SIST EN 16845-1:2017
(Main)Photocatalysis - Anti-soiling chemical activity using adsorbed organics under solid/solid conditions - Part 1: Dyes on porous surfaces
Photocatalysis - Anti-soiling chemical activity using adsorbed organics under solid/solid conditions - Part 1: Dyes on porous surfaces
This European standard specifies a test method for the evaluation of the photocatalytic self cleaning performance of materials showing photocatalytic activity, usually based on semiconducting metal oxides such as titanium dioxide, by the measure under solid/solid conditions of the de-colourisation ability of a test sample under illumination with ultraviolet light (UV-A), previously coloured by spreading on it a dye solution and dried This European standard is intended for use with opaque and rough surfaces of different kinds, such as construction materials in flat sheet, board or plate shape, that are the basic forms of materials for various applications. This European standard also applies to fabric, plastic or composites containing photocatalytic materials that are not soluble in acetone. This European standard does not apply to photocatalytic glass, granular materials (unless they are deposited in compact films or layers over flat solid surface) and flat non porous materials. The method evaluates only the self cleaning ability of the material under ultraviolet light irradiation. It cannot be applicable to evaluate other performance attributes of photocatalytic materials, i.e., decomposition of water contaminants in liquid or gas phases contacting the material, and antifogging and antibacterial actions.
Photokatalyse - Schmutzabweisende, chemische Aktivität unter Verwendung adsorbierender organischer Stoffe im Zustand fest/fest - Teil 1: Farbstoffe auf porösen Oberflächen
Diese Europäische Norm legt ein Prüfverfahren für die Bewertung der photokatalytischen Selbstreinigungs¬wirkung von Materialien mit photokatalytischer Aktivität fest, üblicherweise auf Basis von halbleitenden Metalloxiden, z. B. Titandioxid, durch Messung der Entfärbungsfähigkeit bei Bestrahlung mit UV-Licht (UV-A) einer mit einer Farbstofflösung besprühten und getrockneten Probe unter fest/fest-Bedingungen.
Diese Europäische Norm ist zur Anwendung bei opaken rauen Oberflächen verschiedener Art vorgesehen, z. B. Baustoffe in Form von Blechen, Brettern oder Platten, die die Grundformen von Materialien für ver-schiedene Anwendungen darstellen.
Diese Europäische Norm gilt außerdem für Gewebe, Kunststoffe oder Verbundstoffe, die photokatalytische Materialien enthalten, die in Aceton nicht löslich sind. Diese Europäische Norm gilt nicht für photo¬kata-lytisches Glas, photokatalytische Granulate (außer sie wurden als Kompaktfolie oder kompakte Schicht auf einer flachen, festen Oberfläche aufgetragen) und flache, nichtporöse photokatalytische Materialien.
Das Verfahren bewertet nur die Selbstreinigungsfähigkeit des Materials bei Bestrahlung mit UV-Licht. Es kann nicht angewendet werden, um andere Leistungsattribute photokatalytischer Materialien zu bewerten, d. h. Zersetzung von Wasserverunreinigungen in flüssigen oder gasförmigen Phasen, die mit dem Material in Berührung kommen, und Antibeschlagwirkung und antibakterielle Wirkung.
Photocatalyse - Activité chimique anti-salissures à l’aide de matières organiques adsorbées dans des conditions solide/solide - Partie 1 : Colorants sur des surfaces poreuses
La présente Norme européenne spécifie une méthode d’essai pour l’évaluation de la performance d’auto-nettoyage photocatalytique des matériaux présentant une activité photocatalytique, reposant généralement sur des oxydes métalliques semi-conducteurs comme le dioxyde de titane, par mesure dans des conditions solide/solide de la capacité de décoloration sous irradiation avec de la lumière ultraviolette (UV-A) d’un échantillon d’essai sur lequel une solution de colorant est pulvérisée et séchée.
La présente Norme européenne est destinée à être utilisée pour des surfaces opaques et rugueuses de différents types, comme les matériaux de construction sous forme de tôles plates, de panneaux ou de plaques, c’est-à-dire les formes de base des matériaux destinés à diverses applications.
La présente Norme européenne s’applique également aux tissus, plastiques ou composites contenant des matériaux photocatalytiques qui ne sont pas solubles dans l’acétone. La présente Norme européenne ne s’applique pas au verre photocatalytique, aux matériaux granulaires (sauf s’ils sont déposés en films ou couches compacts sur une surface solide plane) et aux matériaux non poreux plats.
La méthode évalue uniquement la capacité auto-nettoyante du matériau sous irradiation à la lumière ultraviolette. Elle ne peut pas être appliquée pour évaluer d’autres attributs de performance des matériaux photocatalytiques, à savoir la décomposition des polluants de l’eau en phase liquide ou gazeuse en contact avec le matériau, ou les actions anti-buée et anti-bactérienne.
Fotokataliza - Kemično ukrepanje proti onesnaženju z uporabo adsorbiranih organskih snovi v pogojih trden/trden - 1. del: Barvila na poroznih površinah
Ta evropski standard določa preskusno metodo za ocenjevanje fotokatalitskih samočistilnih lastnosti materialov, ki izkazujejo fotokatalitsko dejavnost, običajno na podlagi polprevodniških kovinskih oksidov, kot je titanov dioksid, in sicer z merjenjem zmožnosti razbarvanja preskusnega vzorca pri osvetlitvi z ultravijolično svetlobo (UV-A), predhodno obarvanega z barvno raztopino in posušenega, v pogojih trden/trden. Ta evropski standard je namenjen za uporabo pri različnih neprosojnih in grobih površinah, kot so gradbeni materiali v ploski ali ploščati obliki, ki sta osnovni obliki materialov za različne načine uporabe. Ta evropski standard se uporablja tudi za tekstilije, plastiko ali kompozite, ki vsebujejo fotokatalitske materiale, netopne v acetonu. Ta evropski standard se ne uporablja za fotokatalitsko steklo, sipke materiale (če niso naneseni v kompaktnih slojih ali plasteh na ravno trdno površino) in za ravne neporozne materiale. Metoda ocenjuje zgolj samočistilno zmožnost materiala pri obsevanju z ultravijolično svetlobo. Ne more se uporabljati za ocenjevanje drugih zmogljivosti fotokatalitskih materialov, npr. razkrajanje vodnih onesnaževalcev v tekočih ali plinskih fazah, ki vsebujejo material, ter protizamegljevalne in antibakterijske učinke.
