1、Designation: C1365 06 (Reapproved 2011)C1365 18Standard 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 design
2、ation indicates 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*Scope1.1 This test method covers di
3、rect determination of the proportion 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), ferri
4、te (tetracalcium aluminoferrite), periclase(magnesium oxide), gypsum (calcium sulfate dihydrate), bassanite (calcium sulfate hemihydrate), anhydrite (calcium sulfate), andcalcite (calcium carbonate).1.2 This test method specifies certain general aspects of the analytical procedure, but does not spec
5、ify detailed aspects.Recommended procedures are described, but not specified. Regardless of the procedure selected, the user shall demonstrate byanalysis of certified reference materials (CRMs) that the particular analytical procedure selected for this purpose qualifies (thatis, provides acceptable
6、precision and bias) (see Note 1). The recommended procedures are ones used in the round-robin analysesto determine the precision levels of this test method.NOTE 1A similar approach was used in the performance requirements for alternative methods for chemical analysis in Test Methods C114.1.3 The val
7、ues stated in SI units shall be regarded as the standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices a
8、nd determine theapplicability of regulatory limitations prior to use. For specific hazards, see Section 9.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of Internat
9、ional Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2C114 Test Methods for Chemical Analysis of Hydraulic CementC150C150/C150M Specification for Portland CementC183C183/C183M Practice
10、for Sampling and the Amount of Testing of Hydraulic CementC219 Terminology Relating to Hydraulic CementC670 Practice for Preparing Precision and Bias Statements for Test Methods for Construction MaterialsE29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specificati
11、onsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions: Definitions are in accordance with Terminology C219.3.2 Phases (1):31 This test method is under the jurisdiction of ASTM Committee C01 on Cement and is the direct respon
12、sibility of Subcommittee C01.23 on Compositional Analysis.Current edition approved Dec. 1, 2011March 1, 2018. Published May 2012April 2018. Originally approved in 1998. Last previous edition approved in 20062011 asC1365 - 98 (2006).C1365 06 (2011). DOI: 10.1520/C1365-06R11.10.1520/C1365-18.2 For ref
13、erencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The boldface numbers in parentheses refer to the list of references
14、at the end of this standard.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends
15、that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, Wes
16、t Conshohocken, PA 19428-2959. United States13.2.1 alite, ntricalcium silicate (C3S)4 modified in composition and crystal structure by incorporation of foreign ions; occurstypically between 30 to 70 % (by mass) of the portland-cement clinker; and is normally either the M1 or M3 crystal polymorph,eac
17、h of which is monoclinic.3.2.2 alkali sulfates, narcanite (K2SO4) may accommodate Na+, Ca2+, and CO3 in solid solution, aphthitalite (K4-x,Nax)SO4with x usually 1 but up to 3), calcium langbeinite (K2Ca2SO43) may occur in clinkers high in K2O, and thenardite (Na2SO4) inclinkers with high Na/K ratios
18、 (1).3.2.3 aluminate, ntricalcium aluminate (C3A) modified in composition and sometimes in crystal structure by incorporation ofa substantial proportion of foreign ions; occurs as 2 to 15 % (by mass) of the portland-cement clinker; is normally cubic whenrelatively pure and orthorhombic or monoclinic
19、 when in solid solution with significant amounts of sodium (2).3.2.4 anhydrite, ncalcium sulfate CS! and is orthorhombic (see Note 2).NOTE 2Calcium sulfate is added to the clinker during grinding to control setting time, strength development, and volume stability. Several phasesmay form as a result
20、of dehydration of gypsum. The first 1.5 molecules of water are lost between 0 and 65 C 65C with minor changes in structure;and, above 95 C, 95C, the remaining 0.5 molecules of water are lost transforming the structure to the metastable polymorph of anhydrite (sometimesreferred to as soluble anhydrit
