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

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: aluminate (tricalcium aluminate, C3A), ferrite (tetracalcium aluminoferrite, C4AF), and periclase (magnesium oxide, M) (see Note 1).
Note 1-In the future, Subcommittee C1.23 plans to add additional phases: alite (tricalcium silicate, C3S, belite (dicalcium silicate, C2S), gypsum (CSH2) hemihydrate (CSH1/2), and anhydrite (CS).
1.2 This test method specifies certain general aspects of the analytical procedure, but does not specify detailed aspects. A recommended procedure is described, but not specified. Regardless of the procedure selected, the user must demonstrate by analysis of reference materials (RM's) that the particular analytical procedure selected for this purpose qualifies (that is, provides acceptable precision and bias) (Note 2). The recommended procedure is the one used in the round-robin analysis to determine the precision and bias levels of this test method.
Note 2-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.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards, see Section 9.

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Publication Date
09-Jul-1998
Technical Committee
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ASTM C1365-98 - 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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:C 1365–98
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 C 1365; 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 (ϵ) indicates an editorial change since the last revision or reapproval.
1. Scope C114 Test Methods for Chemical Analysis of Hydraulic
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Cement
1.1 This test method covers direct determination of the
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C 150 Specification for Portland Cement
proportion by mass of individual phases in portland cement or
C 183 Practice for Sampling and the Amount of Testing of
portland-cement clinker using quantitative X-ray (QXRD)
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Hydraulic Cement
analysis. The following phases are covered by this standard:
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2 C 219 Terminology Relating to Hydraulic Cement
aluminate (tricalcium aluminate, C A), ferrite (tetracalcium
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C 670 Practice for Preparing Precision and Bias Statements
aluminoferrite, C AF), and periclase (magnesium oxide, M)
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for Test Methods for Construction Materials
(see Note 1).
E29 Practice for Using Significant Digits in Test Data to
NOTE 1—In the future, Subcommittee C1.23 plans to add additional 5
Determine Conformance with Specifications
phases: alite (tricalcium silicate, C S), belite (dicalcium silicate, C S),
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E 691 Practice for Conducting an Interlaboratory Study to
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Determine the Precision of a Test Method
gypsum ~CSH ! , hemihydrate ~CSH |n$ ! , and anhydrite ~CS! .
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3. Terminology
1.2 This test method specifies certain general aspects of the
3.1 Definitions are in accordance with Terminology
analytical procedure, but does not specify detailed aspects. A
C 219C 219.
recommended procedure is described, but not specified. Re-
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3.2 Phases (1):
gardless of the procedure selected, the user must demonstrate
3.2.1 alite, n—tricalcium silicate (C S) modified in compo-
by analysis of reference materials (RM’s) that the particular
3
sition and crystal structure by incorporation of foreign ions;
analytical procedure selected for this purpose qualifies (that is,
occurs typically between 30 to 70 % (by mass) of the Portland-
provides acceptable precision and bias) (see Note 2). The
cement clinker; and is normally either the M or M crystal
recommended procedure is the one used in the round-robin
1 3
polymorph, each of which is monoclinic.
analysis to determine the precision and bias levels of this test
3.2.2 aluminate, n—tricalcium aluminate (C A) modified in
method.
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composition and sometimes in crystal structure by incorpora-
NOTE 2—Asimilarapproachwasusedintheperformancerequirements
tion of a substantial proportion of foreign ions; occurs as
for alternative methods for chemical analysis in Test Methods C 114.
2–15 % (by mass) of the Portland-cement clinker; is normally
1.3 The values stated in SI units shall be regarded as the
cubic when relatively pure and orthorhombic when in solid
standard.
solution with significant amounts of sodium, though tetragonal
1.4 This standard does not purport to address all of the
aluminate containing a substantial amount of potassium has
safety concerns, if any, associated with its use. It is the
been reported (2).
responsibility of the user of this standard to establish appro-
3.2.3 belite, n—dicalcium silicate (C S) modified in com-
2
priate safety and health practices and determine the applica-
position and crystal structure by incorporation of foreign ions;
bility of regulatory limitations prior to use. For specific
occurs typically as 15 to 45 % (by mass) of the Portland-
hazards, see Section 9.
cement clinker as normally the β polymorph, which is mono-
clinic. In lesser amounts, other polymorphs can be present.
2. Referenced Documents
3.2.4 ferrite, n—tetracalcium aluminoferrite solid solution
2.1 ASTM Standards:
of approximate composition C (A,F) modified in composition
2
1 3
This test method is under the jurisdiction ofASTM Committee C-1 on Cement Annual Book of ASTM Standards, Vol 04.01.
4
and is the direct responsibility of Subcommittee C01.23 on CompositionalAnalysis. Annual Book of ASTM Standards, Vol 04.02.
5
Current edition approved July 10, 1998. Published December 1998. Annual Book of ASTM Standards, Vol 14.02.
2 6
When expressing chemical formulae, C = CaO, S-SiO ,A=Al O ,F=Fe O , The boldface numbers in parentheses refer to the list of references at the end of
2 2 3 2 3
M = MgO, S =SO , and H = H O. this test method.
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