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.UELUDQLKPhotocatalyse - Activité chimique anti-salissures à l’aide de matières organiques adsorbées dans des conditions solide/solide - Partie 1 : Colorants sur des surfaces poreusesPhotocatalysis - Anti-soiling chemical activity using adsorbed organics under solid/solid conditions - Part 1: Dyes on porous surfaces25.220.20Površinska obdelavaSurface treatmentICS:Ta slovenski standard je istoveten z:EN 16845-1:2017SIST EN 16845-1:2017en,fr,de01-maj-2017SIST EN 16845-1:2017SLOVENSKI
STANDARD
SIST EN 16845-1:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16845-1
March
t r s y ICS
t wä t t rä t r English Version
Photocatalysis æ Antiæsoiling chemical activity using solid conditions æ Part
sã Dyes on porous surfaces Photocatalyse æ Activité chimique antiæsalissures à l 5aide de matières organiques adsorbées dans des surfaces poreuses
Photokatalyse æ Schmutzabweisendeá chemische Aktivität unter Verwendung adsorbierender Farbstoffe auf porösen Oberflächen This European Standard was approved by CEN on
s v November
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x z v wæ sã t r s y ESIST EN 16845-1:2017
EN 16845-1:2017 (E) 2 Contents Page European foreword . 4 1 Scope . 5 2 Normative references . 5 3 Terms and definitions . 5 4 Symbols and abbreviations . 6 5 Principle . 7 6 Instruments . 7 6.1 Spraying system . 7 6.2 Analytical balance . 9 6.3 Diffuse Reflectance Spectrometer . 10 6.4 Light source . 10 6.5 Other experimental needs . 10 7 Materials . 10 7.1 Dyes used . 10 7.2 Preparation of Solutions to Spray . 11 7.3 Test Samples . 11 7.4 Other experimental needs . 11 8 Procedure. 11 8.1 General Aspects . 11 8.1.1 General . 11 8.1.2 Initial set up and calibration . 12 8.1.3 Measurement of the Reflectance Spectra of the Surface . 12 8.2 Optimization of the Experimental Setup . 12 8.2.1 General . 12 8.2.2 Optimization of the Spraying Distance and Flow . 12 8.2.3 Measurement of the Spraying Flow Rate . 12 8.2.4 Evaluation of the Deposition Rate (DR) . 13 8.3 Test Procedure . 13 8.3.1 Evaluation of the Dirt Parameter Calibration Function . 13 8.3.2 Choice of Test Sample Covered with Dye for Irradiation . 14 8.3.3 Evaluation of the Photocatalytic Self-cleaning Performance . 14 8.3.4 Results . 15 9 Calculation . 15 9.1 General . 15 9.2 Spraying Flow (f) . 15 9.3 Dirt Parameter . 16 9.4 Covered Area . 16 9.5 Deposition Rate . 17 9.6 Standard Spraying Time . 17 9.7 Dirt Parameter Calibration Function . 18 9.8 Remaining . 18 9.9 Dye Half-Life . 18 10 Precision and Reproducibility . 19 SIST EN 16845-1:2017
EN 16845-1:2017 (E) 3 11 Test Method for Samples with Low to Negligible Performance . 19 12 Test Report . 19 Annex A (informative)
Typical Experimental Data . 21 A.1 General . 21 A.2 Optimization of the Spraying Conditions (example) . 21 A.3 Measurement of the Spraying Mass Flows (example) . 22 A.4 Measurement of the Covered Area (example) . 23 A.5 Evaluation of the Dirt Parameter Calibration Function (example) . 25 A.6 Evaluation of the Self-cleaning Effect (example) . 27 Bibliography . 29
SIST EN 16845-1:2017
EN 16845-1:2017 (E) 4 European foreword This document (EN 16845-1:2017) has been prepared by Technical Committee CEN/TC 386 “Photocatalysis”, 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 September 2017, and conflicting national standards shall be withdrawn at the latest by September 2017. 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. EN 16845, Photocatalysis — Anti-soiling chemical activity using adsorbed organics under solid/solid conditions, is dedicated to anti-soiling chemical activity using adsorbed organics under solid/solid conditions and is constituted by the following parts: — Part 1: Dyes on porous surfaces; — Part 2: Simulated weathering conditions. 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16845-1:2017
EN 16845-1:2017 (E) 5 1 Scope This European Standard specifies a test method for the evaluation of the photocatalytic self-cleaning performance of materials showing photocatalytic activity, usually based on semiconducting metal oxides such as titanium dioxide, by the measurement under solid/solid conditions of the decolouring ability under irradiation with ultraviolet light (UV-A) of a test sample on which a dye solution is sprayed and dried. This European Standard is intended for use with opaque and rough surfaces of different kinds, such as construction materials in flat sheet, board or plate shape, that are the basic forms of materials for various applications. This European Standard also applies to fabric, plastic or composites containing photocatalytic materials that are not soluble in acetone. This European Standard does not apply to photocatalytic glass, granular materials (unless they are deposited in compact films or layers over flat solid surface) and flat non porous materials. The method evaluates only the self-cleaning ability of the material under ultraviolet light irradiation. It cannot be applicable to evaluate other performance attributes of photocatalytic materials, i.e. decomposition of water contaminants in liquid or gas phases contacting the material, and antifogging and antibacterial actions. 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. CEN/TS 16599, Photocatalysis - Irradiation conditions for testing photocatalytic properties of semiconducting materials and the measurement of these conditions CEN/TS 16981, Photocatalysis — Glossary of terms EN ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Terms and definitions For the purposes of this document, the terms and definitions given in CEN/TS 16981 and the following apply. 3.1 self-cleaning ability of a material to maintain clean or to clean itself if soiled on its surface 3.2 photocatalytic self-cleaning self-cleaning ability of a material as a consequence of the irradiation of the material surface with
UVVISIR radiation 3.3 spraying distance distance from the outlet of the spraying gun (see experimental setup) and the surface of the test sample SIST EN 16845-1:2017
EN 16845-1:2017 (E) 6 3.4 covered area CA area of the sample where the colour intensity is
