ASTM C1365-06

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
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 C 150 (Annex A1).
This test method assumes that the operator is qualified to operate an X-ray diffractometer and to interpret X-ray diffraction spectra.
This test method may be used as part of a quality control program in cement manufacturing.
This test method may be used in predicting properties and performance of hydrated cement and concrete that are a function of phase composition.
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 0
A similar approach was used in the performance requirements for alternative methods for chemical analysis in Test Methods C 114.
1.3 The values stated in SI units shall be regarded as the standard.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards, see Section 9.

General Information

• Status: Historical
• Publication Date: 14-Dec-2006
• ICS: 91.100.10 - Cement. Gypsum. Lime. Mortar
• Technical Committee: C01 - Cement
• Drafting Committee: C01.23 - Compositional Analysis

Relations

• Replaces: ASTM C1365-98(2004) - Standard Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis
• Effective Date: 15-Dec-2006
• Replaced By: ASTM C1365-06(2011) - Standard Test Method for Determination of the Proportion of Phases in Portland Cement and Portland-Cement Clinker Using X-Ray Powder Diffraction Analysis
• Effective Date: 01-Dec-2011
• Referred By: ASTM E3294-22 - Standard Guide for Forensic Analysis of Geological Materials by Powder X-Ray Diffraction
• Effective Date: 15-Dec-2006

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: C1365 – 06
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* 2. Referenced Documents
2
1.1 This test method covers direct determination of the 2.1 ASTM Standards:
proportion by mass of individual phases in portland cement or C114 Test Methods for Chemical Analysis of Hydraulic
portland-cement clinker using quantitative X-ray (QXRD) Cement
analysis. The following phases are covered by this standard: C150 Specification for Portland Cement
alite (tricalcium silicate), belite (dicalcium silicate), aluminate C183 Practice for Sampling and the Amount of Testing of
(tricalcium aluminate), ferrite (tetracalcium aluminoferrite), Hydraulic Cement
periclase (magnesium oxide), gypsum (calcium sulfate dihy- C219 Terminology Relating to Hydraulic Cement
drate), bassanite (calcium sulfate hemihydrate), anhydrite (cal- C670 Practice for Preparing Precision and Bias Statements
cium sulfate), and calcite (calcium carbonate). for Test Methods for Construction Materials
1.2 This test method specifies certain general aspects of the E29 Practice for Using Significant Digits in Test Data to
analytical procedure, but does not specify detailed aspects. Determine Conformance with Specifications
Recommended procedures are described, but not specified. E691 Practice for Conducting an Interlaboratory Study to
Regardless of the procedure selected, the user shall demon- Determine the Precision of a Test Method
strate by analysis of certified reference materials (CRM’s) that
3. Terminology
the particular analytical procedure selected for this purpose
3.1 Definitions are in accordance with Terminology C219.
qualifies (that is, provides acceptable precision and bias) (see
3
Note 1). The recommended procedures are ones used in the 3.2 Phases (1):
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round-robin analyses to determine the precision levels of this 3.2.1 alite, n—tricalcium silicate (C S) modified in com-
3
position and crystal structure by incorporation of foreign ions;
test method.
occurs typically between 30 to 70 % (by mass) of the portland-
NOTE 1—Asimilarapproachwasusedintheperformancerequirements
cement clinker; and is normally either the M or M crystal
1 3
for alternative methods for chemical analysis in Test Methods C114.
polymorph, each of which is monoclinic.
1.3 The values stated in SI units shall be regarded as the
3.2.2 alkali sulfates, n—arcanite (K SO ) may accommo-
2 4
standard. + +
date Na , Ca2 , and CO in solid solution, aphthitalite (K
3 4-
1.4 This standard does not purport to address all of the
x,Na )SO with x usually 1 but up to 3), calcium langbeinite
x 4
safety concerns, if any, associated with its use. It is the
(K Ca [SO ] ) may occur in clinkers high in K O, and
2 2 4 3 2
responsibility of the user of this standard to establish appro-
thenardite (Na SO ) in clinkers with high Na/K ratios (1).
2 4
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific
2
hazards, see Section 9. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1
This test method is under the jurisdiction ofASTM Committee C01 on Cement the ASTM website.
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and is the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis. The boldface numbers in parentheses refer to the list of references at the end of
Current edition approved Dec. 15, 2006. Published January 2007. Originally this standard.
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approved in 1998. Last previous edition approved in 2004 as C1365 - 98 (2004). Whenexpressingchemicalformulae,C=CaO,S=SiO ,A=Al O ,F=Fe O ,
2 2 3 2 3
DOI: 10.1520/C1365-06. M = MgO, S 5 SO,andH=H O.
3 2
*A Summary of Changes section appears at the end of this standard.
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C1365 – 06
3.2.3 aluminate, n—tricalcium aluminate (C A) modified in 3.3.3 phase, n—a homogeneous, physically distinct, and
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composition and sometimes in crystal structure by incorpora- mechanically separable portion of a material, identifiable by its
tion of a substantial proportion of foreign ions; occurs as 2 to chemical composition and crystal structure.
15 % (by mass) of the
...