Standard Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis

SIGNIFICANCE AND USE
6.1 This test method allows direct determination of the proportion of some individual phases in cement or portland-cement clinker. Thus it provides an alternative to the indirect estimation of phase proportion using the equations in Specification C150/C150M (Annex A1).  
6.2 This test method assumes that the operator is qualified to operate an X-ray diffractometer and to interpret X-ray diffraction spectra.  
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 function of phase composition.  
6.5 QXRD provides a bulk analysis (that is, the weighted average composition of several grams of material). Therefore, results may not agree precisely with results of microscopical methods.
SCOPE
1.1 This test method covers direct determination of the proportion by mass of individual phases in portland cement or portland-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 aluminoferrite), periclase (magnesium oxide), gypsum (calcium sulfate dihydrate), bassanite (calcium sulfate hemihydrate), anhydrite (calcium sulfate), and calcite (calcium carbonate).  
1.2 This test method specifies certain general aspects of the analytical procedure, but does not specify detailed aspects. Recommended procedures are described, but not specified. Regardless of the procedure selected, the user shall demonstrate by analysis of certified reference materials (CRM's) that the particular analytical procedure selected for this purpose qualifies (that is, provides acceptable precision and bias) (see Note 1). The recommended procedures are ones used in the round-robin analyses to determine the precision levels of this test method.  
Note 1: A similar approach was used in the performance requirements for alternative methods for chemical analysis in Test Methods C114.  
1.3 The values 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 responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability 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 standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

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ASTM C1365-18 - Standard Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C1365 − 18
Standard Test Method for
Determination of the Proportion of Phases in Portland
Cement and Portland-Cement Clinker Using X-Ray Powder
1
Diffraction Analysis
This standard is issued under the fixed designation C1365; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers direct determination of the
proportion by mass of individual phases in portland cement or
2. Referenced Documents
portland-cement clinker using quantitative X-ray (QXRD)
2
2.1 ASTM Standards:
analysis. The following phases are covered by this standard:
C114 Test Methods for Chemical Analysis of Hydraulic
alite (tricalcium silicate), belite (dicalcium silicate), aluminate
Cement
(tricalcium aluminate), ferrite (tetracalcium aluminoferrite),
C150/C150M Specification for Portland Cement
periclase (magnesium oxide), gypsum (calcium sulfate
C183/C183M Practice for Sampling and the Amount of
dihydrate), bassanite (calcium sulfate hemihydrate), anhydrite
Testing of Hydraulic Cement
(calcium sulfate), and calcite (calcium carbonate).
C219 Terminology Relating to Hydraulic Cement
1.2 This test method specifies certain general aspects of the
C670 Practice for Preparing Precision and Bias Statements
analytical procedure, but does not specify detailed aspects.
for Test Methods for Construction Materials
Recommended procedures are described, but not specified.
E29 Practice for Using Significant Digits in Test Data to
Regardless of the procedure selected, the user shall demon-
Determine Conformance with Specifications
strate by analysis of certified reference materials (CRM’s) that
E691 Practice for Conducting an Interlaboratory Study to
the particular analytical procedure selected for this purpose
Determine the Precision of a Test Method
qualifies (that is, provides acceptable precision and bias) (see
Note 1). The recommended procedures are ones used in the
3. Terminology
round-robin analyses to determine the precision levels of this
3.1 Definitions: Definitions are in accordance with Termi-
test method.
nology C219.
NOTE 1—Asimilar approach was used in the performance requirements
3
3.2 Phases (1):
for alternative methods for chemical analysis in Test Methods C114.
4
3.2.1 alite, n—tricalcium silicate (C S) modified in com-
3
1.3 The values stated in SI units shall be regarded as the
position and crystal structure by incorporation of foreign ions;
standard.
occurs typically between 30 to 70 % (by mass) of the portland-
1.4 This standard does not purport to address all of the
cement clinker; and is normally either the M or M crystal
1 3
safety concerns, if any, associated with its use. It is the polymorph, each of which is monoclinic.
responsibility of the user of this standard to establish appro-
3.2.2 alkali sulfates, n—arcanite (K SO ) may accommo-
2 4
+ +
priate safety, health, and environmental practices and deter-
date Na , Ca2 , and CO in solid solution, aphthitalite (K ,
3 4-x
mine the applicability of regulatory limitations prior to use.
Na )SO with x usually 1 but up to 3), calcium langbeinite
x 4
For specific hazards, see Section 9.
(K Ca [SO ] ) may occur in clinkers high in K O, and
2 2 4 3 2
1.5 This international standard was developed in accor-
thenardite (Na SO ) in clinkers with high Na/K ratios (1).
2 4
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1 the ASTM website.
This test method is under the jurisdiction ofASTM Committee C01 on Cement
3
The boldface numbers in parentheses refer to the list of references at the end of
and is the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis.
this standard.
Current edition approved March 1, 2018. Published April 2018. Originally
4
Whenexpressingchemicalformulae,C=CaO,S=SiO ,A=Al O ,F=Fe O ,
2 2 3 2 3
approved in 1998. Last previous edition approved in 2011 as C1365 – 06 (2011).
¯
DOI: 10.1520/C1365-18. M = MgO, S =SO,andH=H O.
3 2
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428
...

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. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: C1365 − 06 (Reapproved 2011) C1365 − 18
Standard Test Method for
Determination of the Proportion of Phases in Portland
Cement and Portland-Cement Clinker Using X-Ray Powder
1
Diffraction Analysis
This standard is issued under the fixed designation C1365; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*Scope
1.1 This test method covers direct determination of the proportion by mass of individual phases in portland cement or
portland-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 aluminoferrite), periclase
(magnesium oxide), gypsum (calcium sulfate dihydrate), bassanite (calcium sulfate hemihydrate), anhydrite (calcium sulfate), and
calcite (calcium carbonate).
1.2 This test method specifies certain general aspects of the analytical procedure, but does not specify detailed aspects.
Recommended procedures are described, but not specified. Regardless of the procedure selected, the user shall demonstrate by
analysis of certified reference materials (CRM’s) that the particular analytical procedure selected for this purpose qualifies (that
is, provides acceptable precision and bias) (see Note 1). The recommended procedures are ones used in the round-robin analyses
to determine the precision levels of this test method.
NOTE 1—A similar approach was used in the performance requirements for alternative methods for chemical analysis in Test Methods C114.
1.3 The values 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 responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability 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 standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
C114 Test Methods for Chemical Analysis of Hydraulic Cement
C150C150/C150M Specification for Portland Cement
C183C183/C183M Practice for Sampling and the Amount of Testing of Hydraulic Cement
C219 Terminology Relating to Hydraulic Cement
C670 Practice for Preparing Precision and Bias Statements for Test Methods for Construction Materials
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions: Definitions are in accordance with Terminology C219.
3
3.2 Phases (1):
1
This test method is under the jurisdiction of ASTM Committee C01 on Cement and is the direct responsibility 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 as
C1365 - 98 (2006).C1365 – 06 (2011). DOI: 10.1520/C1365-06R11.10.1520/C1365-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The boldface numbers in parentheses refer to the list of references at the end of this standard.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
C1365 − 18
4
3.2.1 alite, n—tricalcium silicate (C S) modified in composition and crystal structure by incorporation of foreign ions; occurs
3
typically between 30 to 70 % (by mass) of the portland-cement clinker; and is normally either the M or M crystal polymorph,
1 3
each of which is monoclinic.
+ +
3.2.2 alkali sulfates, n—arcanite
...

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