SIST EN 16581:2015
(Main)Conservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products
Conservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products
This European Standard specifies the methodology for laboratory evaluation of the performance of water repellent products on porous inorganic materials.
It is based on the measurement of several parameters which assess the performance of the product using standard test methods before and after ageing.
NOTE Acceptable performance within the laboratory does not constitute a blanket endorsement of application in every conservation situation. It is recommended that the particular context of the heritage object, including such factors as material designation, state of conservation, exposure, salt content and problems related to water ingress are further investigated.
Erhaltung des kulturellen Erbes - Oberflächenschutz für poröse anorganische Materialien - Laborprüfverfahren für die Ermittlung der Wirksamkeit von wasserabweisenden Produkten
Die vorliegende Europäische Norm legt die Verfahrensweise für die Ermittlung der Wirksamkeit von wasserabweisenden Produkten auf porösen anorganischen Materialien im Labor fest.
Sie beruht auf der Messung mehrerer Parameter, die die Wirksamkeit des Produkts unter Verwendung von Standardprüfverfahren vor und nach der Alterung bewerten.
ANMERKUNG Zulässige Wirksamkeit innerhalb des Labors bedeutet keine pauschale Übertragbarkeit auf die Anwendung in jeder Erhaltungssituation. Es wird empfohlen, dass der spezielle Kontext des Gegenstands des Kulturerbes einschließlich solcher Faktoren wie Materialbezeichnung, Erhaltungszustand, Beanspruchung, Salzgehalt und Probleme bezüglich der Wasseraufnahme weiter untersucht wird.
Conservation du patrimoine culturel - Protection de surface des matériaux inorganiques poreux - Méthodes d'essai en laboratoire pour l'évaluation des performances des produits hydrofuges
La présente Norme européenne spécifie la méthodologie pour l'évaluation en laboratoire des performances de produits hydrofuges sur des matériaux inorganiques poreux.
Cette norme repose sur le mesurage de plusieurs paramètres qui permettent d'apprécier les performances du produit à l'aide de méthodes d'essai standard avant et après vieillissement.
NOTE Des performances acceptables en laboratoire ne constituent pas une approbation globale de l'application dans chaque situation de conservation. Il est recommandé d'étudier de façon plus approfondie le contexte particulier de l'objet patrimonial, notamment des facteurs tels que la désignation du matériau, l'état de conservation, l'exposition, la salinité et les problèmes liés à la pénétration de l'eau.
Ohranjanje kulturne dediščine - Zaščita površine poroznih anorganskih materialov - Laboratorijske preskusne metode za vrednotenje učinkovitosti vodoodbojnih sredstev
Ta evropski standard določa metodologijo za laboratorijsko vrednotenje učinkovitosti vodoodbojnih sredstev na poroznih anorganskih materialih.
Temelji na merjenju več parametrov, ki ocenjujejo učinkovitost sredstva z uporabo običajnih preskusnih metod pred staranjem in po njem.
OPOMBA: Sprejemljiva učinkovitost v laboratoriju ne pomeni zajamčenega zagovarjanja uporabe v vseh položajih ohranjanja. Priporoča se, da se dodatno raziščejo posamezne okoliščine predmeta kulturne dediščine, med drugim dejavniki, kot so označevanje materiala, stanje ohranjenosti, izpostavljenost, vsebnost soli in težave, povezane z vdiranjem vode.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.GRRGERMQLKVUHGVWHYErhaltung des kulturellen Erbes - Oberflächenschutz für poröse anorganische Materialien - Laborprüfverfahren für die Ermittlung der Wirksamkeit von wasserabweisenden ProduktenConservation du patrimoine culturel - Protection de surface des matériaux inorganiques poreux - Méthodes d'essai en laboratoire pour l'évaluation des performances des produits hydrofugesConservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products97.195Umetniški in obrtniški izdelkiItems of art and handicrafts25.220.01Površinska obdelava in prevleke na splošnoSurface treatment and coating in generalICS:Ta slovenski standard je istoveten z:EN 16581:2014SIST EN 16581:2015en,fr,de01-februar-2015SIST EN 16581:2015SLOVENSKI
STANDARD
SIST EN 16581:2015
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16581
December 2014 ICS 97.195 English Version
Conservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products
Conservation du patrimoine culturel - Protection de surface des matériaux inorganiques poreux - Méthodes d'essai en laboratoire pour l'évaluation des performances des produits hydrofuges
Erhaltung des kulturellen Erbes - Oberflächenschutz für poröse anorganische Materialien - Laborprüfverfahren für die Ermittlung der Wirksamkeit von wasserabweisenden Produkten This European Standard was approved by CEN on 18 October 2014.
