ДСТУ Б EN 196-2:2015
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1 Scope 1
2 Normative references 2
З? General requirements for testing .... 2
3.1 Number of tests 2
3.2 Repeatability and reproducibility . . 3
3.3 Expression of masses, volumes, factors and results 3
4 Analysis by wet chemistry 4
4.1 General 4
4.2 Reagents 5
4.3 Apparatus 22
4.4 Analysis procedure 27
4.5 Determination of major elements . 35
5 Chemical analysis by X-ray
fluorescence 66
5.1 Reagents and reference materials 66
5.2 Apparatus 68
5.3 Flux 70
5.4 Determination of loss on ignition and the change in mass on fusion of the cement 72
5.5 Factoring test results and correcting total analyses for presence of sulfides and halides 75
5.6 Preparation of fused beads and pressed pellets 78
5.7 Calibration and validation 82
5.8 Calculation and expression of results 94
5.9 Performance criteria (repeatability, accuracy and reproducibility limits) . . 94
Annex A (informative) Examplesof fluxes 95
Annex Sources ofcertified reference materials 96
Annex C (informative)
Examples of calibration standards and monitor beads and pellets 97
Bibliography 98
EN 196-2:2013 - - - -
Part 2: Chemical analysis of cement
1 1 Scope
This European Standard specifies th emethods 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 2 , AI 2 O 3 , Fe 2 O 3 , CaO, MgO, SO 3 , K 2 O, Na 2 O, TiO 2 , P 2 O 5 , Mn 2 O 3 , SrO, Cl and Br. When correctly calibrated according to the specified procedures and reference materials, it provides a method equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. It can be applied to other relevant elements when adequate calibrations have been established. 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.
Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
2 EN 196-7 ISO 385 ISO 835 ISO ISO 3.1 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, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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
ISO 385, Laboratory glassware - Burettes
ISO 835, Laboratory glassware - Graduated pipettes
ISO Guide 30, Terms and definitions used in connection with reference materials
ISO Guide 31, Reference materials - Contents of certificates and labels
3 Generalrequirements for testing
3.1 Number of tests
Analysis of a cement may require the determination of a number of its chemical properties. For each determination, one or more tests shall be carried out in which the number of measurements to be taken shall be as specified in the relevant clause of this document.
Where the analysis is one of a series subject to statistical control, the determination of each chemical property by a single test shall be the minimum required.
Where the analysis is not part of a series subject to statistical control, the number of tests for determination of each chemical property shall be two (see also 3.3 and 5.8).
3.2 3.3 In the case of a dispute, the number of tests for determination of each chemical property shall be two (see also 3.3).
3.2 Repeatability and reproducibility
Repeatability: Precision under repeatability conditions 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 short intervals of time.
Reproducibility: Precision under reproducibility conditions where test results are obtained with the same method on identical test items (material) in different laboratories with different operators using different equipment.
Repeatability and reproducibility in this document are expressed as repeatability standard deviations) and reproducibility standard deviation(s) in e.g. absolute percent, grams, etc., according to the property tested.
3.3 Expression of masses, volumes, factors and results
Express masses in grams to the nearest 0,000 1 g and volumes from burettes in millilitres to the nearest 0,05 ml.
Express the factors of solutions, given by the mean of three measurements, to three decimal places.
Express the results, where a single test result has been obtained, as a percentage generally to two decimal places.
Express the results, where two test results have been obtained, as the mean of the results, as a percentage generally to two decimal places.
If the two test results differ by more than twice the standard deviation of repeatability, repeat the test and take the mean of the two closest test results.
4 4.1 4.1.1 4.1.2 4.1.3 4.1.4 4.1.5 The results of all individual tests shall be recorded.
4 Analysis by wet chemistry
4.1 General
4.1.1 Ignitions
Carry out ignitions as follows.
Place the filter paper and its contents into a crucible which has been previously ignited and fared. Dry it, then incinerate slowly in an oxidising atmosphere in order to avoid immediate flaming, while ensuring complete combustion. Ignite the crucible and its contents at the stated temperature then allow to cool to the laboratory temperature in a desiccator. Weigh the crucible and its contents.
4.1.2 Determination of constant mass
Determine constant mass by making successive 15 min ignitions followed each time by cooling and then weighing. Constant mass is reached when the difference between two successive weighings is less than 0,000 5 g.
4.1.3 Check for absence of chloride ions (silver nitrate test)
After generally five to six washes of a precipitate, rinse the base of the filter stem with a few drops of water. Wash the filter paper and its contents with several millilitres of water and collect this in a test tube. Add several drops of silver nitrate solution (4.2.44). Check the absence of turbidity or precipitate in the solution. If present, continue washing while carrying out periodic checks until the silver nitrate test is negative.
4.1.4 Blank determinations
Carry out a blank determination without a sample, where relevant, following the same procedure and using the same amounts of reagents. Correct the results obtained for the analytical determination accordingly.
4.1.5 Preparation of a test sample of cement
Before chemical analysis, treat the laboratory sample, taken in accordance with EN 196-7, as follows to obtain a homogeneous test sample.
4.2 4.2.1 - - - Take approximately 100 g of the laboratory sample by means of a sample divider or by quartering. Sieve this portion on a 150 pm or 125 pm sieve until the residue remains constant. Remove metallic iron from the material retained on the sieve by means of a magnet (see Note 1). Then grind the iron-free fraction of the retained material so that it completely passes the 150 pm or 125 pm sieve. Transfer the sample to a clean dry container with an airtight closure and shake vigorously to mix it thoroughly.
Carry out all operations as quickly as possible to ensure that the test sample is exposed to ambient air only for the minimum time.
NOTE 1 Where the analysis is one of a series subject to statistical control and the level of the metallic iron content has been shown to be insignificant in relation to the chemical properties to be determined then it is not necessary to remove metallic iron.
NOTE 2 Where the sample is to be used for XRF analysis and it contains quartz, it might be necessary to grind the sample to pass a 90 pm sieve in order to obtain a satisfactory fusion (see 5.6). The time and temperature required to obtain a satisfactory fusion is affected by the fineness of the sample.
NOTE 3 Where the sample is to be used for XRF analysis using pressed pellets, accuracy can be improved by grinding the sample more finely.
4.2 Reagents
4.2.1 General
Use only reagents of analytical quality. References to water mean distilled or de-ionised water having an electrical conductivity < 0,5 mS/m.
Unless otherwise stated, percent means percent by mass.
Unless otherwise stated, the concentrated liquid reagents used in this document have the following densities (p) (in g/cm 3 at 20 - hydrochloric acid 1,18 to 1,19 - nitric acid 1,40 to 1,42 - perchloric acid 1,60 to 1,67 - acetic acid 1,05 to 1,06 - - 4.2.2 4.2.3 4.2.4 4.2.5 4.2.6 4.2.7 4.2.8 4.2.9 4.2.10 4.2.11 4.2.12 4.2.13 4.2.14 4.2.15 4.2.16 4.2.17 4.2.18 4.2.19 4.2.20 4.2.21 - phosphoric acid 1,71 to 1,75
- ammonium hydroxide 0,88 to 0,91
The degree of dilution is always given as a volumetric sum, for example: dilute hydrochloric acid 1 + 2 means that Ivolume of concentrated hydrochloric acid is to be mixed with 2 volumes of water.
4.2.2 Concentrated hydrochloric acid (HCI)
4.2.3 Dilute hydrochloric acid (1 + 1)
4.2.4 Dilute hydrochloric acid (1 + 2)
4.2.5 Dilute hydrochloric acid (1 + 3)
4.2.6 Di