·
13,5% of the maximum intensity 3.5 dirt parameter DP dye amount spread or persistent over the sample surface 3.6 dirt parameter calibration function mathematical function that describes the relation between the Dirt Parameter and the amount of dye spread over the sample surface 4 Symbols and abbreviations a, b, c polynomial constant parameters obtained by the fit using Formula (7) Anet
CA Covered Area (cm2) Cdye concentration of the dye in the spraying solution (g cm–3) dac density of acetone at the temperature of the measurement (g cm–3) DP dirt parameter (nm): the parameter is indexed depending on the context DR deposition rate (g s–1 cm «2) f volumetric spraying flow (cm3 s–1) Fi mass flow (g s «1) kdye first order kinetic constant of the specified dye for the photocatalytic self-cleaning process (min–1) MW molecular weight n number of steps used for deposition of the dye on the sample surface; typically, n = 5, but can be larger if the surface is excessively wet
spei and j referring to steps of spraying and illumination, respectively Rbackground
SC standard dye covering defined in Table 2 (g cm «2) T temperature in °C ti irradiation time in min tspr spraying time (s), calculated as tspr = sprstdt/n W the full width at half maximum (FWHM) of the sprayed dye colour peak (cm)
average covering of dye at the surface (g cm–2); indexes i and j refer to steps of spraying and illumination, respectively o maximum average covering of dye at the surface (g cm–2), obtained at sprstdt SIST EN 16845-1:2017
EN 16845-1:2017 (E) 7
wavelength (nm) max wavelength (nm) at which there is a maximum of absorbance sprstdt standard spraying time (s) τ1/2dye half-life of the dye for the photocatalytic self-cleaning process (min) 5 Principle This standard concerns the comparison and the quality assurance of photocatalytic materials used as self-cleaning materials. The method described is intended to measure the photocatalytic self-cleaning performance of a photocatalytic material by evaluating its ability to clean its surface, previously covered by a known amount of coloured organic compound, as a consequence of the exposition to ultraviolet light. A controlled amount of a dye solution dissolved in a volatile solvent (acetone) is spread on the tested surface by using a spraying gun. The photocatalytic material turns out to be covered by the solid dye. The relation between the amount of the spread dye and the spectrophotometric reflectance is defined in the calibration step. The calibration function involves the measurement of the reflectance spectra of the sample surface as a function of the dyes covering. Dyes used in separate experiments are Metanil Yellow, Rhodamine B, and Methylene Blue. The test shall be carried out with the dye showing the maximum optical contrast with the material to be tested. Criteria for the choice of the best dye are here given (see 8.3.2). Optionally, the test can be carried out with the others dyes as the reactivity of each dye can depend on the specimen. The measurement with more than one dye is encouraged, but it is not compulsory. The self-cleaning activity measured by this test shall be referred to the used dye. The soiled surface is then irradiated in air by UV-A light under defined conditions and the decrease of the dye amount on the surface is monitored by measuring the reflectance spectra of the surface of the test sample in the visible range. By using the calibration function the change of the reflectance spectra can be related to the kinetic of disappearance of the dye from the surface. The photocatalytic self-cleaning performance is determined as the half-life (minutes) of the dyes applied to the surface. 6 Instruments 6.1 Spraying system The method described in this standard relies on the possibility to cover the sample surface with the dye in a controlled way. A spraying system shall be used to spread over the sample surface a solution of the dye (dye solution) in volatile solvent (acetone). The spraying system consists of a sample support and in a pneumatic system under pressure able to spray the dye solution over the sample for different definite times. The dye solution shall be spread by using a spraying gun that forms a circular spot. This involves a normal (Gaussian) distribution of the amount of dye centred in the spot of the dye on the surface. The amount of solution spread over the test sample is controlled by changing the spraying time (tspr) with a timer that opens and closes, with a precision of ± 0,01 s, the dye solution flow. The relative distance and orientation between the gun and the sample shall be changed in a way to obtain a symmetric covering of the surface of the test sample and the desired surface covered area. Due to the normal distribution of the colour intensity at the test piece surface, the dye surface covered area is defined as the area of the sample where the colour intensity is
·
% of the maximum intensity (see 8.2). The optimal distance from the gun outlet to the surface of the test sample is referred as the spraying distance. A sketch of the pneumatic spraying system and of the sample support is shown in Figure 1 and Figure 2. SIST EN 16845-1:2017
EN 16845-1:2017 (E) 8 One pressurized ((3,0 ± 0,1) bar) bottle containing water and at least one pressurized ((3,0 ± 0,1) bar) bottle containing the dye solution (spraying liquids) are connected to the spraying gun by tubes made of materials resistant to the used solvent (for example PTFE (polytetrafluoroethylene)). The bottles and gun materials shall also be chemically inert to water and acetone. Bottles containing dye solutions or water can be selected acting on the corresponding valves. The gun is connected to air and N2 pressurized lines ((3,0 ± 0,1) bar) that supply the atomization and the actuator gases. The actuator line is controlled by an electro-valve connected to a digital timer. The amount of solution spread over the test sample is controlled by changing the spraying time with a digital timer that opens and closes the actuator line with a precision of ± 0,01 s.