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. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16581:2014 ESIST EN 16581:2015
EN 16581:2014 (E) 2 Contents Page Foreword .3 Introduction .4 1 Scope .5 2 Normative references .5 3 Terms and definitions .5 4 Symbols and abbreviations .6 5 Test methods for evaluation .7 6 Evaluation of long term performances .7 7 Test equipment for the treatment (apparatus and reagents) .7 8 Test procedure .8 8.1 Steps of evaluation of water repellent products .8 8.2 Specimen preparation and determination of dry mass .9 8.2.1 Number and dimensions of the test specimens .9 8.2.2 Surface preparation . 11 8.2.3 Initial characterization before treatment . 11 8.2.4 Measurement of dry mass after characterization tests and before the treatment (m0B) . 11 8.3 Methodology of treatment application. 11 8.3.1 General . 11 8.3.2 Conditioning of the specimens . 11 8.3.3 Duration of water repellent application . 11 8.3.4 Water repellent application by capillarity and measurement of dry constant mass after treatment (moA) . 11 9 Determination of the amount of water repellent applied . 12 10 Measurements and methods for treatment evaluation . 13 10.1 Determination of water absorption by capillarity . 13 10.2 Protection Degree by capillarity PDC . 13 10.3 Determination of water vapour permeability (/p) . 14 10.4 oeduction of water vapour permeability (/p red) . 14 10.5 Determination of static contact angle. 14 10.6 Colour measurement of surfaces . 15 10.7 Determination of water absorption by pipe method . 15 10.8 Protection Degree of water absorption by pipe method PDLP . 15 10.9 Determination of drying properties. 16 11 Test report . 17 11.1 General information . 17 11.2 Determination of water absorption by capillarity . 17 11.3 Determination of water vapour permeability . 17 11.4 Colour measurement of surfaces . 18 11.5 Measurement of water absorption by pipe method . 18 11.6 Determination of drying properties. 18 11.7 Determination of static contact angle. 18 11.8 Gloss measurement . 18 11.9 Long term performances after ageing tests . 19 Bibliography . 20
SIST EN 16581:2015
EN 16581:2014 (E) 3 Foreword This document (EN 16581:2014) has been prepared by Technical Committee CEN/TC 346 “Conservation of Cultural Heritage”, the secretariat of which is held by UNI. 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 June 2015, and conflicting national standards shall be withdrawn at the latest by June 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16581:2015
EN 16581:2014 (E) 4 Introduction As part of the conservation of built heritage, a variety of surface treatments can be carried out to delay the decay processes. This document focuses on water repellent treatments of porous inorganic materials. The main goal of a water repellent is to reduce the penetration of liquid water and the substances dissolved in the water into porous material by changing its surface properties. A water repellent product when applied to the surface of a material decreases its surface tension and prevents wetting of the surface. The water repellent treatment is applied to the surface and penetrates into the pores of the material, the depth of penetration being dependent on the capillary properties of the material, the properties of the hydrophobic, the type and duration of application as well as the moisture content of the substrate and the temperature. Many deterioration mechanisms result from the presence of water and therefore the reduction of water absorption without significantly decreasing water vapour permeability may positively influence the preservation of porous inorganic materials. Coatings including varnishes and paints are not considered within this European Standard. A water repellent should fulfil the following requirements to: — reduce the absorption of liquid water in the substrate, — minimize change of water vapour permeability of the substrate, — minimize change in colour and gloss of the substrate, — produce no harmful by-products after the application, — maintain its physical and chemical stability. Water repellent products should be applied on the surface of heritage objects only after they have been tested on representative samples of porous inorganic materials in the laboratory. Field trials on small areas are strongly recommended prior to final application. This European Standard for the evaluation of water repellent treatments is based on the measurement of appropriate parameters to assess the performance of the product using standardized test methods. In situ application methods include brushing, spraying, immersion, capillary rise absorption and poultice. Due to the dimensions of samples and the requirements to perform reproducible treatment procedures for laboratory testing, the capillarity method is specified. Where a treatment cannot be applied according to the standard method (for example when an emulsion is used) the application method should be clearly described in the test report. Technical and chemical data sheets of treatment under evaluation should be provided; the data sheets which detail at least the chemical formulas of the active substances and concentrations, the names and the ratio of solvents, if applicable. In order to evaluate the durability and in service performance of a water repellent product applied on the substrate, ageing tests representing the environment in which the porous inorganic material is located can be carried out. SIST EN 16581:2015
EN 16581:2014 (E) 5 1 Scope This European Standard specifies the methodology for laboratory evaluation of the performance of water repellent products on porous inorganic materials. It is based on the measurement of several parameters which assess the performance of the product using standard test methods before and after ageing. Acceptable performance within the laboratory does not constitute a blanket endorsement of application in every situation. The particular context of the heritage object, including such factors as material designation, condition, exposure, salt content and problems related to water ingress requires further investigation. 