Reference test method for release of nickel from those parts of spectacle frames and sunglasses intended to come into close and prolonged contact with the skin

This European Standard specifies a method for simulating the release of nickel from those parts of spectacle frames and sunglasses intended to come into direct and prolonged contact with the skin in order to determine whether they release nickel at a rate greater than 0,5 µg/cm2/week.
NOTE 1   This European Standard, EN 16128, has been prepared in reply to the European Commission's Mandate M/448 addressed to CEN. From the technical point of view, this European Standard provides an unchanged re-publication of the technical requirements that had previously been specified in EN 1811:1998, but restricted in scope to apply only to spectacle frames and sunglasses.
NOTE 2   Users of this European Standard may wish to note that, also in reply to the European Commission's Mandate M/448, this European Standard is currently subject to review with the objective of developing a new standardized method to supersede this European Standard when the new method becomes available.
NOTE 3   Nickel release testing of products other than spectacle frames and sunglasses is specified in prEN 1811:2009.

Referenzprüfverfahren zur Bestimmung der Nickellässigkeit derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß unmittelbar und länger mit der Haut in Berührung kommen

Diese Europäische Norm legt ein Verfahren fest, um die Nickelabgabe derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß in direkten und länger andauernden Kontakt mit der Haut zu kommen, zu simulieren, und um zu bestimmen, ob ihre Nickelabgabe größer als 0,5 µg/cm2/Woche ist.
ANMERKUNG 1   Diese Europäische Norm, FprEN 16128, wurde vom CEN aufgrund des Mandats M/448 der Europäischen Kommission erstellt. In technischer Hinsicht handelt es sich bei dieser Europäischen Norm um eine unveränderte Neuherausgabe der technischen Anforderungen, die bisher in EN 1811:1998 enthalten waren, wobei jedoch der Anwendungsbereich auf die Anwendung auf Brillenfassungen und Sonnenbrillen eingeschränkt wurde.
ANMERKUNG 2   Die Anwender dieser Europäischen Norm werden darauf hingewiesen, dass diese Europäische Norm – ebenfalls aufgrund des Mandats M/448 der Europäischen Kommission – derzeit einer Überprüfung unterzogen wird. Das Ziel ist, ein neues genormtes Prüfverfahren zu entwickeln, das diese Europäische Norm ersetzen wird, sobald die Erarbeitung abgeschlossen wurde.
ANMERKUNG 3   Die Bestimmung der Nickellässigkeit von anderen Gegenständen als Brillenfassungen und Sonnen¬brillen ist in prEN 1811:2009 festgelegt.

Méthode d'essai de référence relative à la libération du nickel par les parties des montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peau

La présente Norme européenne spécifie une méthode pour simuler la libération du nickel par les parties des
montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peau dans
le but de déterminer si elles libèrent du nickel à un taux supérieur à 0,5 µg/cm2/semaine.
NOTE 1 La présente Norme européenne, EN 16128, a été élaborée en réponse au Mandat M/448 de la Commission
Européenne adressé au CEN. Du point de vue technique, cette Norme européenne correspond à la publication sans
modification des exigences techniques précédemment spécifiées dans l’EN 1811:1998, mais le domaine d’application a
été restreint pour s’appliquer uniquement aux montures de lunettes et lunettes de soleil.
NOTE 2 Les utilisateurs de la présente Norme européenne sont informés que la présente Norme européenne est
actuellement soumise à une révision, également en réponse au Mandat M/448 de la Commission Européenne, dans le but
d’élaborer une nouvelle méthode normalisée destinée à remplacer la présente Norme européenne dès qu’elle sera
disponible.
NOTE 3 Les essais de libération de nickel par d’autres produits que les montures de lunettes et lunettes de soleil sont
spécifiés dans l’EN 1811:2011.

