oSIST prEN 196-2:2024
(Main)Methods of testing cement - Part 2: Chemical analysis of cement
Methods of testing cement - Part 2: Chemical analysis of cement
This document specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3, SrO, Cl and Br. This method is based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria.
An alternative performance-based method using inductively coupled plasma optical emission spectroscopy (ICP-OES) is described for SO3.
When correctly calibrated according to the specified procedures and reference materials, XRF and ICP-OES provides methods equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. They can be applied to other relevant elements when adequate calibrations have been established.
Any other methods can be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods. Standard specifications state which methods are to be used.
Prüfverfahren für Zement - Teil 2: Chemische Analyse von Zement
Dieses Dokument legt die Verfahren zur Durchführung der chemischen Analyse von Zement fest.
Dieses Dokument beschreibt die Referenzverfahren und in einigen Fällen Alternativverfahren, deren Ergebnisse denen des Referenzverfahrens entsprechen. Im Streitfall sind die Referenzverfahren maßgebend.
Ein alternatives leistungsbasiertes Verfahren unter Anwendung der Röntgenfluoreszenzanalyse (XRF, en: X ray fluorescence) wird für SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3, SrO, Cl und Br beschrieben. Dieses Verfahren beruht auf Schmelztabletten der Probe und der analytischen Validierung mithilfe zertifizierter Referenzmaterialien in Kombination mit Leistungskriterien. Ein Verfahren auf der Grundlage von Pulverpresslingen aus unaufgeschlossenen Proben kann als gleichwertig angesehen werden, sofern die analytische Leistung dieselben Kriterien erfüllt.
Ein alternatives leistungsbasiertes Verfahren unter Anwendung der optische Emissionsspektroskopie mit induktiv gekoppeltem Plasma (ICP OES, en: inductively coupled plasma optical emission spectroscopy) wird für SO3 beschrieben.
Wenn die Kalibrierung ordnungsgemäß entsprechend den festgelegten Verfahren und mit den festgelegten Referenzmaterialien durchgeführt wurde, sind die mit Röntgenfluoreszenzanalyse und optischer Emissionsspektroskopie mit induktiv gekoppeltem Plasma möglichen Verfahren gleichwertig zu den Referenzverfahren, wurden jedoch hinsichtlich Konformität und Streitfällen noch nicht für die Anwendung als Referenzverfahren validiert. Nach Festlegung angemessener Kalibrierungen können sie für andere Elemente angewendet werden.
Es können andere Verfahren angewendet werden, sofern diese gegen die Referenzverfahren oder gegen international anerkannte Referenzmaterialien kalibrieret werden, um ihre Gleichwertigkeit nachzuweisen.
Dieses Dokument legt Verfahren fest, die in erster Linie für Zemente gelten. Die Verfahren können jedoch auch auf deren Bestandteile angewendet werden. Die Verfahren gelten auch für andere Stoffe, sofern in den entsprechenden Normen darauf verwiesen wird. In den Anwendungsnormen ist festgelegt, welche Verfahren anzuwenden sind.
Méthodes d'essais des ciments - Partie 2: Analyse chimique des ciments
Metode preskušanja cementa - 2. del: Kemijska analiza cementa
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
01-oktober-2024
Metode preskušanja cementa - 2. del: Kemijska analiza cementa
Methods of testing cement - Part 2: Chemical analysis of cement
Prüfverfahren für Zement - Teil 2: Chemische Analyse von Zement
Méthodes d'essais des ciments - Partie 2: Analyse chimique des ciments
Ta slovenski standard je istoveten z: prEN 196-2
ICS:
71.040.40 Kemijska analiza Chemical analysis
91.100.10 Cement. Mavec. Apno. Malta Cement. Gypsum. Lime.
Mortar
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2024
ICS 91.100.10 Will supersede EN 196-2:2013
English Version
Methods of testing cement - Part 2: Chemical analysis of
cement
Méthodes d'essais des ciments - Partie 2: Analyse Prüfverfahren für Zement - Teil 2: Chemische Analyse
chimique des ciments von Zement
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 51.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 196-2:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 General requirements for testing . 7
4.1 Number of tests . 7
4.2 Repeatability and reproducibility . 7
4.3 Expression of masses, volumes, factors and results. 7
5 Analysis by wet chemistry . 8
5.1 General. 8
5.2 Reagents . 9
5.3 Apparatus . 21
5.4 Analysis procedure . 27
5.5 Determination of major elements . 35
6 Chemical analysis by X-ray fluorescence . 60
6.1 Reagents and reference materials . 60
6.2 Apparatus . 62
6.3 Flux . 63
6.4 Determination of loss on ignition and the change in mass on fusion of the cement . 64
6.5 Factoring test results and correcting total analyses for presence of sulfides and
halides . 66
6.6 Preparation of fused beads and pressed pellets . 68
6.7 Calibration and validation . 70
6.8 Calculation and expression of results . 80
6.9 Performance criteria (repeatability, accuracy and reproducibility limits) . 81
7 Chemical analysis by inductively coupled plasma optical emission spectroscopy (ICP-
OES) . 81
7.1 Determination of SO – alternative method . 81
Annex A (informative) Examples of fluxes . 84
Annex B (informative) Sources of certified reference materials . 85
Annex C (informative) Examples of calibration standards and monitor beads and pellets . 86
Annex D (informative) . 87
D.1 Preparation of standard calibration solution . 87
D.2 Stock solutions . 87
D.3 Blank calibration solution . 87
Bibliography . 89
European foreword
This document (prEN 196-2:2024) has been prepared by Technical Committee CEN/TC 51 “Cement and
building limes”, the secretariat of which is held by NBN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 196-2:2013.