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 15801, Conservation of cultural property - Test methods - Determination of water absorption by capillarity EN 15802, Conservation of cultural property - Test methods - Determination of static contact angle EN 15803, Conservation of cultural property - Test methods - aetermination of water vapour permeability (/p) EN 15886, Conservation of cultural property - Test methods - Colour measurement of surfaces EN 15898, Conservation of cultural property - Main general terms and definitions EN 16085, Conservation of Cultural property - Methodology for sampling from materials of cultural property - General rules EN 16302, Conservation of cultural heritage - Test methods - Measurement of water absorption by pipe method EN 16322, Conservation of Cultural Heritage - Test methods - Determination of drying properties EN ISO 2813, Paints and varnishes - Determination of specular gloss of non-metallic paint films at 20°, 60° and 85° (ISO 2813) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15898 and the following apply. 3.1 water-repellency ability of the substrate to resist the ingress of liquid water 3.2 water repellent product product increasing the water-repellency of the treated surface of porous inorganic materials 3.3 water repellent treatment application of a water repellent product to the surface of a material by a specified methodology SIST EN 16581:2015
EN 16581:2014 (E) 6 3.4 protection degree by capillarity reduction of the amount of water absorption by capillarity before and after the treatment 3.5 protection degree by pipe reduction of the amount of water absorption by pipe before and after the treatment 3.6 specular gloss ratio of the luminous flux reflected from an object in the specular direction for a specified source and receptor angle to the luminous flux reflected from glass with a refractive index of 1,567 in the specular direction 4 Symbols and abbreviations For the purposes of this document, the following symbols and abbreviations apply: m0 B dry mass after characterization tests and before the treatment, in kg; m0 A dry mass after the treatment, in kg; ti time elapsed from the beginning of the test, in s; Qi water absorbed by capillarity per unit area, in kg/m2; AC capillary water absorption coefficient, in kg/(m2•s1/2); Qp water repellent product absorbed, as a mass %; PDCi Protection Degree by capillarity at time ti, as a mass %; QBi amount of absorbed water by capillarity of untreated specimen at time ti, in kg/m2; QAi amount of absorbed water of treated specimen at time ti, in kg/m2; ip water vapour permeability, in kg/(m ⋅ s ⋅ Pa); ip B water vapour permeability before treatment, in kg/(m ⋅ s ⋅ Pa); ip A water vapour permeability after treatment, in kg/(m ⋅ s ⋅ Pa); ip red reduction of water vapour permeability, as a %; L* lightness coordinate. The scale for L* ranges from 0 (black) to 100 (white); a* red/green coordinate, with +a* indicating redness and -a* indicating greenness; b* yellow/blue coordinate, with +b* indicating yellowness and -b* indicating blueness; L*B Lightness coordinate before treatment; L*A Lightness coordinate after treatment; a*B red/green coordinate before treatment; a*A red/green coordinate after treatment; b*B yellow/blue coordinate before treatment; b*A yellow/blue coordinate after treatment; ûü* total colour difference; PDLP Protection Degree by pipe method, as a %; (Wf)B amount of absorbed water by pipe method at the end of the test before the treatment, in ml/cm2; (Wf)A amount of absorbed water by pipe method at the end of the test after the treatment, in ml/cm2; SIST EN 16581:2015
EN 16581:2014 (E) 7 D1 B drying rate corresponding to the first drying phase before the treatment, in kg/(m2 •h); D1 A drying rate corresponding to the first drying phase after the treatment, in kg/(m2 •h); D1 red reduction of the drying rate, as a %;
contact angle, in °. 5 Test methods for evaluation The methods listed here below are used for the evaluation of a water repellent product in relation to the possible changes of the characteristics of porous inorganic materials. 1) Determination of water absorption by capillarity (EN 15801) 2) Determination of static contact angle (EN 15802) 3) Determination of water vapour permeability (EN 15803) 4) Colour measurement of surfaces (EN 15886) 5) Determination of water absorption by pipe method (EN 16302) 6) Determination of drying properties (EN 16322) 7) Gloss measurement (EN ISO 2813) 6 Evaluation of long term performances Water repellents are expected to demonstrate suitable durability on exposure to natural weathering or laboratory tests (such as light irradiation, freeze and thaw, wetting and drying, thermal cycles, salt crystallization, pollutant simulation, biological growth, etc.) representing the environment in which the object is located. In the event that a specific methodology for the assessment of environmental degradation is standardised in the field of conservation of cultural heritage, it shall be used. Where these do not exist, a suitable assessment method for Cultural Heritage should be used and described in the test report. It is important to monitor the performances of water repellent products after ageing repeating the tests listed in Clause 5, taking into account that different comparisons of the results are possible (i.e. after ageing-before treatment or after ageing-before ageing, etc…). The comparison of the results allow to evaluate the durability of products. 7 Test equipment for the treatment (apparatus and reagents) 7.1
Crystallization vessel 7.2
Bedding layer such as filter paper, foam or cotton. 7.3 Chronometer with an accuracy of 1 s. 7.4
Ventilated oven which can maintain a temperature of (40 ± 2) °C. 7.5
Analytical balance with an accuracy of at least 0,01 g. SIST EN 16581:2015
EN 16581:2014 (E) 8 7.6
Linear measuring device (calliper) with an accuracy of 0,1 mm. 7.7
Chamber capable of maintaining a constant temperature of (23 ± 2) °C. 7.8
Sand paper with grain size of 82 µm (corresponding to grit number P180 according to the FEPA 1) classification). 7.9
Desiccator filled with desiccant such as self-indicating silica gel or other drying agents. 7.10
Deionised water (with max. conductivity of 6
7.11
Soft bristle brush 7.12
Ammonium chloride saturated solution, or a climatic chamber capable of maintaining a relative humidity of (80 ± 5) %. 7.13
Magnesium nitrate saturated solution, or a climatic chamber capable of maintaining a relative humidity of (53 ± 5)%. 7.14
Glass spheres or bars (e.g. 3 mm to 4 mm diameter). 8 Test procedure 8.1 Steps of evaluation of water repellent products The evaluation of water repellent products applied on porous inorganic materials should be carried out according to the following steps (Figure 1).
