ДСТУ Б EN 772-5:2013
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1 2 3 4 ^a 1 2 3 4 5 6 O 7 8 9 B 10 A 11 12 CONTENTS
page
Foreword V
1 Scope 1
2 Normative references 1
3 Principle 2
4 Symbols 2
5 Materials 2
6 Apparatus 3
7 Preparation of sample 3
8 Extraction procedure 4
9 Determinations of cations by
instrumental techniques 5
10 Alternative method of determination
of the content of active soluble 7
11 Expression of results 9
12 Test report 9 EN 772-5:2001 - - - - FOREWORD
This European Standard has been prepared by Technical Committee CEN/TC 125 "Masonry", the secretariat of which is held by BSI.
This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2000, and conflicting national standards shall be withdrawn at the latest by December 2000.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.
^AЦ?IO^AЁ?Ь?^И?Й? Methods of test for masonry units - Part 5:
Determination of the active soluble salts content of clay masonry units
This European Standard specifies a method for determining the active soluble salts content of clay masonry units.
This European Standard incorporates by dated or undated reference, provision from other publications. The normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references, the latest edition of the publication referred to applies (including amendments).
EN 771-1 Specification for masonry units - Part 1: Clay masonry units.
ISO 3310-1 Test sieves - Technical requirements and testing - Part 1: Test sieves of metal wire cloth.
ISO 3310-2 Test sieves - Technical requirements and testing - Part 2: Test sieves of perforated metal plate.
3 4 M Mg - х? , C i - ( ( E i - E x - d - 5 5.1 5.2 ^ 3 PRINCIPLE
The method adopted is based on water extraction from a crushed representative sample of the clay masonry units, and determines the amounts of soluble magnesium, sodium and potassium ions, released under the test conditions, which may be correlated with the potentially damaging effect of salts of those ions on cementitious mortars in certain circumstances, or even on the units themselves. These salts are known as "active" soluble salts in EN 771-1.
M Mg is the number of milligrams of Mg equi
valent to 1 ml of EDTA
x , y is the volume of EDTA titrated, en milli
litres (ml)
C i is the lower reference sample concen
tration, in percentage (%)
C 2 is the higher reference sample, concen
tration, in percentage (%)
tage (%)
E i is the measured signal for the lower
reference sample concentration E 2 is the measured signal for the higher
reference sample, concentration C 2
E x is the measured signal for sample
d is the dilution factor
5.1 For all methods
Distilled or deionized water for extraction of active soluble salts from the sample, and for preparation of analytical test solutions.
Hydrochloric acid (relative density 1,18).
All chemicals shall be of analytical reagent grade.
5.2 Instrumental method Atomic Absorption Spectroscopy (AAS ) and flame photometry Hydrated Lanthanum chloride
La Cl 3 x 7H 2 O210g/l Solution
Caesium Chloride CsCl 63 g/l Solution
5.3 5.4 - - - - 6 O 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 6.10 7 7.1 5.3 Instrumental method Atomic Absorption Spectroscopy (AAS) and flame photometry or inductively coupled plasma spectrometry (ICP) High purity standard solutions
5.4 EDTA method (alternative)
Magnesium metal
Ethylenediamine tetra acetic acid (EDTA) Indicators: Calcein
Methyl thymol blue complexone
Potassium hydroxide
Ammonia solution (relative density 0,88) Potassium nitrate
6.1 Test sieves, complying with the requirements of ISO 3310-1, ISO 3310-2
6.2 Mortar or other suitable grinding equipment capable of producing particles to pass a 150 p m test sieve.
6.3 Polyethylene bottle or Conical flask, typically with a capacity 500 ml
6.4 Weighing instrument, readable to the nearest 0,1 mg
6.5 Burette, typically 10 ml
6.6 Pipette, typically 10 ml, 50 ml
6.7 Graduated flask typically 1l
6.8 Volumetric flask typically 100 ml
6.9 One dimensional horizontal shaking equipment capable of oscillating at (120 + 5) min -1 having a horizontal movement of 20 mm, or a rotary shaker capable of revolving at 30 r/min + 3 min -1 .
6.10 Polyethylene bottle typically with a capacity of between 1l and 1,5 l.
7.1 Sampling
The method of sampling shall be in accordance with EN 771-1. The minimum number of specimens for the determination of the active soluble salts content shall be six and shall comprise whole units but a larger number may be specified in the product specification, in which case that larger number shall be used. The specimens shall be sampled in such a manner that they have not 7.2 8 been exposed to water that would lead to leaching of soluble salts from the units.