Primerjalna preskusna metoda za sproščanje niklja iz tistih delov okvirjev očal in sončnih očal, ki so predvideni za neposredni in daljši stik s kožo

Ta evropski standard določa metodo za posnemanje sproščanja niklja iz tistih delov okvirjev očal in sončnih očal, ki so predvideni za neposredni in daljši stik s kožo, s katero se ugotavlja, ali sproščajo nikelj s hitrostjo, ki presega 0,5 µg/cm2/teden.
OPOMBA 1: Ta evropski standard FprEN 16128 je pripravljen kot odgovor na pooblastilo Evropske komisije M/448, namenjen CEN. S tehničnega vidika ta evropski standard zagotavlja nespremenjeno ponovno objavo tehničnih zahtev, predhodno določenih v EN 1811:1998, vendar je omejen glede obsega uporabe, tako da velja samo za okvire za očala in sončna očala.
OPOMBA 2: Uporabniki tega evropskega standarda lahko opazijo, da se ta evropski standard tudi kot odziv na pooblastilo Evropske komisije M/448 trenutno preučuje zato, da bi se razvila nova standardizirana metoda, ki bo nadomestila ta evropski standard, ko bo nova metoda na voljo.
OPOMBA 3: Preskušanje sproščanja niklja iz proizvodov, ki niso okvirji za očala in sončna očala, določa prEN 1811:2009.

General Information

Status
Withdrawn
Publication Date
08-Mar-2011
Withdrawal Date
03-Nov-2015
Technical Committee
Current Stage
9960 - Withdrawal effective - Withdrawal
Completion Date
04-Nov-2015

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RReferenzprüfverfahren zur Bestimmung der Nickellässigkeit derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß unmittelbar und länger mit der Haut in Berührung kommenMéthode d'essai de référence relative à la libération du nickel par les parties des montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peauReference test method for release of nickel from those parts of spectacle frames and sunglasses intended to come into close and prolonged contact with the skin11.040.70Oftalmološka opremaOphthalmic equipmentICS:Ta slovenski standard je istoveten z:EN 16128:2011SIST EN 16128:2011en,fr,de01-september-2011SIST EN 16128:2011SLOVENSKI

STANDARDSIST EN 1811:1999+A1:20081DGRPHãþD
SIST EN 16128:2011
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16128
March 2011 ICS 11.040.70 Supersedes EN 1811:1998+A1:2008English Version

Reference test method for release of nickel from those parts of spectacle frames and sunglasses intended to come into close and prolonged contact with the skin

Méthode d'essai de référence relative à la libération du nickel par les parties des montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peau

Referenzprüfverfahren zur Bestimmung der Nickellässigkeit derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß unmittelbar und länger mit der Haut in Berührung kommen This European Standard was approved by CEN on 9 January 2011.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,

B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16128:2011: ESIST EN 16128:2011

EN 16128:2011 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41Scope ......................................................................................................................................................52Principle ..................................................................................................................................................53Reagents .................................................................................................................................................54Apparatus ...............................................................................................................................................65Samples ..................................................................................................................................................75.1Sample area ............................................................................................................................................75.1.1Definition of sample area ......................................................................................................................75.1.2Determination of sample area ..............................................................................................................75.1.3Areas other than sample areas ............................................................................................................75.2Sample preparation ...............................................................................................................................75.3Reference disc .......................................................................................................................................76Procedure ...............................................................................................................................................86.1Preparation of test solution ..................................................................................................................86.2Release procedure .................................................................................................................................86.3Determination of nickel .........................................................................................................................86.4Number of replicates .............................................................................................................................86.5Blank tests ..............................................................................................................................................97Calculations ............................................................................................................................................97.1Nickel release .........................................................................................................................................97.2Interpretation of results ........................................................................................................................98Test report ..............................................................................................................................................9Annex A (informative)

Statistical uncertainty of the test procedure and interpretation of results ......... 11Annex B (informative)

Rules for production and preparation of reference material ................................. 13Annex C (informative)