1) Federation of European Producers of Abrasives SIST EN 16581:2015
EN 16581:2014 (E) 9
Figure 1 — Flow diagram for recommended test procedure 8.2 Specimen preparation and determination of dry mass 8.2.1 Number and dimensions of the test specimens Specimens shall have a regular shape such as cubes, parallelepipeds or cylinders (see Table 1). SIST EN 16581:2015
EN 16581:2014 (E) 10 Table 1 — Number and dimensions of the test specimens Test method Characteristics of test specimens Test specimens (numbers of measurements for each test specimen) Shape Dimensions mm Determination of water absorption by capillarity 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Determination of static contact angle 3 (5 measurements on each test specimen) flat surface - Determination of water vapour permeability 3
50 × 50 × 10
45 × 5 Colour measurement of surfaces 3 (5 measurements on each test specimen) flat surface - Determination of water absorption by pipe method NOTE Supplied dimensions relate to the use of vertical pipe. 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Determination of drying properties 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Gloss measurement 3 (5 measurements on each test specimen) flat surface - In the case of non-homogeneous materials, such as mortars, containing coarse aggregates, the dimensions shall be at least three times (and preferably five times) the largest grain size. The number of specimens is also dependent on the heterogeneity of the material. In case of anisotropy, the specimens shall always be tested according to the same orientation. All dimensions shall have a ± 0,5 mm tolerance. The constraints of sampling material from the cultural heritage may limit sizes and numbers of samples. However, they should be as close to the requirements above as possible. When evaluating inorganic porous materials from cultural heritage, the sampling shall follow EN 16085. SIST EN 16581:2015
EN 16581:2014 (E) 11 8.2.2 Surface preparation The surface chosen for the application of a treatment and evaluation of its performance shall be flat and wet or dry polished with sand paper. After polishing, the specimens shall be washed with water, gently brushed with a soft brush and immersed in deionised water for 30 ± 5 min. In case of water sensitive materials, for example gypsum containing materials, only dry polishing and compressed air shall be used. 8.2.3 Initial characterization before treatment Measurements for the initial characterization are carried out before the treatment according to standards listed in Clause 5. Where the listed standards allow a choice of apparatus, the one selected shall be used for both before and after treatment. 8.2.4 Measurement of dry mass after characterization tests and before the treatment (m0B) After all classification tests have been carried out, the specimens shall be dried to constant mass in a ventilated oven at a temperature of (60 ± 2)°C. If the material is temperature-sensitive, the pre-conditioning shall be conducted in a desiccator filled with desiccant or in a ventilated oven at a temperature of (40 ± 2) °C until constant mass is reached. Constant mass (m0B) is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,1 % of the mass of the specimen. In the case of materials with porosity less than 5 % constant mass is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,01 % of the mass of the specimen. 8.3 Methodology of treatment application 8.3.1 General The application method detailed in following clauses is to be used unless specifically contraindicated by material incompatibility or by an alternative application method specified by the manufacturer. The application method shall be reported and any deviations from the standard have to be described and justified in the test report. 8.3.2 Conditioning of the specimens Before treatment with water repellent products, specimens shall be pre-conditioned for 24 h at a temperature of (23 ± 2) °C and (50 ± 5) % RH, by using a climatic chamber or a desiccator maintained at (23 ± 2) °C containing a saturated solution of Mg(NO3)2. 8.3.3 Duration of water repellent application The duration of treatment depends on the chemical composition and concentration of the product/agent, on the type of the solvent and evaporation rate, and on the porosity of material. Therefore the duration of the treatment shall be established through preliminary tests on specimens and should take into account the recommendations of the manufacturer if any (technical data sheet). Where specific recommendations do not exist, preliminary tests to determine the duration of the treatment shall be carried out at the following intervals: 1 min, 5 min, 10 min, 30 min, 1 h, 2 h, and the protection degree by capillarity (PDC), see 10.2, shall be calculated for each individual interval of duration of the treatment. 8.3.4 Water repellent application by capillarity and measurement of dry constant mass after treatment (moA) a) A drying bedding layer (7.2) 1 cm of thickness and the diameter at least 1 cm larger than the maximum size of the test specimen is placed on the bottom of a crystallization vessel (7.1). SIST EN 16581:2015
EN 16581:2014 (E) 12 b) The bedding layer has to be saturated to within a few millimetres of the upper surface with water repellent solution. The solution level should not exceed the upper surface of the bedding layer and should be maintained at constant height throughout the test by adding further solution when necessary. c) The crystallization vessel is placed in a desiccator containing a saturated solution of Mg(NO3)2 and conditioned at (23 ± 2) °C for 1 h or alternatively held for 1 h at (23 ± 2) °C and (53 ± 5) % RH, by using a climatic chamber. d) Specimens are laid in contact with the bedding layer with the test face down and in contact with the water repellent solution for the time previously determined (see 8.3.3). e) At the end of the treatment specimens are turned (test face up) and placed on small glass balls or glass rods and maintained at (20 ± 2) °C and (80 ± 5) % RH. This environmental condition can be obtained either in a climatic chamber at (80 ± 5) % RH or in a desiccator containing a saturated solution of NH4Cl. f) Specimens shall be weighed during the stabilization as described in e) after 15 days and successively every seven days until constant mass is reached (m0A). Constant mass is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,01 % of the mass of the specimen (m0A). Evaluation of constant mass should be done in the same conditions as for the determination of weight before treatment otherwise the calculation of the amount of product will not be correct (see note). g) After the stabilization of treatment the specimens shall be dried in a ventilated oven at a temperature of (60 ± 2) °C. If the material is temperature-sensitive, drying shall be conducted in a desiccator filled with desiccant or in a ventilated oven at a temperature of (40 ± 2) °C until constant mass is reached. Stabilization of treatment indicates full evaporation of solvents and/or curing reactions have taken place, although guidance from the manufacturer should be taken into account. Constant mass indicates that stabilization has been achieved. Characterization tests should be carried out only when constant mass is reached. Care should be taken during the application and stabilization of samples to prevent cross contamination, particularly when using volatile molecules as active agents. 9 Determination of the amount of water repellent applied Specimen is weighed before and after the treatment ensuring that complete evaporation of the solvent according to g) of procedure 8.2.3 has occurred. The amount of water repellent product absorbed (Qp) by the specimen is determined by the following formula as the difference between dry weights before and after the treatment according to: ()100
-0B0B0A•=mmmQp (1) where Qp is the amount of applied product, expressed as a percentage (mass fraction); m0B is the constant mass before the treatment (see 8.2.4), in kg; m0A is the constant mass after the treatment (see 8.3.4), in kg. SIST EN 16581:2015
EN 16581:2014 (E) 13 10 Measurements and methods for treatment evaluation 10.1 Determination of water absorption by capillarity The water absorption experiment provides information about the material’s transport properties for liquid water. EN 15801 is based on the process of water capillary rise to calculate the water absorption coefficient (AC) and to determine the amount of water absorbed (Qi) at different time. Capillarity mea
...