Key A (N2) actuator gas line (N2) A air atomization AIR A tressurized bottles Aw water Ad dye/dyes solution B spraying gun 123 digital timer EV electrovalve GR gas regulator with manometer GT gastap pair pressurized AIR S sample V(N2) vent gas line (N2) Figure 1 — Pneumatic spraying system SIST EN 16845-1:2017
EN 16845-1:2017 (E) 9
Key A position of the spraying gun B sample arrows forward or back, up or down translation of the sample position Figure 2 — Sample support The spraying distance between the gun and the sample (see Figure 2) is typically fixed after setup of the instrumentation (see 8.2); the test samples are placed orthogonally to the spraying flow direction. The spraying gun shall provide a circular sprayed spot. Using a 0,8 mm fluid nozzle orifice under the given pressure, the typical spray distance is 200 mm. Typically, the fluid flow through the gun shall be regulated to obtain a value close to 0,2 cm3 s–1. For the accurate measurement of the spraying flow see 8.2.2. The atomization air flow is typically (270 ± 20) N dm3 min–1. The system shall be operated under a ventilated chemical hood. Safety precautions shall be taken for use of acetone (CAS No: 67-64-1) such as safety glasses, good ventilation, removal of sources of ignition from the working area. 6.2 Analytical balance An analytical balance with the precision of 10 «4 g is used for all the gravimetric operations. SIST EN 16845-1:2017
EN 16845-1:2017 (E) 10 6.3 Diffuse Reflectance Spectrometer The diffuse reflectance spectra of the sample surfaces shall be measured by using a diffuse reflectance spectrophotometer working in the VIS wavelength range from 400 nm to 750 nm excluding the specular component. Any commercial spectrophotometer with integrating sphere accessory can be used, including low cost instruments having wavelength band pass
¶ 3 nm. The reflectance spectra are measured by using a diffuse reflectance standard such as BaSO4 as a reference of 100 % reflectance material. 6.4 Light source The light source should agree with CEN/TS 16599. It shall provide UV-A irradiation within a wavelength range of 345 nm to 385 nm for a specimen containing TiO2. Suitable sources include the so-called black light (BL) and black light blue (BLB) fluorescent lamps, with a maximum at 351 nm or 368 nm, and xenon arc lamps with optical filters that block radiation below 345 nm. In the case of xenon arc lamp, a cooling system shall be used. The test sample shall be irradiated uniformly. The distance between the light source and the sample shall be adjusted so that the UV irradiance (300 nm to 400 nm) at the sample surface is (20 ± 0,5) W m–2. A UV radiometer in conformity with CEN/TS 16599 shall be put at the same distance as the surface of the test sample to be tested. The irradiance along the length of the test sample shall also be constant within ± 5 %. The temperature of the sample during the test shall be (25 ± 5) °C. 6.5 Other experimental needs a) A bottle with a neck diameter larger than the spot dye spot size, as determined under b) in 8.2.3. b) Ventilated chemical hood. c) Sonication bath. d) Safety glasses. e) Vial (from 20 ml to 30 ml in
volume) for use in a) and c) in 8.2.3. 7 Materials 7.1 Dyes used Three different dyes can be used in the test (see Table 1). The dyes shall be dissolved in acetone (2-propanone), a volatile organic solvent that allows a perfect solubilisation of the dyes. The dyes have different optical contrast on the test sample depending on their colour. When a dye is chosen, a calibration function shall be performed (see 8.3). Depending on the effective test sample chromatic properties and the obtained calibration function, the proper dye is selected. SIST EN 16845-1:2017
EN 16845-1:2017 (E) 11 Table 1 —Dyes used in the test Dyes CAS Number IUPAC name Synonyms Empirical Formula MW max (nm) Amount (mg) for 1 L solution Methylene Blue (hydrated) 7220–79–3 3,7-bis(Dimethylamino)-phenothiazin-5-ium chloride Basic blue 9 C16H18ClN3S·x H2O where x = 3 373,90 657 187,0 Rhodamine B 81–88–9 [9-(2-carboxyphenyl)-6-diethylamino-3-xanthenylidene]-diethylammonium chloride Basic Violet 10, Brilliant Pink B, Rhodamine O, Tetraethylrhodamine C28H31ClN2O3 479,01 556 239,5 Metanil Yellow 587–98–4 3-(4-Anilinophenylazo)benzenesulfonic acid Acid Yellow 36 C18H14N3NaO3S 375,38 411 187,7 7.2 Preparation of Solutions to Spray The dye solution shall be prepared dissolving the corresponding amount of the compound (Methylene Blue, Rhodamine B or Metanil Yellow) in acetone. To facilitate the dissolution a sonicator bath is recommended. The required concentration of the dye in solution is 5x10 «4 MW (see, in Table 1, the amount needed to prepare 1 L of such a solution). The solution shall be filtered on a common laboratory filter paper (see 7.4) before transferring it into the pressurized bottle to avoid the presence of suspended solids in the bottles. 7.3 Test Samples The test sample shall be a flat material; its form shall be square (side size
· 7 cm x 7 cm) or circular (diameter
· 7 cm). The thickness of the test sample can changed as it is not relevant. The right distance from the light source to obtain the specified light power intensity as outlined in 6.4, and the right distance from the spraying gun (see below in 8.2.1) shall be fixed. This standard needs three identical test samples to be used, as three samples are needed, either for the evaluation of the dye that gives the best optical contrast (see 8.3.2), or for performing the full measurement using three dyes. 7.4 Other experimental needs Laboratory filter paper1) made of pure cellulose, about 80 g m «2, porosity from 10 20 or routine applications with funnels having a medium retention and flow rate. 8 Procedure 8.1 General Aspects 8.1.1 General This clause details the procedure for the measurement of the disappearance rate of a dye on the surface of the test sample to quantify the photocatalytic self-cleaning rate of the test sample.