From the bulk sample of units a representative sample of 50 g to 250 g of material, ground to pass a 150 p m test sieve (6.1), is prepared, using the crushing method described in 7.2.
7 .2 Crushing
Crush each unit or for large units fragments representative of the interior and exterior namely 1/5 or not less than 3 kg of each unit to give lumps not greater than 10 mm. Obtain from each crushed specimen a representative subsample of at least 50 g, either by coning and quartering or using a suitable mechanical sampling device. Mix this material and crush it to give particles not greater than approximately 1 mm. Reduce the prepared sample to 50 to 250 g using the same splitting method. Finally grind the complete sample to pass a 150 p m test sieve (6.1) complying with ISO 3310-1 or ISO 3310-2, using a mortar (6.2) or other suitable grinding equipment.
Weigh 20 g + 0,05 g of the sample and transfer it to a 500 ml polyethylene bottle, or a 500 ml conical flask (6.3) when using horizontal shaking equipment (6.9). Add 200 ml of distilled or deionized water at room temperature, close the bottle with a screw-on polyethylene top and shake the bottle for 60 min, using a one dimensional horizontal shaking equipment at with a horizontal movement of 20 mm, or a rotary shaker (6.9) revolving at 30 min -1 + 3 min -1 . Filter the suspended sample using an ashless blue ribbon filterpaper or equivalent and collect the filtrate in a clean dry flask (6.10). Do not wash the residue on the filter. Alternatively use a centrifuge. It is essential that the filtrate shall be clear.
9.1 General
Determine the metal ion content using an established method, e.g. inductively coupled plasma spectrometry, atomic absorption spectroscopy, or flame photometry. Alternatively determine and calculate the magnesium content following the procedure described in clause 10.
9.2 Atomic absorption spectroscopy method (AAS) and flame photometry
9.2.1 Sample preparation
Pipette (6.6) a 50 ml aliquot of the soluble salts extract into a 100 ml volumetric flask (6.8) add 4 ml of hydrochloric acid (1 + 1 volume) and 4 ml of lanthanum chloride. If Na and 9.2.2 Calibration : preparation of the reference series
Either use dilutions of commercially available standard solutions, magnesium 1000 ppm, potassium 1 000 ppm, sodium 1 000 ppm. or, use a multi-element solution for example:
weigh the following substances up to nearest 0,1 mg:
1000 mg magnesium metal
1767,3 mg potassium carbonate K 2 CO 3 dried to 105 2305,1 mg sodium carbonate Na 2 CO 3 dried to 105 add 50 ml of hydrochloric acid (1+1 volume) wait till the reaction is completed and warm up carefully on a heating plate until complete dissolution ; complete to the mark in a 1000 ml graduated flask (6.7).
All chemicals shall be of analytical reagent grade. Then prepare a series of reference solutions as suggested in Table 1. Table 1 - Suggested reference solution series
Solution 4 ml of each 0 1 L 1) Only in case where Na, Note: If the concentration is higher than 0,03 % pipette (6.6) a low aliquot of the solution salts extract and multiply by dilution factor d (e.g.: aliquot 25 ml, dilution factor d = 2).
9.2.3 Table 2 - Suggested spectroscopic lines and
9.2.3 Spectroscopic lines and parameters for AAS and flame photometry analysis.
The data to be used for the analysis may be as given in Table 2.
parameters for AAS and flame photometry analysis 9.3 9.3.1 9.3 Inductively coupled plasma Spectrometry method (ICP)
9.3.1 General
The sample preparation (see 9.2.1) and the preparation of reference series (see 9.2.2) shall be as that for the atomic absorption spectroscopy method, but without any addition of lanthanum chloride or cesium chloride.
9.3.2 9.3.2 Spectroscopic lines for ICP analysis
The data to be used for the analysis can be as given in Table 3. Table 3 - Suggested spectroscopic lines for ICP analysis
9.4 E i - 9.4 Calculation of the results
Construct calibration on the basis of measurements taking into account the directions given by the instrument manufacturers.
For example:
E i measured signal for the lower reference sample concentration d
E 2 measured signal for the higher reference sample, concentration E x measured signal for sample
- C 1 )( E x - E i )
10 A 10.1 10.1.1 (1,0 If the concentration of the sample is greater than 0,001 % then subtract the concentration value found for the blank solution from the ca