EUROPEAN STANDARD EN 17542-3 NORME EUROPEENNE EUROPAISCHE NORM June 2022 Ics 93.020 English Version Earthworks - Geotechnical laboratory tests - Part 3: Methylene blue value VBS on soils and rocks ‘Terrassements- Essais géotechniques en laboratoire Erdarbeiten -Geotechnische Laborversuche~Teil3 Partie 3: Valeur de bleu de methylene VBS un sol ou Metiylonblauwert VBS an Boden unc Fels dune roche ‘This European Standard was approved by CEN on 20 April 2022. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status ofa national standard without any alteration. Up-to-date lists and bibliographical references ‘concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre of to any CEN ‘member ‘This European Standard exists in three official versions (English, French, Gorman). version in any other language made by translation under the responsibilty of CEN member into its ovn language and netified to the CEN-CENELEC Management Centre has the same status as the official versions, CEN members are the natfonal standards bodies of Austria, Belgium, Rulgarka, Croatla, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of North Macedoni2, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. Jaa! EUROPEAN COMMITTEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATION EUROPAISCHES KOMITEE FOR NORMUNG CEN-CENELEC Management Centre: Rue de la Seience 23, B-1040 Brussels. ©2022.CEN —Allrights of exploitation in any form and by any means reserved Ref. No. EN 17542-3:2022 E ‘worldwide for CEN national Members,EN 17542-3 022 (E) Contents Page European foreword Apparatus 1 2 3 4 Principle of the test: 5 6 Reagents... 61 Dye solution 6.2 Preparation of 10 g/I methylene blue solution... 7 Preparation of the test portion: 7A IfDaax is greater than 50 mm. ranging between 5 mm and 50 mm. procedure for materials > 5 mm 73.3. Step 2- Washing. 74 IfDaaxis smaller or equal at 5 mm... 8 — Procedure 8.1 Description of the stain test. 82 Preparation of suspension 83 Determination of the quantity of dye adsorbed... Boos commnnme yuyu anounue es 9 Caleulation and expression of results 10 10 Test report Annex A (informative) Example of a test data sheet Table A.1 — Identification of the specimen tested ... Table A.2 - Test results...» Annex B (informative) Alternative size fraction, Bibliography .. WX: ivd-byEN 17542-3:2022 (E) European foreword ‘This document (EN 17542-3:2022) has been prepared by Technical Committee CEN/TC 396 “Earthworks”, the secretariat of which is held by AFNOR. 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 2022, and conflicting national standards shall be withdrawn at the latest by December 2022. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights, CEN shall not be held responsible for identifying any or all such patent rights, Any feedback and questions on this document should be directed to the users’ national standards body. A.complete listing of these bodies can be found on the CEN website. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: 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, Turkey and the United Kingdom. WX: ivd-byEN 17542-3 022 (E) Introduction The Methylene blue value Ves on soils and rocks is an identification parameter adopted in the classification of materials for earthworks according to EN 16907-2. It is also used for providing some specifications for construction procedures according to EN 16907-3. WX: ivd-byEN 17542-3:2022 (E) 1 Scope ‘This document describes the reference method for the determination of the methylene blue value (Ves) in soils and rocks for earthworks. ‘The test is based on measuring the quantity of methylene blue that can be adsorbed by the material suspended in water. This quantity of adsorbed methylene blue is reported by direct proportionality to the 0/50 mm ground. The soil blue value is directly related to the specific surface area of the soil particles or rocky material. NOTE The Vas test uses common equipment and calibration as the methylene blue test MB for aggregates (EN 933-9), but it applies to another granular fraction (5 mm for Vas and 2 mm for MB, respectively). Thus, the results obtained between the two tests cannot be compared in the general case. 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 ISO 17892-1, Geotechnical investigation and testing - Laboratory testing of soil - Part 1: Determination of water content (ISO 17892-1) EN ISO 17892-4, Geotechnical investigation and testing - Laboratory testing of soil - Part 4: Determination of particle size distribution (ISO 17892-4) EN 1S0 835, Laboratory glassware - Graduated pipettes (150 835) EN [80 385, Laboratory glassware - Burettes (150 385) EN 1S0 3819, Laboratory glassware - Beakers (150.3819) EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042) 3. Terms and definitions For the purposes of this document, the following terms and definitions apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses: — 180 Online browsing platform: available at https://www.isn.org/abp —_ IEC Electropedia: available at https://www-electropedia.org/ 34 subsample sample obtained by means of