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.GRRGERMQLKVUHGVWHYErhaltung des kulturellen Erbes - Oberflächenschutz für poröse anorganische Materialien - Laborprüfverfahren für die Ermittlung der Wirksamkeit von wasserabweisenden ProduktenConservation du patrimoine culturel - Protection de surface des matériaux inorganiques poreux - Méthodes d'essai en laboratoire pour l'évaluation des performances des produits hydrofugesConservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products97.195Umetniški in obrtniški izdelkiItems of art and handicrafts25.220.01Površinska obdelava in prevleke na splošnoSurface treatment and coating in generalICS:Ta slovenski standard je istoveten z:FprEN 16581kSIST FprEN 16581:2014en,fr,de01-september-2014kSIST FprEN 16581:2014SLOVENSKI
STANDARD
kSIST FprEN 16581:2014
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN 16581
July 2014 ICS 97.195 English Version
Conservation of Cultural Heritage - Surface protection for porous inorganic materials - Laboratory test methods for the evaluation of the performance of water repellent products
Conservation du patrimoine culturel - Protection de surface des matériaux inorganiques poreux - Méthodes d'essai en laboratoire pour l'évaluation des performances des produits hydrofuges
Erhaltung des kulturellen Erbes - Oberflächenschutz für poröse anorganische Materialien - Laborprüfverfahren für die Ermittlung der Wirksamkeit von wasserabweisenden Produkten This draft European Standard is submitted to CEN members for formal vote. It has been drawn up by the Technical Committee CEN/TC 346.
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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey 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:
Avenue Marnix 17,
B-1000 Brussels © 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. FprEN 16581:2014 EkSIST FprEN 16581:2014
FprEN 16581:2014 (E) 2 Contents Page Foreword .3 Introduction .4 1 Scope .5 2 Normative references .5 3 Terms and definitions .5 4 Symbols and abbreviations .6 5 Test methods for evaluation .7 6 Evaluation of long term performances .7 7 Test equipment for the treatment (apparatus and reagents) .7 8 Test procedure .8 8.1 Steps of evaluation of water repellent products .8 8.2 Specimen preparation and determination of dry mass . 10 8.2.1 Number and dimensions of the test specimens . 10 8.2.2 Surface preparation . 11 8.2.3 Initial characterization before treatment . 11 8.2.4 Measurement of dry mass after characterization tests and before the treatment (m0B) . 11 8.3 Methodology of treatment application. 11 8.3.1 General . 11 8.3.2 Conditioning of the specimens . 11 8.3.3 Duration of water repellent application . 11 8.3.4 Water repellent application by capillarity and measurement of dry constant mass after treatment (moA) . 11 9 Determination of the amount of water repellent applied . 12 10 Measurements and methods for treatment evaluation . 13 10.1 Determination of water absorption by capillarity . 13 10.2 Protection Degree by capillarity PDC . 13 10.3 Determination of water vapour permeability (/p) . 14 10.4 oeduction of water vapour permeability (/p red) . 14 10.5 Determination of static contact angle. 14 10.6 Colour measurement of surfaces . 15 10.7 Determination of water absorption by pipe method . 15 10.8 Protection Degree of water absorption by pipe method PDLP . 15 10.9 Determination of drying properties. 16 11 Test report . 17 11.1 General information . 17 11.2 Determination of water absorption by capillarity . 17 11.3 Determination of water vapour permeability . 17 11.4 Colour measurement of surfaces . 18 11.5 Measurement of water absorption by pipe method . 18 11.6 Determination of drying properties. 18 11.7 Determination of static contact angle. 18 11.8 Gloss measurement . 18 11.9 Long term performances after ageing tests . 19 Bibliography . 20
kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 3 Foreword This document (FprEN 16581:2014) has been prepared by Technical Committee CEN/TC 346 “Conservation of Cultural Heritage”, the secretariat of which is held by UNI. This document is currently submitted to the Formal Vote. kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 4 Introduction As part of the conservation of built heritage, a variety of surface treatments can be carried out to delay the decay processes. This document focuses on water repellent treatments of porous inorganic materials. The main goal of a water repellent is to reduce the penetration of liquid water and the substances dissolved in the water into porous material by changing its surface properties. A water repellent product when applied to the surface of a material decreases its surface tension and prevents wetting of the surface. The water repellent treatment is applied to the surface and penetrates into the pores of the material, the depth of penetration being dependent on the capillary properties of the material, the properties of the hydrophobic treatment and the type and duration of application. Many deterioration mechanisms result from the presence of water and therefore the reduction of water absorption may positively influence the preservation of porous inorganic materials. Coatings including varnishes and paints are not considered within this European Standard. A water repellent should fulfil the following requirements to: — reduce the absorption of liquid water in the substrate, — minimize change of water vapour permeability of the substrate, — minimize change in colour and gloss of the substrate, — produce no harmful by-products after the application, — maintain its physical and chemical stability. Water repellent products should be applied on the surface of heritage objects only after they have been tested on representative samples of porous inorganic materials in the laboratory. This European Standard for the evaluation of water repellent treatments is based on the measurement of appropriate parameters to assess the performance of