Identification and determination of sample area; and coating of non-significant areas.................................................................................................................................. 15C.1Identification and determination of sample area ............................................................................. 15C.2Coating of non-significant areas ....................................................................................................... 15Annex D (informative)

Articles made from materials that can release small amounts of nickel ............. 16Bibliography ..................................................................................................................................................... 17 SIST EN 16128:2011

EN 16128:2011 (E) 3 Foreword This document (EN 16128:2011) has been prepared by Technical Committee CEN/TC 170 “Ophthalmic optics”, the secretariat of which is held by DIN. 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 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. 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. This document, together with EN 1811:2011, supersedes EN 1811:1998+A1:2008. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document supports essential requirements of Commission Regulation (EC) No 1907/2006 (REACH) of the European Parliament and the Council. List of the significant technical changes that have been made in this new version of EN 1811 in comparison with the former edition EN 1811:1998+A1:2008: The scope of the former European Standard was divided: EN 1811:2011 is applicable for all products but spectacle frames and sunglasses; EN 16128:2011 is applicable for spectacle frames and sunglasses; List of the significant technical changes of EN 1811:2011 as compared to the former European Standard: • The scope was expanded to include all post assemblies which are inserted into pierced parts of the human body; • The preparation of the test solution was tested and changed; • The correction factor was eliminated and the concept of measurement uncertainty introduced; • The Standard contains a new normative Annex C on the preparation of articles prior to nickel testing; EN 16128:2011 is technically unchanged as compared to the former European Standard EN 1811:1998+A1:2008. 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 16128:2011

EN 16128:2011 (E) 4 Introduction Adverse skin reaction to nickel has been known for many decades. Nickel is now the most frequent cause of contact allergy in Europe, and 10 % to 20 % of the female population is allergic to nickel. Skin absorption of nickel ions, which are released from some nickel-containing materials in direct and prolonged contact with the skin, causes sensitisation. Further exposure to soluble nickel salts results in allergic contact dermatitis. It is known that sensitisation to nickel requires higher exposure levels than does the elicitation in already sensitised individuals. There is a large variation in the degree of sensitivity to nickel between individuals. This widespread health problem has forced the urgent introduction of a number of measures designed to reduce its prevalence. They include this standard which attempts to provide an in-vitro chemical test that correlates as far as possible with the variable human biological reactions that occur when metallic articles containing nickel are in direct and prolonged contact with the skin. The standard provides a measure of the amount of nickel release from an article immersed for one week in artificial sweat. It is a first attempt at the standardisation of a test method that previously has been used in research, and it is expected to require early revision in the light of further experience. The standard also describes the preparation of a reference material intended to assist a laboratory in achieving an acceptable precision. Clinical patch-testing of a small selection of nickel-containing alloys and coatings on nickel-sensitized persons indicates that high and low results achieved with the present analytical method correspond closely with patch-test reactivity. Moreover, a nickel release rate threshold of 0,5 µg/cm2/week has been set in European Parliament and Council Directive 94/27/EC (OJ No. L188 of 22.7.94). In order to ensure that articles yielding values near this figure are not unnecessarily excluded from European trade as a result of the difficulties inherent in the test method, particularly when applied to intricately-shaped articles, the measured release figures are multiplied by a factor of 0,1. Materials recognized as causing sensitisation to nickel would not become acceptable by use of this adjustment. Application of this standard is confidently expected to reduce significantly the development of allergic contact dermatitis due to nickel. Experience of its use and further epidemiological and clinical research may justify changes to test procedure and/or interpretation of the test result. SIST EN 16128:2011

EN 16128:2011 (E) 5 1 Scope This European Standard specifies a method for simulating the release of nickel from those parts of spectacle frames and sunglasses intended to come into direct and prolonged contact with the skin in order to determine whether they release nickel at a rate greater than 0,5 µg/cm2/week. NOTE 1 This European Standard, EN 16128, has been prepared in reply to the European Commission's Mandate M/448 addressed to CEN. From the technical point of view, this European Standard provides an unchanged re-publication of the technical requirements that had previously been specified in EN 1811:1998, but restricted in scope to apply only to spectacle frames and sunglasses.