1)
For example Grade I, Whatman, available in sheets. SIST EN 16845-1:2017
EN 16845-1:2017 (E) 12 8.1.2 Initial set up and calibration Initially is necessary to setup and calibrate the spraying system to obtain a regular dye spot and to evaluate the dye deposition rate. This consists in the procedure (see 8.2) for the optimization of the experimental setup. It is performed once for the initial setup of the system. The test procedure consists of two different steps: a) calibration of the change in the spectral features of the surface (see 8.1.3) of the test sample as a function of the amount of the spread dye. This calibration shall be performed for every test sample (see 8.3). b) evaluation of the change in the reflectance spectra of the test sample covered be the dye after different times under ultraviolet light (see 8.1.3). This evaluation shall be performed for every test sample (see 8.3.2). 8.1.3 Measurement of the Reflectance Spectra of the Surface The diffuse reflectance spectra of the sample surfaces shall be measured in the (400-750) nm range excluding the specular component. The reflectance spectra are measured by using a diffuse reflectance standard such as BaSO4 as a reference of 100 % reflectance material. The spectra of each sample shall be the average of at least three spectra acquired in three different places of the sample near the centre of the colour spot on the test piece. The spectra of the sample surface shall be collected before the spraying (pristine surface), along the dye covering on the test sample (calibration function development, see 8.3), after the spraying (time zero condition) and after different irradiation times (i-time condition). 8.2 Optimization of the Experimental Setup 8.2.1 General The calibration of the test apparatus shall be performed once and controlled every 200 samples have been tested. Once optimized the experimental setup is fixed. 8.2.2 Optimization of the Spraying Distance and Flow It consists in spraying a volume of a chosen dye solution (e.g. methylene blue) under the adopted conditions (tank pressure, gun model) on a white, flat and absorbing substrate (e.g. laboratory filter paper). The spraying distance and orientation between the gun and the sample shall be changed in a way to obtain a circular spot with a normal (Gaussian) distribution of the amount of dye centred in the spot of the dye on the surface. The spots obtained at different spraying distances, different spraying times and different spraying flows are compared. The optimal spraying distance, flow and optimal spraying time shall be set when a good chromatic contrast between the bare substrate and the spread surface is obtained, and normal distribution of the colour intensity at the surface is obtained. An example is reported in A.2 where the optimum distance is at 25 cm from the gun outlet and a spraying time of 12 s. 8.2.3 Measurement of the Spraying Flow Rate It consists in measuring for the experimental setup adopted under 8.2.2 the mass of water and acetone sprayed at different spraying times by using an analytical balance with sensitivity
¶ 0,001 g. Three different measurements shall be made: a) using water f
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Photocatalysis - Anti-soiling chemical activity using adsorbed organics under solid/solid
conditions - Part 1: Dyes on porous surfaces
Photocatalyse - Activité chimique anti-salissures à l’aide de matières organiques
adsorbées dans des conditions solide/solide - Partie 1 : Colorants sur des surfaces
poreuses
Ta slovenski standard je istoveten z: prEN 16845-1
ICS:
25.220.20 Površinska obdelava Surface treatment
oSIST prEN 16845-1:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 16845-1:2015
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oSIST prEN 16845-1:2015
EUROPEAN STANDARD
DRAFT
prEN 16845-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2015
ICS 25.220.20
English Version
Photocatalysis - Anti-soiling chemical activity using adsorbed
organics under solid/solid conditions - Part 1: Dyes on porous
surfaces
Photocatalyse - Activité chimique anti-salissures à l'aide de
matières organiques adsorbées dans des conditions
solide/solide - Partie 1 : Colorants sur des surfaces
poreuses
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/TC 386.
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
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 16845-1:2015 E
worldwide for CEN national Members.
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Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions .4
4 Symbols and abbreviations .5
5 Principle .5
6 Instruments .6
6.1 Spraying system .6
6.2 Analytical balance.9
6.3 Diffuse Reflectance Spectrometer .9
6.4 Light source .9
6.5 Other experimental needs .9
7 Materials .9
7.1 Dyes used .9
7.2 Preparation of Solutions to Spray. 10
7.3 Test Samples . 10
7.4 Other experimental needs . 10
8 Procedure . 10
8.1 General Aspects. 10
8.2 Optimization of the Experimental Setup. 11
8.3 Test Procedure . 12
9 Calculation . 14
9.1 General . 14
9.2 Spraying Flow (f) . 14
9.3 Dirt Parameter (DP) . 14
9.4 Covered Area (CA) . 15
9.5 Deposition Rate (DR) . 15
9.6 Standard Spraying Time . 16
9.7 Dirt Parameter (DP) Calibration Function . 16
9.8 Remaining Dye (βi) after Different Times of Irradiation . 17
9.9 Dye Half-Life . 17
10 Precision and Reproducibility . 18
11 Test Method for Samples with Low to Negligible Performance . 18
12 Test Report . 18
Annex A (informative) Typical Experimental Data . 19
A.1 Optimization of the Spraying Conditions (example) . 19
A.2 Measurement of the Spraying Mass Flows (example) . 20
A.3 Measurement of the Covered Area (example) . 21
A.4 Evaluation of the Dirt Parameter Calibration Function (example) . 23
A.5 Evaluation of the Self-cleaning Effect (example) . 25
Bibliography . 27
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Foreword
This document (prEN 16845-1:2015) has been prepared by Technical Committee CEN/TC 386
“PHOTOCATALYSIS”, the secretariat of which is held by AFNOR.