the product using standardized test methods. In situ application methods include brushing, spraying, immersion, capillary rise absorption and poultice. Due to the dimensions of samples and the requirements to perform reproducible treatment procedures for laboratory testing, the capillarity method is specified. Where a treatment cannot be applied according to the standard method (for example when an emulsion is used) the application method should be clearly described in the test report. Technical and chemical data sheets of treatment under evaluation should be provided; the data sheets which detail at least the chemical formulas of the active substances and concentrations, the names and the ratio of solvents, if applicable. In order to evaluate the durability and in service performance of a water repellent product applied on the substrate, ageing tests representing the environment in which the porous inorganic material is located can be carried out. kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 5 1 Scope This European Standard specifies the methodology for laboratory evaluation of the performance of water repellent products on porous inorganic materials. It is based on the measurement of several parameters which assess the performance of the product using standard test methods before and after ageing. Acceptable performance within the laboratory does not constitute a blanket endorsement of application in every situation. The particular context of the heritage object, including such factors as material designation, condition, exposure, salt content and problems related to water ingress requires further investigation. 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 15801, Conservation of cultural property - Test methods - Determination of water absorption by capillarity EN 15802, Conservation of cultural property - Test methods - Determination of static contact angle EN 15803, Conservation of cultural property - Test methods - aetermination of water vapour permeability (/p) EN 15886, Conservation of cultural property - Test methods - Colour measurement of surfaces EN 15898, Conservation of cultural property - Main general terms and definitions EN 16085, Conservation of Cultural property - Methodology for sampling from materials of cultural property - General rules EN 16302, Conservation of cultural heritage - Test methods - Measurement of water absorption by pipe method EN 16322, Conservation of Cultural Heritage - Test methods - Determination of drying properties EN ISO 2813, Paints and varnishes - Determination of specular gloss of non-metallic paint films at 20°, 60° and 85° (fpl l813:1994f including Technical Corrigendum 1:199T) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15898 and the following apply. 3.1 water-repellency ability of the substrate to resist the ingress of liquid water 3.2 water repellent product product increasing the water-repellency of the treated surface of porous inorganic materials 3.3 water repellent treatment application of a water repellent product to the surface of a material by a specified methodology kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 6 3.4 protection degree by capillarity reduction of the amount of water absorption by capillarity before and after the treatment 3.5 protection degree by pipe reduction of the amount of water absorption by pipe before and after the treatment 3.6 specular gloss ratio of the luminous flux reflected from an object in the specular direction for a specified source and receptor angle to the luminous flux reflected from glass with a refractive index of 1,567 in the specular direction 4 Symbols and abbreviations For the purposes of this document, the following symbols and abbreviations apply: m0 B dry mass after characterization tests and before the treatment, in kg; m0 A dry mass after the treatment, in kg; ti
time elapsed from the beginning of the test, in s; Qi
water absorbed by capillarity per unit area, in kg/m2; AC
capillary water absorption coefficient, in kg/(m2•s1/2); Qp water repellent product absorbed, as a mass %; PDCi
Protection Degree by capillarity at time ti, as a mass %; QBi
amount of absorbed water by capillarity of untreated specimen at time ti, in kg/m2; QAi
amount of absorbed water of treated specimen at time ti, in kg/m2; ip
water vapour permeability, in kg/m s Pa; ip B water vapour permeability before treatment, in kg/m s Pa; ip A water vapour permeability after treatment, in kg/m s Pa; ip red reduction of water vapour permeability, as a %; L*
lightness coordinate. The scale for L* ranges from 0 (black) to 100 (white); a* red/green coordinate, with +a* indicating redness and -a* indicating greenness; b* yellow/blue coordinate, with +b* indicating yellowness and -b* indicating blueness; L*B Lightness coordinate before treatment; L*A Lightness coordinate after treatment; a*B red/green coordinate before treatment; a*A red/green coordinate after treatment; b*B yellow/blue coordinate before treatment; b*A yellow/blue coordinate after treatment; ûü* total colour difference; PDLP Protection Degree by pipe method, as a %; (Wf)B
amount of absorbed water by pipe method at the end of the test before the treatment, in ml/cm2; (Wf)A
amount of absorbed water by pipe method at the end of the test after the treatment, in ml/cm2; kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 7 D1 B
drying rate corresponding to the first drying phase before the treatment, in kg/m2 h; D1 A drying rate corresponding to the first drying phase after the treatment, in kg/m2 h; D1 red reduction of the drying rate, as a %;