NOTE 2 Users of this European Standard may wish to note that, also in reply to the European Commission's Mandate M/448, this European Standard is currently subject to review with the objective of developing a new standardized method to supersede this European Standard when the new method becomes available. NOTE 3 Nickel release testing of products other than spectacle frames and sunglasses is specified in EN 1811:2011.

2 Principle The parts to be tested for nickel release are placed in an artificial sweat test solution for 1 week. The concentration of dissolved nickel in the solution is determined by atomic absorption spectrometry, inductively-coupled plasma spectrometry or other appropriate analytical method. The nickel release is expressed in micrograms per square centimetre per week (µg/cm2/week). 3 Reagents Except where indicated, all reagents shall be of recognized pro analysis, p.a., grade or better and shall be free of nickel. 3.1 Deionized and aerated water. Fill a tall-form 2-l beaker with deionized water, specific conductivity max. 1 µS/cm. Saturate with air by attaching a gas distribution tube (porosity 1) to a cork and positioning the lower end of the tube on the bottom of the beaker. Allow grease-free air to flow at a rate of 150 ml/min. for 30 min. 3.2 Sodium chloride. 3.3 DL-Lactic acid, ρ = 1,21 g/ml, >88 % (m/m). 3.4 Urea. 3.5 Ammonia solution, ρ = 0,91 g/ml, 25 % (m/m). 3.6 Dilute ammonia solution, 1 % (m/m). Transfer 10 ml of ammonia solution (3.5) into a 250-ml beaker containing 100 ml of deionized water. Stir and cool to room temperature. Transfer the solution to a 250-ml volumetric flask and make up to volume with deionized water. 3.7 Nitric acid, ρ = 1,40 g/ml, 65 % (m/m). 3.8 Dilute nitric acid, approximately 5 % (m/m). Transfer 30 ml of nitric acid (3.7) into a 500-ml beaker containing 350 ml of deionized water. Stir and cool to room temperature. Transfer the solution to a 500-ml volumetric flask and make up to volume with deionized water. SIST EN 16128:2011

EN 16128:2011 (E) 6 3.9 Degreasing solution. Dissolve 5 g of an anionic surface-active agent such as sodium dodecylbenzene sulfonate or sodium alkylaryl sulfonate in 1 000 ml water. An appropriately-diluted, neutral, commercially-available detergent may be used. 3.10 Wax or lacquer (suitable for electroplating purposes) capable of protecting a surface from nickel release. The wax or lacquer shall be shown to prevent nickel release from a nickel-releasing surface when one or more coats of the wax or lacquer are applied in the same manner as on a test sample, and tested for nickel release according to Clause 6 (see Annex C). 4 Apparatus 4.1 A pH-meter, accurate to ± 0,02 pH. 4.2 An analytical spectrometer capable of detecting a concentration of 0,01 mg nickel per litre. The instrument shall, after optimization, meet the performance criteria given in 4.2.1 and 4.2.2. It is recommended that either an inductively-coupled plasma − optical emission spectrometer or an electrothermal excitation atomic absorption spectrometer is used. 4.2.1 Minimum precision. The standard deviation of 10 measurements of the absorption of a full matrix calibration solution containing 0,05 mg nickel per litre shall not exceed 10 %. 4.2.2 Limit of detection. The limit of detection shall be considered as twice the standard deviation of 10 measurements of the absorbance of a full matrix solution containing nickel at a concentration level selected to give an absorbance just above that of the zero calibration solution. The limit of detection of nickel in a matrix similar to the final test solution shall be better than 0,01 mg/l. 4.3 Thermostatically controlled water-bath or oven, capable of maintaining a temperature of (30 ± 2) °C. 4.4 A vessel with lid, both composed of a non-metallic, nickel-free and nitric-acid-resistant material, such as glass and/or polypropylene and/or polytetrafluoroethylene and/or polystyrene. The sample shall be suspended in the liquid by a holder made from the same materials as listed above, so as to minimize contact of the sample area (5.1.1) with the walls and base of the vessel. The size and shape of vessel and holder shall be chosen so as to minimize the volume of test solution required to completely cover the object to be tested. In order to remove any trace of nickel, the vessel and holder shall be pre-treated by being stored in a solution of dilute nitric acid (3.8) for at least 4 h. After acid treatment, rinse the vessel and holder with deionized water and dry. SIST EN 16128:2011

