3,F=Fe2O3,M = MgO, S =SO3,andH=H2O.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International,
15、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.3 aluminate, ntricalcium aluminate (C3A) modified incomposition and sometimes in crystal structure by incorpora-tion of a substantial proportion of foreign ions; occurs as 2 to15 % (by mass) of the portland-cemen
16、t clinker; is normallycubic when relatively pure and orthorhombic or monoclinicwhen in solid solution with significant amounts of sodium (2).3.2.4 anhydrite, ncalcium sulfate CS! and is orthorhom-bic (see Note 2).NOTE 2Calcium sulfate is added to the clinker during grinding tocontrol setting time, s
17、trength development, and volume stability. Severalphases may form as a result of dehydration of gypsum. The first 1.5molecules of water are lost between 0 and 65 C with minor changes instructure; and, above 95 C, the remaining 0.5 molecules of water are losttransforming the structure to the metastab
18、le g polymorph of anhydrite(sometimes referred to as soluble anhydrite) and subsequently theorthorhombic form (3).3.2.5 bassanite, ncalcium sulfate hemihydrate CSH1/2!and is monoclinic.3.2.6 belite, ndicalcium silicate (C2S) modified in com-position and crystal structure by incorporation of foreign
19、ions;occurs typically as 15 to 45 % (by mass) of the portland-cement clinker as normally the b polymorph, which is mono-clinic. In lesser amounts, other polymorphs can be present.3.2.7 calcite, ncalcium carbonate is trigonal and may bepresent in a cement as an addition or from carbonation of freelim
20、e.3.2.8 ferrite, ntetracalcium aluminoferrite solid solutionof approximate composition C2(A,F) modified in compositionby variation in the Al/Fe ratio and by substantial incorporationof foreign ions as C4AXF2-Xwhere0x1.4; constituting 5to 15 % (by mass) of a portland-cement clinker; and isorthorhombi
21、c.3.2.9 free lime, nfree calcium oxide (C); cubic (see Note3).NOTE 3Free lime (CaO) may be present in clinker and cement butreadily hydrates to form portlandite (Ca(OH)2). Portlandite may carbonateto form calcium carbonate, generally as calcite. Heat-treating a freshly-ground sample to 600 C is usef
22、ul to convert any portlandite back to freelime but will also dehydrate the hydrous calcium sulfate phases (gypsumand bassanite) to anhydrite.3.2.10 gypsum, ncalcium sulfate dihydrate CSH2! and ismonoclinic .3.2.11 periclase, nfree magnesium oxide (M); cubic.3.3 Definitions of Terms Specific to This
23、Standard:3.3.1 Certified Reference Material (CRM), na materialwhose properties (in this case phase abundance, XRD peakposition or intensity, or both) are known and certified (see Note4).NOTE 4NIST Standard Reference Material (SRMt) Clinkers 2686,2687, and 2688 are suitable CRMs for qualification.53.
24、3.2 diffractometer, nthe instrument, an X-ray powderdiffractometer, for determining the X-ray diffraction pattern ofa crystalline powder.3.3.3 phase, na homogeneous, physically distinct, andmechanically separable portion of a material, identifiable by itschemical composition and crystal structure.3.
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