contact angle, in °. 5 Test methods for evaluation The methods listed here below are used for the evaluation of a water repellent product in relation to the possible changes of the characteristics of porous inorganic materials. 1) Determination of water absorption by capillarity (EN 15801) 2) Determination of static contact angle (EN 15802) 3) Determination of water vapour permeability (EN 15803) 4) Colour measurement of surfaces (EN 15886) 5) Determination of water absorption by pipe method (EN 16302) 6) Determination of drying properties (EN 16322) 7) Gloss measurement (EN ISO 2813) 6 Evaluation of long term performances Water repellents are expected to demonstrate suitable durability on exposure to natural weathering or laboratory tests (such as light irradiation, freeze and thaw, wetting and drying, thermal cycles, salt crystallization, pollutant simulation, biological growth, etc.) representing the environment in which the object is located. In the event that a specific methodology for the assessment of environmental degradation is standardised in the field of conservation of cultural heritage, it shall be used. Where these do not exist, a suitable method for Cultural Heritage should be used and described in the test report. It is important to monitor the performances of water repellent products after ageing repeating the tests listed in Clause 5, taking into account that different comparisons of the results are possible (i.e. after ageing-before treatment or after ageing-before ageing, etc…). The comparison of the results allow to evaluate the durability of products. 7 Test equipment for the treatment (apparatus and reagents) 7.1
Crystallization vessel 7.2
Bedding layer such as filter paper, foam or cotton. 7.3 Chronometer with an accuracy of 1 s. 7.4
Ventilated oven which can maintain a temperature of (40 ± 2) °C. 7.5
Analytical balance with an accuracy of at least 0,01 g. kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 8 7.6
Linear measuring device (calliper) with an accuracy of 0,1 mm. 7.7
Chamber capable of maintaining a constant temperature of (23 ± 2) °C. 7.8
Sand paper with grain size of 82 µm (corresponding to grit number P180 according to the FEPA 1) classification). 7.9
Desiccator filled with desiccant such as self-indicating silica gel or other drying agents. 7.10
Deionised water (with max. conductivity of 6
7.11
Soft bristle brush 7.12
Ammonium chloride saturated solution, or a climatic chamber capable of maintaining a relative humidity of (80 ± 5) %. 7.13
Magnesium nitrate saturated solution, or a climatic chamber capable of maintaining a relative humidity of (53 ± 5)%. 7.14
Glass spheres or bars (e.g. 3 mm to 4 mm diameter). 8 Test procedure 8.1 Steps of evaluation of water repellent products The evaluation of water repellent products applied on porous inorganic materials should be carried out according to the following steps (Figure 1).
1) Federation of European Producers of Abrasives kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 9
Figure 1 — Flow diagram for recommended test procedure kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 10 8.2 Specimen preparation and determination of dry mass 8.2.1 Number and dimensions of the test specimens Specimens shall have a regular shape such as cubes, parallelepipeds or cylinders (see Table 1). Table 1 — Number and dimensions of the test specimens Test method Characteristics of test specimens Test specimens (numbers of measurements for each test specimen) Shape Dimensions mm Determination of water absorption by capillarity 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Determination of static contact angle 3 (5 measurements on each test specimen) flat surface - Determination of water vapour permeability 3
50 × 50 × 10
45 × 5 Colour measurement of surfaces 3 (5 measurements on each test specimen) flat surface - Determination of water absorption by pipe method NOTE Supplied dimensions relate to the use of vertical pipe. 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Determination of drying properties 3
OR
50 × 50 × 20 OR 40 × 40 × 80 OR 40 × 80 Gloss measurement 3 (5 measurements on each test specimen) flat surface - In the case of non-homogeneous materials, such as mortars, containing coarse aggregates, the dimensions shall be at least three times (and preferably five times) the largest grain size. The number of specimens is also dependent on the heterogeneity of the material. In case of anisotropy, the specimens shall always be tested according to the same orientation. All dimensions shall have a ± 0,5 mm tolerance. The constraints of sampling material from the cultural heritage may limit sizes and numbers of samples. However, they should be as close to the requirements above as possible. When evaluating inorganic porous materials from cultural heritage, the sampling shall follow EN 16085. kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 11 8.2.2 Surface preparation The surface chosen for the application of a treatment and evaluation of its performance shall be flat and wet or dry polished with sand paper. After polishing, the specimens shall be washed with water, gently brushed with a soft brush and immersed in deionised water for 30 ± 5 min. In case of water sensitive materials, for example gypsum containing materials, only dry polishing and compressed air shall be used. 8.2.3 Initial characterization before treatment Measurements for the initial characterization are carried out before the treatment according to standards listed in Clause 5. Where the listed standards allow a choice of apparatus, the one selected shall be used for both before and after treatment. 8.2.4 Measurement of dry mass after characterization tests and before the treatment (m0B) After all classification tests have been carried out, the specimens shall be dried to constant mass in a ventilated oven at a temperature of (60 ± 2)°C. If the material is temperature-sensitive, the pre-conditioning shall be conducted in a desiccator filled with desiccant or in a ventilated oven at a temperature of (40 ± 2) °C until constant mass is reached. Constant mass (m0B) is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,1 % of the mass of the specimen. In the case of materials with porosity less than 5 % constant mass is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,01 % of the mass of the specimen. 