EN 16128:2011 (E) 7 5 Samples 5.1 Sample area 5.1.1 Definition of sample area Only the surface(s) of those parts of spectacle frames or sunglasses (referred to hereafter as "frames") liable to come into direct and prolonged contact with the skin 1) shall be analyzed. In this standard such surfaces are defined as "sample area". 5.1.2 Determination of sample area Determination of the sample area (a) in square centimetres is achieved by marking the contour of the sample area defined in 5.1.1 (see Annex C). In order to achieve the required degree of analytical sensitivity, a minimum sample area of 0,2 cm2 shall be tested. If necessary, identical items may be treated together to obtain this minimum area. NOTE If a frame is being tested to ascertain its conformity with Directive 94/27/EC, the accuracy with which the sample area of the frame or part has to be determined is dependent on the nickel release of the frame or part. The closer the nickel release is to 0,5 µg/cm2/week, the limit laid down in the directive, the more accurately the surface area has to be determined. 5.1.3 Areas other than sample areas In order to prevent release of nickel from areas other than the sample area, such areas shall be removed or protected from the test solution. This may be achieved after degreasing (see 5.2) by, for example, the application of one or more coatings of a wax or lacquer which has been shown to protect from nickel release (3.10). Annex C gives guidance on the coating of protected areas prior to testing. Where it is not feasible to remove or protect all areas other than the sample area, for example with certain watch bracelets, such unprotected surfaces shall be considered as part of the sample area.

NOTE If, when non-significant surfaces are considered to be part of the sample area, the nickel release from the frame is found to be unacceptable, consideration should be given to dismantling the frame and testing any internal components for nickel release. If the nickel release from such internal components is si

...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.RReferenzprüfverfahren zur Bestimmung der Nickellässigkeit derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß unmittelbar und länger mit der Haut in Berührung kommenMéthode d'essai de référence relative à la libération du nickel par les parties des montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peauReference test method for release of nickel from those parts of spectacle frames and sunglasses intended to come into close and prolonged contact with the skin11.040.70Oftalmološka opremaOphthalmic equipmentICS:Ta slovenski standard je istoveten z:FprEN 16128kSIST FprEN 16128:2010en,fr,de01-september-2010kSIST FprEN 16128:2010SLOVENSKI

STANDARD
kSIST FprEN 16128:2010
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN 16128
July 2010 ICS
Will supersede EN 1811:1998+A1:2008English Version

Reference test method for release of nickel from those parts of spectacle frames and sunglasses intended to come into close and prolonged contact with the skin

Méthode d'essai de référence relative à la libération du nickel par les parties des montures de lunettes et lunettes de soleil destinées à entrer en contact direct et prolongé avec la peau

Referenzprüfverfahren zur Bestimmung der Nickellässigkeit derjenigen Teile von Brillenfassungen und Sonnenbrillen, die bestimmungsgemäß unmittelbar und länger mit der Haut in Berührung kommen This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/TC 170.