This document is currently submitted to the CEN Enquiry.
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1 Scope
This European Standard specifies a test method for the evaluation of the photocatalytic self-cleaning
performance of materials showing photocatalytic activity, usually based on semiconducting metal oxides such
as titanium dioxide, by the measurement under solid/solid conditions of the decolouring ability under
irradiation with ultraviolet light (UV-A) of a test sample on which a dye solution is sprayed and dried.
This European Standard is intended for use with opaque and rough surfaces of different kinds, such as
construction materials in flat sheet, board or plate shape, that are the basic forms of materials for various
applications.
This European Standard also applies to fabric, plastic or composites containing photocatalytic materials that
are not soluble in acetone. This European standard does not apply to photocatalytic glass, granular materials
(unless they are deposited in compact films or layers over flat solid surface) and flat non porous materials.
The method evaluates only the self-cleaning ability of the material under ultraviolet light irradiation. It cannot
be applicable to evaluate other performance attributes of photocatalytic materials, i.e., decomposition of water
contaminants in liquid or gas phases contacting the material, and antifogging and antibacterial actions.
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.
CEN/TS 16599:2014, Photocatalysis — Irradiation conditions for testing photocatalytic properties of
semiconducting materials and the measurement of these conditions
EN ISO/IEC 17025:2005, General requirements for the competence of testing and calibration laboratories
(ISO/IEC 17025:2005)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in Glossary of Photocatalytic Terms
CEN/TC386 WI00386014 and the following apply.
3.1
self-cleaning
ability of a material to maintain clean or to clean itself if soiled on its surface
3.2
photocatalytic self-cleaning
self-cleaning ability of a material as a consequence of the irradiation of the material surface with UV-Vis-IR
radiation
3.3
spraying distance
distance from the outlet of the spraying gun (see experimental setup) and the surface of the test sample
3.4
Covered Area (CA)
area of the sample where the colour intensity is ≥ exp(-2)≈ 13,5% of the maximum intensity
3.5
Dirt Parameter (DP)
measurement of the dye amount spread or persistent over the sample surface
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3.6
Dirt Parameter (DP) Calibration Function
mathematical function that describes the relation between the Dirt Parameter and the amount of dye spread
over the sample surface
4 Symbols and abbreviations
a, b, c polynomial constant parameters obtained by the fit using Formula.(7);
A (λ) Net Absorbance of the dye covering of the sample surface at the wavelength λ;
net
2
CA Covered Area (cm );
–3
C concentration of the dye in the spraying solution (g cm );
dye
–3
d density of acetone at the temperature of the measurement (g cm );
ac
DP dirt parameter (nm);
–1 2
DR deposition rate (g sec cm );
3 –1
f
volumetric spraying flow (cm sec );
-1
F mass flow (g sec );
i
k first order kinetic constant of the specified dye for the photocatalytic self-cleaning process
dye
–1
(min );
n
number of steps used for deposition of the dye on the sample surface. Typically, n=5, but
can be larger if the surface excessively wet;
Spectral Reflectance at the wavelength λ of the sample surface; R(λ) has indexes i and j
R(λ)
referring to steps of spraying and illumination, respectively;
R (λ) reflectance of the pristine surface at the wavelength λ;
background
-2
SC standard dye covering defined in Table 2 (g cm );
T
temperature in °C;
t irradiation time (min);
i
spr
spr spr
t
spraying time (sec), calculated as t = t /n;
std
W the full width at half maximum (FWHM) of the sprayed dye colour peak (cm);
–2
average covering of dye at the surface (g cm ); indexes i and j refer to steps of spraying
β
and illumination, respectively;
–2 spr
β
o
maximum average covering of dye at the surface (g cm ), obtained at t ;
std
λ wavelength (nm);
spr
standard spraying time (sec);
t
std
dye
half-life of the dye for the photocatalytic self-cleaning process (min);
τ
1/2
5 Principle
This norm concerns the comparison and the quality assurance of photocatalytic materials used as self-
cleaning materials. The method described is intended to measure the photocatalytic self-cleaning
performance of a photocatalytic material by evaluating its ability to clean its surface, previously covered by a
known amount of coloured organic compound, as a consequence of the exposition to ultraviolet light. A
controlled amount of a dye solution dissolved in a volatile solvent (acetone) is spread on the tested surface by
using a spraying gun.
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The photocatalytic material turns out to be covered by the solid dye. The relation between the amount of the
spread dye and the spectrophotometric reflectance is defined in the calibration step. The calibration function
involves the measurement of the reflectance spectra of the sample surface as a function of the dyes covering.
Dyes used in separate experiments are Metanil Yellow, Rhodamine B, and Methylene Blue. The test shallt be
carried out with the dye showing the maximum optical contrast with the material to be tested. Criteria for the
choice of the best dye are here given (see 8.3.2). Optionally, the test can be carried out with the others dyes
as the reactivity of each dye can depend on the specimen. The measurement with more than one dye is
encouraged, but it is not compulsory. The self-cleaning activity measured by this test shall be referred to the
dye used
The soiled surface is then irradiated in air by UV-A light under defined conditions and the decrease of the dye
amount on the surface is monitored by measuring the reflectance spectra of the surface of the test sample in
the visible range. By using the calibration function the change of the reflectance spectra can be related to the
kinetic of disappearance of the dye from the surface. The photocatalytic self-cleaning performance is
determined as the half-life (minutes) of the dyes applied to the surface.