a sample reduction procedure 32 test portion sample used as a whole ina single test WX: ivd-byEN 17542- 22022 (E) 33 particle fraction mass percentage of particles in a range of particle sizes with defined lower and upper diameters referring to the total mass of particles in a soil volume or sample EXAMPLES Sand fraction: mass percentage of particles with particle sizes between 0,063 mm and 2,0 mm 34 constant mass successive weightings after drying at least 1h apart not differing by more than 0,1 % 35 maximum dimension Dax maximum dimension of the largest elements contained in the soil 4 Principle of the test Increments of a solution of methylene blue are added successively to a suspension of the test portion in water. The adsorption of the dye solution by test portion is checked after each addition of solution by carrying out a stain test on filter paper to detect the presence of free dye (dyes are the methylene blue particles here). When the presence of free dye is confirmed, the methylene blue value is calculated and expressed as grams of dye adsorbed per 100 g of the 0/50 mm fraction tested. 5 Apparatus 5.1 Burette or pipette, conforming to EN ISO 385 or EN ISO 835, respectively: a dosing device to inject volumes of methylen blue solution in steps of 10 ml, 5 mland 2 ml and to know the total quantity injected at+ 1m. 5.2. White Filter paper, surface mass (95 + 5) g/m?, for quantitative analysis and ash-free (<0,010 %); thickness (0,20 + 0,02) mm; filtration speed (75 4 10) s; pore size (8 + 5) um 5.3. Glass rod, length 300 mm; diameter (8 4 1) mm. 8 agitator: having a rotational speed covering at least the range of (400 £40) r/min to (600 # 60) r/min.with three or four impeller blades of (75 + 5) mm diameter. 5.5 Balance, with a maximum permissible measurement error less than 0,2 % of the weighed mass. 5.6 Stopwatch or stopelock, readable to 1 s. 5.7 Test sieves, 63 jum, 50 mm and 5 mm aperture, with guard sieve (if necessary). An alternative size fraction is given in Annex B for the preparation of the test sample. Testing other size fractions may produce results different from those obtained using the reference size fractions, The size fraction used and the reference to Annex B should then be given in the test report. 5.8 Beaker, conforming to EN ISO 3819, glass or plastic, capacity 3 000 ml mii diameter (155 +10) mm, imum and internal 5.9 Flask, class A conforming to EN ISO 1042, glass, capacity 1 000 ml. 5.10 Ventilated oven, thermostatically controlled to maintain a temperature of (100 + 5)EN 17542-3:2022 (E) 5.11 Thermometer, readable to 1 °C. 5.12 Spatula. 5.13 Desiccator. 5.14 Closed storage tainted glass bottle, capacity 1 000 mi. 6 Reagents 6.1 Dye solution Solution of standard or technical quality methylene blue, (10,0 # 0,1) g/l. 6.2 Preparation of 10 g/I methylene blue solution 6.2.1 Use methylene bhue; (CisHisCINsS, nH20 (n = 2 to 3) purity 98,5 %). 6.2.2 Determine the water content wy of the methylene blue powder as follows: — weigh approximately 5 g of methylene blue powder and record the mass to the nearest 0,01 gas Myi — dry this powder at (100 5) °C to constant mass, at Jeast 2 h. Cool in the desiccator, and then weigh immediately after taking out of the desiccator. Record the dry mass to the nearest 0,01 gas My. NOTE _Attemperatures above 105°C, the chemical structure ofthe methylene blue powder can be modified. — calculate and record the water content w, to the nearest decimal place from the following equation: we = (Mn — Mg)/Mg where ‘My _ is the mass of the methylene blue powder, in grams; Mz _ is the mass of the dried methylene blue powder, in grams. The powder used to determine the moisture content shall not be reused ‘The water content shall be determined for the preparation of every new batch of dye solution. 6.2.3. Take a mass of methylene blue powder of (10 x (1 + ws) # 0,01) g (equivalent to 10 g of dry powder) 6.2.4 Warm 500 ml to 700 ml of distilled or demineralized water ina beaker. Ifwarm waters used, the temperature shall not exceed 40°C 6.2.5 Agitate the contents of the beaker whilst slowly pouring the methylene blue powder into the water, until complete dissolution of the powder. 6.2.6 Make sure that the flask of capacity (100045) ml and the water are at a temperature of (20 + 1) °C to conform with the calibration of the flask. Pour the solution into the flask, rinsing with distilled or demineralized water to ensure complete transfer of all dye into the flask and add more Gistilled or demineralized water to the (1 000 + 5) ml graduation mark. 6.2.7 Shake the flask to ensure complete dissolution of the powder. Keep the prepared solution in a closed storage bottle (preferably tinted glass) and protected from light.22022 (E) 62.8 The following details shall be marked on the conservation bottle: — Nature of the content: 10 g/l methylene blue solution; — Date of preparation: — Use-by date, 6.2.9 Methylene blue solution shall be stored in a dark place and shalll not be used more than 1 month after preparation. 