8.3 Methodology of treatment application 8.3.1 General The application method detailed in following clauses is to be used unless specifically contraindicated by material incompatibility or by an alternative application method specified by the manufacturer. The application method shall be reported and any deviations from the standard have to be described and justified in the test report. 8.3.2 Conditioning of the specimens Before treatment with water repellent products, specimens shall be pre-conditioned for 24 h at a temperature of (23 ± 2) °C and (50 ± 5) % RH, by using a climatic chamber or a desiccator maintained at (23 ± 2) °C containing a saturated solution of Mg(NO3)2. 8.3.3 Duration of water repellent application The duration of treatment depends on the chemical composition and concentration of the product/agent, on the type of the solvent and evaporation rate, and on the porosity of material. Therefore the duration of the treatment shall be established through preliminary tests on specimens and should take into account the recommendations of the manufacturer if any (technical data sheet). Where specific recommendations do not exist, preliminary tests to determine the duration of the treatment shall be carried out at the following intervals: 1 min, 5 min, 10 min, 30 min, 1 h, 2 h, and the protection degree by capillarity (PDC), see 10.2, shall be calculated for each individual interval of duration of the treatment. 8.3.4 Water repellent application by capillarity and measurement of dry constant mass after treatment (moA) a) A drying bedding layer (7.2) 1 cm of thickness and the diameter at least 1 cm larger than the maximum size of the test specimen is placed on the bottom of a crystallization vessel (7.1). kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 12 b) The bedding layer has to be saturated to within a few millimetres of the upper surface with water repellent solution. The solution level should not exceed the upper surface of the bedding layer and should be maintained at constant height throughout the test by adding further solution when necessary. c) The crystallization vessel is placed in a desiccator containing a saturated solution of Mg(NO3)2 and conditioned at (23 ± 2) °C for 1 h or alternatively held for 1 h at (23 ± 2) °C and (53 ± 5) % RH, by using a climatic chamber. d) Specimens are laid in contact with the bedding layer with the test face down and in contact with the water repellent solution for the time previously determined (see 8.3.3). e) At the end of the treatment specimens are turned (test face up) and placed on small glass balls or glass rods and maintained at (20 ± 2) °C and (80 ± 5) % RH. This environmental condition can be obtained either in a climatic chamber at (80 ± 5) % RH or in a desiccator containing a saturated solution of NH4Cl. f) Specimens shall be weighed during the stabilization as described in e) after 15 days and successively every seven days until constant mass is reached (m0A). Constant mass is reached when the difference between two successive weighing at an interval of 24 h is not greater than 0,01 % of the mass of the specimen (m0A). Evaluation of constant mass should be done in the same conditions as for the determination of weight before treatment otherwise the calculation of the amount of product will not be correct (see note). g) After the stabilization of treatment the specimens shall be dried in a ventilated oven at a temperature of (60 ± 2) °C. If the material is temperature-sensitive, drying shall be conducted in a desiccator filled with desiccant or in a ventilated oven at a temperature of (40 ± 2) °C until constant mass is reached. Stabilization of treatment indicates full evaporation of solvents and/or curing reactions have taken place, although guidance from the manufacturer should be taken into account. Constant mass indicates that stabilization has been achieved. Characterization tests should be carried out only when constant mass is reached. Care should be taken during the application and stabilization of samples to prevent cross contamination, particularly when using volatile molecules as active agents. 9 Determination of the amount of water repellent applied Specimen is weighed before and after the treatment ensuring that complete evaporation of the solvent according to g) of procedure 8.2.3 has occurred. The amount of water repellent product absorbed (Qp) by the specimen is determined by the following formula as the difference between dry weights before and after the treatment according to: ()100
-0B0B0A•=mmmQp (1) where Qp
is the amount of applied product, expressed as a percentage (mass fraction); m0B is the constant mass before the treatment (see 8.2.4), in kg; m0A
is the constant mass after the treatment (see 8.3.4), in kg. kSIST FprEN 16581:2014
FprEN 16581:2014 (E) 13 10 Measurements and methods for treatment evaluation 10.1 Determination of water absorption by capillarity The water absorption experiment provides information about the material’s transport properties for liquid water. EN 15801 is based on the process of water capillary rise to calculate the water absorption coefficient (AC) and to determine the amount of water absorbed (Qi) at different time. Capillarity measurements are carried out on untreated specimens and repeated after treatments and/or ageing of treated material on the same specimen and measuring the amount of absorbed water at the same time intervals. Before treatment with water repellent products, specimens shall be pre-conditioned for 24 h at a temperature of (23 ± 2) °C and (53 ± 5) % RH, by using a climatic chamber or a desiccators maintained at (23 ± 2) °C containing a saturated solution of Mg(NO3)2. The shape of the curve and the inclination of its linear section provide an indication of both the performances of a protective treatment applied on specimen and of the material’s characteristics. Untr
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