6 Instruments
6.1 Spraying system
The method described in this norm is based on the possibility to cover in a controlled way the sample surface
with the dye. A spraying system shall be used to spread over the sample surface a solution of the dye (dye
solution) in volatile solvent (acetone). The spraying system consists of a sample support and in a pneumatic
system under pressure able to spray for different definite times the dye solution over the sample. The dye
solution shall be spread by using a spraying gun that forms a circular spot. This involves a normal (Gaussian)
distribution of the amount of dye centred in the spot of the dye on the surface. The amount of solution spread
spr
over the test sample is controlled by changing the spraying time (t ) with a timer that opens and closes, with
a precision of ±0,01 sec, the dye solution flow. The relative distance and orientation between the gun and the
sample shall be changed in a way to obtain a symmetric covering of the surface of the test sample and the
desired surface covered area. Due to the normal distribution of the colour intensity at the surface test piece,
the dye surface covered area is defined as the area of the sample where the colour intensity is ≥ exp(-2)≈
13,5% of the maximum intensity (see 8.2). The optimal distance from the gun outlet to the surface of the test
sample is referred as the spraying distance.
A sketch of the pneumatic spraying system and of the sample support is shown in Figure 1.
One pressurized (3,0 ± 0,1 bar) bottle containing water and at least one pressurized (3,0 ± 0,1 bar) bottle
containing the dye solution (spraying liquids) are connected to a spraying gun by tubes made of materials
resistant to the used solvent (for example PTFE (polytetrafluoroethylene)). Also the bottles and gun materials
shall be chemically inert to water and acetone. The desired spraying liquid can be selected acting on the
corresponding valves. The gun is connected to air and N pressurized lines (3,0 ± 0,1 bar) that supply the
2
atomization and the actuator gases. The actuator line is controlled by an electrovalve connected to a digital
timer. The amount of solution spread over the test sample is controlled by changing the spraying time with a
digital timer that opens and closes the actuator line with a precision of ±0,01 sec.
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Key
A (N ) Actuators (N )
2 2
A Atomization AIR
air
A Pressurized bottles
A Water
w
A Dye/Dyes solution
d
B Spraying gun
123 Digital timer
EV Electrovalve
GR Gas regulator with manometer
GT Gastap
P Pressurized AIR
air
Figure 1 — Pneumatic spraying system
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Key
A spraying gun
B sample
Arrows translation direction of the sample position
Figure 2 — Sample support
The spraying distance between the gun and the sample is typically fixed after setup of the instrumentation
(see 8.2); the test samples are placed orthogonally to the spraying flow direction. The spraying gun shall
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provide a circular sprayed spot. Using a 0,8 mm fluid nozzle orifice under the given pressure, the typical spray
distance is 200 mm. Typically, the fluid flow through the gun shall be regulated to obtain a value close to 0,2
3 –1
cm sec . For the accurate measurement of the spraying flow see 8.2.2. The atomization air flow is typically
3 –1
270±20 Ndm min .
The system shall be operated under a ventilated chemical hood. Safety precautions are taken for use of
acetone (CAS No: 67-64-1, safety glasses, good ventilation, removal of sources of ignition from the working
area).
6.2 Analytical balance
-4
An analytical balance with the precision of 10 g is used for all the gravimetric operations.
6.3 Diffuse Reflectance Spectrometer
The diffuse reflectance spectra of the sample surfaces shall be measured by using a diffuse reflectance
spectrophotometer working in the Vis wavelength range (400-750 nm) excluding the specular component. Any
commercial spectrophotometer with integrating sphere accessory can be used, including low cost instruments
having wavelength band pass ≤ 3 nm. The reflectance spectra are measured by using a diffuse reflectance
standard such as BaSO as a reference of 100% reflectance material.
4
6.4 Light source
The light source should agree with CEN/TS 16599. It shall provide UV-A irradiation within a wavelength range
of 305 nm to 380 nm for a specimen containing TiO . Suitable sources include the so-called black light (BL)
2
and black light blue (BLB) fluorescent lamps, with a maximum at 351 nm or 368 nm, and xenon arc lamps with
optical filters that block radiation below 300 nm. In the case of xenon arc lamp, a cooling system shall be
used.
The test sample shall be irradiated uniformly. The distance between the light source and the sample shall be
–2
adjusted so that the UV irradiance (300 nm to 400 nm) at the sample surface is 20 ± 0,5 W m . A UV
radiometer in conformity with CEN/TS 16599 shall be put at the same distance as the surface of the test
sample to be tested. The irradiance along the length of the test sample shall also be constant within ±5%. The
temperature of the sample during the test shall be 25±5 °C.
6.5 Other experimental needs
a) A bottle with a neck diameter larger than the spot dye spot size, as determined under 2) in 8.2.3.
b) Ventilated chemical hood.
c) Sonication bath
d) Safety glasses.
7 Materials
7.1 Dyes used
Three different dyes can be used in the test (see Table 1). The dyes shall be dissolved in acetone (2-
propanone), a volatile organic solvent that allows a perfect solubilisation of the dyes. The dyes have different
optical contrast on the test sample depending on their colour. When a dye is chosen, a calibration function
shall be performed (see 8.3). Depending on the effective test sample chromatic properties and the obtained
calibration function, the proper dye is selected.