7 Preparation of the test portions 7-1 If Dmax is greater than 50 mm. Sample 10 kg of the fraction 0/50 mm, then apply procedure of 7.2. 7.2 If Dmax is ranging between 5 mm and 50 mm. Prepare a mass, m, of wet material such as m> 200 x Daa (m in grams, Drax in millimetres). Sieve, if necessary by washing, the particle fraction 0/5 mm of the sample. 7.3 Washing procedure for materials > 5 mm 7.3.1 Materials concerned Materials thatafter dry sieving visually present a significant amount of elements less than § mm glued on the refusal obtained as a result of this sieving. 7.3.2 Step 1 - Brushing ‘The first step is to perform dry brushing of the refusal obtained to recover the elements less than 5 mm glued or agglomerated. If at the end of this operation, an important amount of elements smaller than 5 mm persists, it is then necessary to carry out a washing, 7.3.3 Step 2 - Washing The procedure is: — soaking the refusal to 5 mm ; — washing (using a brush, a paintbrush or other non-metallic adapted tool) on a 5 mm sieve, using water as least as possible (if possible without adding water after the soaking phase or a quick rinsing with clean water after washing with the water charged with soaking) ; = decantation then sipho: ing (if feasible) ; — drying at a temperature not exceeding 50°C. The materials should not be dried completely. The dry residue shall be disaggregated ; — blend of the 2 fractions 0/5 mm obtained by the initial sieving and the washing operation ; — homogenization and sampling of the test sample by quartering,EN 17542-3:2022 (E) Determine the weight proportion ¢ (%) of the dry fraction 0/5 mm contained in the material (or into the 0/50 mm fraction if Dmx> 50mm). C shall be determined with a granulometric curve (see EN ISO 17892-4) Then apply the procedure of 7.2. 74 If Dax is smaller or equal at 5 mm. Prepare a mass, M of wet material such as M > 200 x Dre (M in grams, Drax in millimetres), Homogenize the fraction 0/5 mm to prepare 3 test shots with approximately the same masses and from the order of: — 30 gto 60 gin case of medium to very high clayed soils; — > 60 gfor the other soils. The first test subsample, voluntarily reduced by water content specifications, is used to determine the water content of the material, according to EN ISO 17892-1. The result of this test is designated as w. Discard this subsample. ‘The second test subsample of mass is used for the stain test (see 8.1). Weigh the test portion of the second subsample as Mo and determine its dry mass Mi to the nearest 0,1 g according to the following: Mi= Mo / (1 +w) ‘The third subsample is kept, in case the test has to be repeated. 8 Procedure 8.1 Description of the stain test After each injection of dye, the stain test consists of taking a drop of suspension by means of the glass rod. and depositing it on the filter paper. The stain which Is formed is composed of a central deposit of material, ofa generally solid blue colour, surrounded by a colourless wet zone. ‘The amount of drop taken shall be such that the diameter of the deposit is between 8 mm and 12 mm. The test is deemed to be positive if, in the wet zone, a halo consisting of a persistent light blue ring. of about 1 mm is formed around the central deposit. As the end-point is near, the halo will appear, but can then disappear again, because the clay minerals can take some time to complete their adsorption of the dye. ‘The saturation of the particle surfaces shall be validated by carrying out 5 control spots at 1 min intervals without adding any additional dye solution. ‘The halo shall he visible on each spot. 82 Preparation of suspension Place (500 + 10) mi of distilled or demineralized water in the beaker of 3 000 ml and introduce the test portion stirring well with the spatula Stir the dye solution (see 5.1) or alternatively mix it thoroughly, Fill the burette with dye solution and return the stock of dye solution to a darks place. Set the agitator to a speed of (600 + 60) min- and position the impeller about S mm above the base of the beaker.EN 17542- 22022 (E) Switch on the agitator and start the stopwatch, agitating the contents of the beaker for a minimum of 5 min at (600 # 60) r/min and subsequently (see 8.3) agitate continuously at (400 + 40) r/min for the remainder of the test 8.3 Determination of the quantity of dye adsorbed Place the filter paper (6.2) on top of an empty beaker, or some other suitable support, so that most of its surface is not in contact with any solid or liquid. After agitating for 5 min at (600 + 60) r/min, inject a dose of 5 ml to 10 ml of dye solution (see 5.1) into the beaker; agitate at (400 + 100) r/min for 1 min + 10 s and carry outa stain test (see 8.1) on the filter paper. Ifafter the addition of this initial 5 ml of dye solution the halo does not appear, add a further 5 ml of dye solution, continue agitating for 1 min, and carry out another stain test. Ifa halo still does not appear, continue agitating, making additions of dye and doing stain tests in this manner until a halo is observed. When this stage is reached, continue agitating and without further additions of dye solution, perform stain tests