21、e) and subsequently the orthorhombic form (3).3.2.5 bassanite, ncalcium sulfate hemihydrate CSH1/2! and is monoclinic.3.2.6 belite, ndicalcium silicate (C2S) modified in composition and crystal structure by incorporation of foreign ions; occurstypically as 15 to 45 % (by mass) of the portland-cement
22、 clinker as normally the polymorph, which is monoclinic. In lesseramounts, other polymorphs can be present.3.2.7 calcite, ncalcium carbonate is trigonal and may be present in a cement as an addition or from carbonation of free lime.3.2.8 ferrite, ntetracalcium aluminoferrite solid solution of approx
23、imate composition C2(A,F) modified in composition byvariation in theAl/Fe ratio and by substantial incorporation of foreign ions as C4AXF2-X where 0 x 1.4; constituting 5 to 15 %(by mass) of a portland-cement clinker; and is orthorhombic.3.2.9 free lime, nfree calcium oxide (C); cubic (see Note 3).N
24、OTE 3Free lime (CaO) may be present in clinker and cement but readily hydrates to form portlandite (Ca(OH)2). Portlandite may carbonate to formcalcium carbonate, generally as calcite. Heat-treating a freshly-ground sample to 600 C 600C is useful to convert any portlandite back to free lime butwill a
25、lso dehydrate the hydrous calcium sulfate phases (gypsum and bassanite) to anhydrite.3.2.10 gypsum, ncalcium sulfate dihydrate CSH2! and is monoclinic .3.2.11 periclase, nfree magnesium oxide (M); cubic.3.3 Definitions of Terms Specific to This Standard:3.3.1 Certified Reference Material (CRM), na m
26、aterial whose properties (in this case phase abundance, XRD peak positionor intensity, or both) are known and certified (see Note 4).NOTE 4NIST Standard Reference Material (SRM) Clinkers 2686, 2687, and 2688 are suitable CRMs for qualification.53.3.2 diffractometer, nthe instrument, an X-ray powder
27、diffractometer, for determining the X-ray diffraction pattern of acrystalline powder.3.3.3 phase, na homogeneous, physically distinct, and mechanically separable portion of a material, identifiable by itschemical composition and crystal structure.3.3.3.1 DiscussionPhases in portland-cement clinker a
28、nd cements that are included in this test method are four major phases (alite, belite, aluminate,and ferrite) and one minor phase (periclase).3.3.3.2 DiscussionPrecision values are provided for additional phases (gypsum, bassanite, anhydrite, arcanite, and calcite). Values for theseconstituents may
29、be provided using this method but are considered informational until suitable certified reference materials forqualification are available.3.3.4 qualification, nprocess by which a QXRD procedure is shown to be valid.3.3.5 Rietveld analysis, nprocess of refining crystallographic and instrument variab
30、les to minimize differences betweenobserved and calculated X-ray powder diffraction patterns for one or more phases, estimating their relative abundance.4 When expressing chemical formulae, C = CaO, S = SiO2, A = Al2O3, F = Fe2O3, M = MgO, S = SO3, and H = H2O.5 Portland cement clinker SRMs from the
31、 Standard Reference Material Program, National Institute of Standards and Technology.C1365 1823.3.6 standardization, nprocess of determining the relationship between XRD intensity and phase proportion for one or morephases (see Note 5).NOTE 5In the literature of X-ray powder diffraction analysis, th
32、e standardization process has been commonly referred to as calibration; however, wehave determined that standardization is a more accurate term.3.3.6.1 DiscussionRietveld analysis uses crystal structure models to calculate powder diffraction patterns of phases that serve as the referencepatterns. Th
33、e pattern-fitting step seeks the best-fit combination of selected pattern intensities to the raw data. The relative patternintensities along with the crystallographic attributes of each phase are used to calculate relative abundance. The standardizationapproach uses powdered samples of pure phases t
34、o assess the relationship between diffraction intensity ratios and mass fractionratios of two or more constituents; and is referred to here as the traditional method.3.3.7 X-ray diffraction (XRD), nthe process by which X-rays are coherently scattered by electrons in a crystalline material.4. Backgro
35、und4.1 This test method assumes general knowledge concerning the composition of cement and portland-cement clinker. Necessarybackground information may be obtained from a number of references (1, 4).4.2 This test method also assumes general expertise in XRD and QXRD analysis. Important background in