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Table 1 —Dyes used in the test
Dyes CAS IUPAC name Synonyms Empirical Molecul Maximu Amoun
Number Formula ar m t (mg)
weight, absorban for
g/mol ce (λ , prepari
max
nm) ng 1 L
solutio
n
Methylene 7220-79-3 3,7- Basic blue 9 C H ClN S 373,90 657 187,0
16 18 3
Blue bis(Dimethylamino)
-phenothiazin-5-
(non
ium chloride
hydrated)
Rhodamine B 81-88-9 [9-(2- Basic Violet 10, C H ClN O 479,01 556 239,5
28 31 2 3
carboxyphenyl)-6- Brilliant Pink B,
diethylamino-3- Rhodamine O,
xanthenylidene]- Tetraethylrhoda
diethylammonium mine
chloride
Metanil
587-98-4 3-(4- Acid Yellow 36 C H N NaO 375,38 411 187,7
18 14 3 3
Yellow Anilinophenylazo)b S
enzenesulfonic
acid
7.2 Preparation of Solutions to Spray
The dye solution shall be prepared dissolving the corresponding amount of the compound (Methylene Blue,
Rhodamine B or Metanil Yellow) in acetone. To facilitate the dissolution a sonicator bath is recommended.
–4
The required concentration of the dye in solution is 5x10 M (see Table 1). The solution shall be filtered on a
common laboratory filter paper (see 7.4) before transferring it into the pressurized bottle to avoid the presence
of suspended solids in the bottles.
7.3 Test Samples
The test sample shall be a flat material; its form shall be square (side size ≥ 7x7 cm) or circular (diameter ≥ 7
cm). The thickness of the test sample can change as it is not relevant. The right distance from the light source
to obtain the specified light power intensity as outlined in 6.4 , and the right distance from the spraying gun
(see below in 8.2.1) shall be fixed. This norm needs 3 identical test samples to be used, as 3 samples are
needed, either for the evaluation of the dye that gives the best optical contrast (see 8.3.2), or for performing
the full measurement using 3 dyes.
7.4 Other experimental needs
-2
1
Laboratory filter paper made of pure cellulose, about 80 g m , porosity 10-20 μm, for routine applications
with funnels having a medium retention and flow rate.
8 Procedure
8.1 General Aspects
8.1.1 General
This clause details the procedure for the measurement of the disappearance rate of a dye on the surface of
the test sample to quantify the photocatalytic self-cleaning rate of the test sample.
)
1
for example Grade I, Whatman, available in sheets.
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8.1.2 Initial set up and calibration
Initially is necessary to setup and calibrate the spraying system to obtain a regular dye spot and to evaluate
the dye deposition rate. This consists in the procedure (see 8.2) for the optimization of the experimental setup.
It is performed once for the initial setup of the system.
The test procedure consists of two different steps:
a) calibration of the change in the spectral features of the surface (see 8.1.3) of the test sample as a
function of the amount of the spread dye. This calibration shall be performed for every test sample (see
8.3).
b) evaluation of the change in the reflectance spectra of the test sample covered be the dye after different
times under ultraviolet light (see 8.1.3). This evaluation shall be performed for every test sample (see
8.3.2).
8.1.3 Measurement of the Reflectance Spectra of the Surface
The diffuse reflectance spectra of the sample surfaces shall be measured in the 400-750 nm range excluding
the specular component. The reflectance spectra are measured by using a diffuse reflectance standard such
as BaSO as a reference of 100% reflectance material. The spectra of each sample shall be the average of at
4
least three spectra acquired in three different place of the sample near the centre of the colour spot on the test
piece. The spectra of the sample surface shall be collected before the spraying (pristine surface), along the
dye covering on the test sample (calibration function development, see 8.3), after the spraying (time zero
condition) and after different irradiation times (i-time condition).
8.2 Optimization of the Experimental Setup
8.2.1 General
The calibration of the test apparatus shall be performed once and controlled every 200 samples have been
tested. Once optimized the experimental setup is fixed.
8.2.2 Optimization of the Spraying Distance and Flow
It consists in spraying a volume of a chosen dye solution (e.g. methylene blue) under the adopted conditions
(tank pressure, gun model) on a white, flat and absorbing substrate (e.g. laboratory filter paper).
The spraying distance and orientation between the gun and the sample shall be changed in a way to obtain a
circular spot with a normal (Gaussian) distribution of the amount of dye centred in the spot of the dye on the
surface. The spots obtained at different spraying distances, different spraying times and different spraying
flows are compared. The optimal spraying distance, flow and optimal spraying time shall be set when a good
chromatic contrast between the bare substrate and the spread surface is obtained, and normal distribution of
the colour intensity at the surface is obtained. An example is reported in A.1 where the optimum distance is at
25 cm from the gun outlet and a spraying time of 12 sec.
8.2.3 Measurement of the Spraying Flow Rate
It consists in measuring for the experimental setup adopted under 8.2.2 the mass of water and acetone
sprayed at different spraying times by using an analytical balance with sensitivity ≤ 0,001 g. Three different
measurements shall be made:
1) using water from Tank A (see Figure 1), the water is recovered in a vial positioned near as possible to the
outlet of the gun to recover all the flow from the gun;
2) using water from Tank A (see Figure 1), the water is recovered in a bottle located in place of the sample
at the spraying distance adopted under 8.2.2. The bottle shall have a neck of proper diameter to collect
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the whole net spray reaching the sample. The bottle neck diameter shall be larger than the spot diameter
previously determined (see above 8.2.2). A typical value is 1,70 times the full width at half maximum
(FWHM) of the spot colour (±2σ) (see below 8.2.4). The internal walls of the bottle are covered by
laboratory filter paper, and its bottom filled with facial tissue paper, in such a way to completely absorb
the water spray entering through the bottle neck.
3) using acetone from Tank B (see Figure 1), the acetone is recovered in a vial positioned near as possible
to the outlet of the gun to recover all the flow from the gun. The measurement of the acetone recovered at
the spraying distance is discouraged because the easy volatilization.
The net content of the bottle or the vials in each of the above steps 1)-3) is measured gravimetrically by an
analytical balance. The amount sprayed is measured at least at 4 different spraying times each lasting 1-6
seconds. The duration of this spraying time has to allo
...
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