at 1 min intervals If the halo disappears during the first 4 min, add a further 5 ml of dye solution. If the halo disappears during the fifth minute, add only 2 ml of dye solution. In either case, continue agitating and doing stain tests until the halo persists for 5 min, Record the tatal volume of dye solution Vadded to produce a halo that persists on each control spot after 5 min without adding any additional dye solution, to the nearest 1 ml, In any case, the volume V shall be greater than 20 ml. If the volume Vis less than 20 ml, the test shall be repeated with a higher mass of test portion, If, by emptying the container on the 63 jt sieve, agglomerates of unstained particles are observed, the test shall be repeated with the third test portion by increasing the suspension time of the soil or by adopting any provision making it possible to minimize the formation of these agglomerates (example: drying at 50°C maximum, manual crumbling, then imbibition of sufficient duration to promote the disintegration of clay elements). Containers should be cleaned thoroughly with water as soon as the tests are completed. Traces of any detergents used should be removed by thorough rinsing. The containers used in methylene blue tests should be reserved specifically for that test 9 Calculat n and expression of results ‘The methylene blue value Vo o«, expressed in grams of dye per 100 g of the 0/5 mm fraction is given by Formula (1): Vyoje = =100 1 @) 10EN 17542-3:2022 (E) ‘The methylene blue value Ves, expressed in grams of dye per 100 g of the 0/50 mm fraction is given by Formula (2): Yyg= 2 xe 100 M @) where Vsoys is the methylene blue value on the 0/5 mm fraction, given by Formula (1) Ves is the methylene blue value, VBS, expressed in grams of dye per 100 g of the 0/50 mm. fraction M, isthe mass of the test portion, in grams, given in § 7; B is the total mass of methylene blue injected (solution 10,0 g/l), in gram, determined by B= V 0,01 (Vis givenin§ 8.3); c is the percentage of passing at 5 mm on the particle fraction 0/50. The Vis value shall be recorded to the nearest 0,01 g of dye per 100 g of the 0/50 mm fraction. NOTE The VBS result can be expressed also in grams of dye per kilogram of the 0/50 mm fraction, 10 Test report ‘The test report shall affirm that the test was carried out in accordance with this document and shall cor a) ) °) qd) 8) tain the following information (see Table A.1 and Table A.2): method of test used; identity of laboratory; identification of the specimen tested, e.g, by borehole number, sample number and sample depth and any other relevant details required, e.g, depth of specimen within a sample, method of sample selection, if relevant (see Table A.1); date of test; weight proportion of 0/5 mm on 0/50 mm; if relevant, alternative fraction size used (see Annex B); water content of the first subsample; wet mass and the calculated dry mass of the second subsample used for stain test; total volume of dye solution added; total mass of methylene blue injected: Vas value (see Table A.2); any deviation from the specified test procedure, and any other information that could be important for interpreting the test results. An example of test report is given in the model test sheet of Annex A. cry22022 (E) Annex A (informative) Example ofa test data sheet Table A.1 — Identification of the specimen tested laboratory: Identification of the sample: Test date: Operator: Table A.2 - Test results Maximum dimension of the largest elements contai ‘ined in the soil Dox = mm. For soils with Dr > 5 mm For soils with Dye 5 mm: weight proportion: /Smm 0750 mm Weight proportion: ¢ Ist subsample - water content: wet mass: dry mass: M’= g water content: w= (M-M')/ M'=% 2nd subsample, used for stain test: wet ma: calculated dry mass: Mi = Mo/(1+W) Stain test on the second subsample: total volume of dye solution added (solution 10,0 g/l): ¥= ml total mass of methylene blue injected: B = V x 0,01 methylene blue value on the 0/5 mm fraction: ¥, » @ Bx<100 My, 8 1 BxC%100 ‘sy express in grams of dye per 100 g of the 0/50 mm fraction This sheet is to be stapled with filter paper used for ‘The technician: 12 the test. Date, signature:EN 17542-3:2022 (E) Annex B (informative) Alternative size fraction ‘The following variation to the reference test (see 5.7) is possible on condition that the size fraction used and the reference to this annex are given in the test report. NOTE Testing the size fraction given in this annex may produce results different from those obtained using the reference size fraction. ‘The alternative size fraction that shall be used for the Vss test is 0/5,6 mm instead of 0/5 mm for the preparation of the test portions (see Clause 7), 13EN 17542- (1) [2] 8] 4 14 22022 (E) Bibliography EN 93: blue test Tests for geometrical properties of aggregates - Part 9: Assessment of fines - Methylene Methylene blue test. Bulletin of the Laboratoires des Ponts et Chaussées. Special issue published in 1990 EN 16907-2, Earthworks - Part 2: Classification of materials EN 16907-3, Earthworks - Part 3: Construction procedures