— redefinition of the introduction;
— introduction of concept;
— determination of reactive silica;
— introduction of the concept of determination of Total Carbonate Content instead of determination of
CO ;
— determination of chloride by potentiometric titration as alternative method;
— determination of Total Carbonate Content by gas volumetric method as alternative method;
— determination of Total Carbonate Content by infrared detection system (method A and B) as
alternative method;
— determination of SO by inductively coupled plasma optical emission spectroscopy as alternative
method.
This European Standard series, under the general title Methods of testing cement, comprises the following
parts:
— Part 1: Determination of strength;
— Part 2: Chemical analysis of cement;
— Part 3: Determination of setting times and soundness;
— Part 5: Pozzolanicity test for pozzolanic cement;
— Part 6: Determination of fineness;
— Part 7: Methods of taking and preparing samples of cement;
— Part 8: Heat of hydration — Solution method;
— Part 9: Heat of hydration — Semi-adiabatic method;
— Part 10: Determination of the water-soluble chromium (VI) content of cement;
— Part 11: Heat of hydration — Isothermal conduction calorimetry method.
NOTE Another document, CEN/TR 196-4 Methods of testing cement — Part 4: Quantitative determination of
constituents, has been published as a CEN Technical Report.
Introduction
In this document, the elemental chemical analysis of a clinker or cement, as of any natural or artificial
mineral material (volcanic pozzolan, blast furnace slag, fly ash, etc.) is expressed in a conventional
manner in the form of the weight proportions of the common oxides corresponding to the most frequent
and stable degree of oxidation (Si: SiO2; Al: Al2O3, etc.). This expression of the chemical analysis does not
indicate how these elements are combined into minerals such as silicates, oxides, carbonates, sulphates
or sulphides.
This means that the presence of SiO2 in a chemical analysis sheet does not necessarily implies the
presence of crystalline silica e.g. quartz or cristobalite, but most likely silicates. Moreover, even if Quartz
is detected in the material, this does not necessarily imply an inhalation hazard if the particle size is larger
than the inhalable fraction. Similarly, the presence of TiO2 in a chemical analysis report does not
necessarily imply the presence of the mineralogical phase(s) corresponding to this formula (Rutile,
Anatase, Brookite), although the presence of the mineralogical phase(s) does not necessarily imply an
inhalation hazard if the particle size is larger than the inhalable fraction. In the same way, determination
of Total Carbonate Content (TCC) can be done by dosing CO induced by acid attack, which does not mean,
in any case, that the material contains CO .
The only way to identify mineralogical phases in a powdered mineral material is by X-ray diffraction,
which is the only analytical technique that is sensitive to the crystalline character of minerals. For an
accurate quantification of inhalable fractions, it might be necessary to perform a quantitative particle size
selection (e.g. by aerosolization technique) in order to eliminate coarse fractions that could reduce the
quantitative character of the X-ray Diffraction analysis.
Standardization to 100 made it possible to know if no constituent element had been left out. Hence the
expression “percentage by weight of oxides” in the chemical analysis.
1 Scope
This document specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can
be considered to be equivalent. In the case of a dispute, only the reference methods are used.
An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO , Al O ,
2 2 3
Fe O , CaO, MgO, SO , K O, Na O, TiO , P O , Mn O , SrO, Cl and Br. This method is based on beads of fused
2 3 3 2 2 2 2 5 2 3
sample and analytical validation using certified reference materials, together with performance criteria.
A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that
the analytical performance satisfies the same criteria.
An alternative performance-based method using inductively coupled plasma optical emission
spectroscopy (ICP-OES) is described for SO .
When correctly calibrated according to the specified procedures and reference materials, XRF and ICP-
OES provides methods equivalent to the reference methods but has not been validated for use yet as a
reference procedure for conformity and dispute purposes. They can be applied to other relevant elements
when adequate calibrations have been established.
Any other methods can be used provided they are calibrated, either against the reference methods or
against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to
their constituent materials. They can also be applied to other materials, the standards for which call up
these methods. Standard specifications state which methods are to be used.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
EN 196-7, Methods of testing cement — Part 7: Methods of taking and preparing samples of cement
EN 13656, Soil, treated biowaste, sludge and waste — Digestion with a hydrochloric (HCl), nitric (HNO3)
and tetrafluoroboric (HBF4) or hydrofluoric (HF) acid mixture fo
...
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