ISO 29581-2:2010

INTERNATIONAL ISO
STANDARD 29581-2
First edition
2010-03-01
Cement — Test methods —
Part 2:
Chemical analysis by X-ray fluorescence
Ciments — Méthodes d'essais —
Partie 2: Analyse chimique par spectrométrie de fluorescence X

Reference number
©
ISO 2010
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ii © ISO 2010 – All rights reserved

Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.2
3 Terms and definitions .2
4 General requirements for testing.3
5 Reagents and reference materials.4
6 Apparatus.5
7 Preparation of a test sample of cement .6
8 Flux .7
9 Determination of loss on ignition and the change in mass on fusion of the cement .8
10 Factoring test results and correcting total analyses for presence of sulfides and halides.10
11 Preparation of fused beads and pressed pellets .12
12 Calibration and validation.14
13 Calculation and expression of results .23
14 Performance criteria (repeatability, accuracy and reproducibility limits) .24
Annex A (informative) Examples of fluxes .25
Annex B (informative) Sources of certified reference materials.26
Annex C (informative) Examples of calibration standards and monitor beads and pellets.27
Annex D (informative) Determination of the sulfate content of samples containing sulfide species.28
Bibliography.30

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 29581-2 was prepared by Technical Committee ISO/TC 74, Cement and lime.
ISO 29581 consists of the following parts, under the general title Cement — Test methods:
⎯ Part 1: Analysis by wet chemistry
⎯ Part 2: Chemical analysis by X-ray fluorescence
iv © ISO 2010 – All rights reserved

Introduction
This part of ISO 29581 incorporates the following technical principles based on comments received by the
Secretariat.
a) It provides an analytical method based on X-ray fluorescence (XRF) for use as the alternative method for
the analysis of cement. When correctly calibrated according to the specified procedures and reference
materials, it provides a method of suitable precision for conformity and information purposes.
b) It introduces a reference method for TiO , P O , SrO and Br analysis.
2 2 5
c) Traceability of the method relies upon reference materials and “pure” chemicals so that the ultimate
traceability to basic international chemical standards relies upon classical analytical methods that are
outside of the scope of this part of ISO 29581.
XRF and other instrumental methods, such as differential thermal analysis for determination of carbon dioxide,
atomic absorption spectroscopy, etc., can be used as alternative methods, provided they are calibrated
against the reference methods, or against internationally accepted reference materials.

INTERNATIONAL STANDARD ISO 29581-2:2010(E)

Cement — Test methods —
Part 2:
Chemical analysis by X-ray fluorescence
1 Scope
This part of ISO 29581 describes a performance-based method for the chemical analysis of cement for SiO ,
Al O , Fe O , CaO, MgO, SO , K O, Na O, TiO , P O , Mn O , SrO, Cl and Br using X-ray fluorescence
2 3 2 3 3 2 2 2 5 2 3
(XRF). It can be applied to other relevant elements when adequate calibrations have been established.
This part of ISO 29581 describes an alternative method for analyses of cement for conformity and information
purposes, based on beads of fused sample and analytical validation using certified reference materials,
together with performance criteria.
A method based on pressed pellets of unfused sample can be considered as equivalent, providing that the
analytical performance satisfies the same criteria.
NOTE 1 The use of fused beads generally improves the accuracy of analysis for non-volatile elements, since it
eliminates variability arising from differences in mineralogical forms or oxidation states. Pressed pellets generally improve
the accuracy of analysis for volatile elements and can give adequate accuracy for the routine analysis of non-volatile
elements.
NOTE 2 The presence of sulfide in a sample also leads to restrictions on the scope of the analysis that can be
undertaken using the XRF technique based upon fused beads. In particular, sulfate (SO ) cannot be determined directly
from such a fused bead because of the contribution to the analysis from the unknown amount of sulfide. In addition, sulfide
cannot be determined directly (or accurately, indirectly) because of the contribution of the unknown amount of sulfate to
the analysis and because of the possibility that some sulfide can be lost by volatilization during fusion. Consequently, the
method of ISO 29581-1, included as Annex D to this part of ISO 29581, is the reference method for determining the sulfate
content of samples containing sulfide species.
Other methods can be used, provided they are calibrated, either against the reference method or against
internationally accepted reference materials, in order to demonstrate their equivalence.
In the case of dispute, unless otherwise agreed by all parties, only the reference method in ISO 29581-1 can
be used.
This part of ISO 29581 describes methods that apply principally to cements, but which can also be applied to
their constituent materials and to other materials, the standards for which call up these methods.
International Standard specifications state which methods can be used.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO Guide 30, Terms and definitions used in connection with reference materials
ISO Guide 31, Reference materials — Contents of certificates and labels
ISO 29581-1, Cement — Test methods — Part 1: Analysis by wet chemistry
EN 196-7, Methods of testing cement — Part 7: Methods of taking and preparing samples of cement
EN 197-1, Cement — Part 1: Composition, specifications and conformity criteria for common cements
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
beads
glassy discs of fused sample for analysis by X-rays in the spectrometer
3.2
pellets
compressed discs of finely ground sample for analysis by X-rays in the spectrometer
3.3
calibration beads or pellets
beads or pellets used for establishing the calibration equation
3.4
analysis beads or pellets
beads or pellets containing the sample being analysed
3.5
accuracy
closeness of agreement between a test result and the certified value for a reference material
3.6
repeatability
closeness of agreement among independent test results obtained with the same method on identical test
items in the same laboratory by the same operator using the same equipment within short intervals of time
3.7
reproducibility
closeness of agreement between independent test results obtained with the same method on identical test
items in different laboratories with different operators using different equipment
3.8
expert laboratory
laboratory capable of consistently meeting the expert performance criteria set out in Clause 14
3.9
normal laboratory
laboratory capable of consistently meeting the normal performance criteria set out in Clause 14
2 © ISO 2010 – All rights reserved

4 General requirements for testing
4.1 Number of tests
Analysis of a cement can require the determination of a number of its chemical elements. For each
determination, one or more tests shall be carried out in which the number of measurements taken shall be as
specified in the relevant clause of this part of ISO 29581.
Where the analysis is one of a series subject to statistical control, the determination of each chemical element
by a single test shall be the minimum required.
Where the analysis method (including preparation and measurement) is checked at least once a week, as in
accordance with 12.5.1, a determination of each chemical element by a single test shall be the minimum
required. In the other cases, the number of tests for the determination of each chemical element shall be two;
see also Clause 13.
4.2 Accuracy and precision limits
4.2.1 Accuracy limit
The accuracy performance criterion in this part of ISO 29581 is measured as a limit on the closeness of
agreement between a test result and an accepted reference value for a certified reference material. The limits
for accuracy, expressed in percent absolute, are set out in Table 2; one set is appropriate to the performance
it is expected that an “expert” laboratory can achieve, whereas the other is appropriate for a “normal”
laboratory.
4.2.2 Repeatability limit
The repeatability performance criterion in this part of ISO 29581 is measured as a limit on the repeatability
where independent test results are obtained with the same method on identical test items (material) in the
same laboratory by the same operator using the same equipment within a short interval of time. The limits for
repeatability, expressed in percent absolute, are set out in Table 1; one set is appropriate to the performance
it is expected that an “expert” laboratory can achieve, whereas the other is appropriate to a “normal”
laboratory.
4.2.3 Reproducibility limit
The reproducibility performance criterion in this part of ISO 29581 is measured as a limit on the reproducibility
where test results are obtained with the same method on identical test items (material) in different laboratories
with different operators using different equipment. The limits for reproducibility, expressed in percent absolute,
are set out in Table 3; one set is approp
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