36、formation may beobtained from a number of references (5-10).5. Summary5.1 This test method covers direct determination of the proportion by mass of individual phases in cement or portland-cementclinker using quantitative X-ray powder diffraction analysis. The following phases are covered by this sta
37、ndard: alite (tricalciumsilicate, C3S), belite (dicalcium silicate, C2S), aluminate (tricalcium aluminate, C3A), ferrite (tetracalcium aluminoferrite, C4AF),periclase (magnesium oxide, M), arcanite (potassium sulfate, KS), gypsum (calcium sulfate dihydrate, CSH2), bassanite (calciumsulfate hemihydra
38、te, CSH12), anhydrite (calcium sulfate, CS), and calcite (calcium carbonate, CaCO3).A QXRD test procedure includes some or all of the following: (a) specimen preparation; (b) data collection and phaseidentification; (c) standardization (for the standardization approach); (d) collecting a set of crys
39、tal structure models for refinement(for the Rietveld approach); (e) use of an internal or external standard (to correct for various effects on intensity besides phaseproportion); (f) analysis of the sample (in which the powder diffraction pattern is measured and/or the intensity of selected XRDpeaks
40、 or patterns are measured); and (g) calculation of the proportion of each phase.5.2 This test method does not specify details of the QXRD test procedure. The user must demonstrate by analysis of certifiedreference materials that the particular analytical procedure selected for this purpose provides
41、acceptable levels of precision andbias. Two recommended procedures (the Rietveld approach and the traditional approach used to determine the acceptable levelsof precision and bias) are given in Appendix X1X2 and Appendix X2X3.6. Significance and Use6.1 This test method allows direct determination of
42、 the proportion of some individual phases in cement or portland-cementclinker. Thus it provides an alternative to the indirect estimation of phase proportion using the equations in SpecificationC150C150/C150M (Annex A1).6.2 This test method assumes that the operator is qualified to operate an X-ray
43、diffractometer and to interpret X-ray diffractionspectra.6.3 This test method may be used as part of a quality control program in cement manufacturing.6.4 This test method may be used in predicting properties and performance of hydrated cement and concrete that are a functionof phase composition.6.5
44、 QXRD provides a bulk analysis (that is, the weighted average composition of several grams of material). Therefore, resultsmay not agree precisely with results of microscopical methods.7. Apparatus7.1 X-Ray DiffractometerThe X-ray diffractometer allows measurement of the X-ray diffraction pattern fr
45、om which thecrystalline phases within the sample may be qualitatively identified and the proportion of each phase may be quantitativelydetermined. X-ray diffractometers are manufactured commercially and a number of instruments are available. The suitability ofthe diffractometer for this test method
46、shall be established using the qualification procedure outlined in this test method.C1365 1838. Materials8.1 Standardization PhasesThe use of standardization phases is recommended for establishing the intensity ratio/mass ratiorelationships when using the traditional quantitative method. These phase
47、s must usually be synthesized (11, 12).8.2 CRM ClinkerThe use of three CRM clinkers is required to qualify the QXRD procedure.8.3 Internal StandardThe use of an internal standard is recommended for the standardization approach. Suitable materialsinclude chemical reagents (see 8.4) or CRMs (see Appen
48、dix X1X2).8.4 Reagent ChemicalsReagent grade chemicals, if used either as an internal standard or during chemical extraction of certainphases, shall meet the specifications of the Committee on Analytical Reagents of the American Chemical Society where suchspecifications are available.6 Other grades
49、may be used, provided it is first ascertained that the chemical is sufficiently pure topermit its use without lessening the accuracy of the determination.9. Hazards9.1 The importance of careful and safe operation of an X-ray diffractometer cannot be overemphasized. X-rays are particularlyhazardous. An X-ray diffractometer must be operated safely to avoid serious injury or death. The X-rays are generated by highvoltages, perhaps as high as 55 kV peak, requiring care to avoid serious electric shock. Klug and Alexander (6
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