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 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

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
Management Centre:
Avenue Marnix 17,

B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. FprEN 16128:2010: EkSIST FprEN 16128:2010

FprEN 16128:2010 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41Scope ......................................................................................................................................................52Principle ..................................................................................................................................................53Reagents .................................................................................................................................................54Apparatus ...............................................................................................................................................65Samples ..................................................................................................................................................76Procedure ...............................................................................................................................................87Calculations ............................................................................................................................................98Test report ..............................................................................................................................................9Annex A (informative)

Statistical uncertainty of the test procedure and interpretation of results ......... 11Annex B (informative)

Rules for production and preparation of reference material ................................. 13Annex C (informative)

Identification and determination of sample area; and coating of non-significant areas.................................................................................................................................. 15Annex D (informative)

Articles made from materials that can release small amounts of nickel ............. 16Bibliography ..................................................................................................................................................... 17 kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 3 Foreword This document (FprEN 16128:2010) has been prepared by Technical Committee CEN/TC 170 “Ophthalmic optics”, the secretariat of which is held by DIN. This document is currently submitted to the Unique Acceptance Procedure. This document, together with prEN 1811:2009, supersedes EN 1811:1998+A1:2008.

This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of Commission Regulation (EC) No 1907/2006 (REACH) of the European Parliament and the council.

kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 4 Introduction Adverse skin reaction to nickel has been known for many decades. Nickel is now the most frequent cause of contact allergy in Europe, and 10 % to 20 % of the female population is allergic to nickel. Skin absorption of nickel ions, which are released from some nickel-containing materials in direct and prolonged contact with the skin, causes sensitisation. Further exposure to soluble nickel salts results in allergic contact dermatitis. It is known that sensitisation to nickel requires higher exposure levels than does the elicitation in already sensitised individuals. There is a large variation in the degree of sensitivity to nickel between individuals. This widespread health problem has forced the urgent introduction of a number of measures designed to reduce its prevalence. They include this standard which attempts to provide an in-vitro chemical test that correlates as far as possible with the variable human biological reactions that occur when metallic articles containing nickel are in direct and prolonged contact with the skin. The standard provides a measure of the amount of nickel release from an article immersed for one week in artificial sweat. It is a first attempt at the standardisation of a test method that previously has been used in research, and it is expected to require early revision in the light of further experience. The standard also describes the preparation of a reference material intended to assist a laboratory in achieving an acceptable precision. Clinical patch-testing of a small selection of nickel-containing alloys and coatings on nickel-sensitized persons indicates that high and low results achieved with the present analytical method correspond closely with patch-test reactivity. Moreover, a nickel release rate threshold of 0,5 µg/cm2/week has been set in European Parliament and Council Directive 94/27/EC (OJ No. L188 of 22.7.94). In order to ensure that articles yielding values near this figure are not unnecessarily excluded from European trade as a result of the difficulties inherent in the test method, particularly when applied to intricately-shaped articles, the measured release figures are multiplied by a factor of 0,1. Materials recognized as causing sensitisation to nickel would not become acceptable by use of this adjustment. Application of this standard is confidently expected to reduce significantly the development of allergic contact dermatitis due to nickel. Experience of its use and further epidemiological and clinical research may justify changes to test procedure and/or interpretation of the test result. kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 5 1 Scope This European Standard specifies a method for simulating the release of nickel from those parts of spectacle frames and sunglasses intended to come into direct and prolonged contact with the skin in order to determine whether they release nickel at a rate greater than 0,5 µg/cm2/week. NOTE 1 This European Standard, FprEN 16128, has been prepared in reply to the European Commission's Mandate M/448 addressed to CEN. From the technical point of view, this European Standard provides an unchanged re-publication of the technical requirements that had previously been specified in EN 1811:1998, but restricted in scope to apply only to spectacle frames and sunglasses.

NOTE 2 Users of this European Standard may wish to note that, also in reply to the European Commission's Mandate M/448, this European Standard is currently subject to review with the objective of developing a new standardized method to supersede this European Standard when the new method becomes available. NOTE 3 Nickel release testing of products other than spectacle frames and sunglasses is specified in prEN 1811:2009.

2 Principle The parts to be tested for nickel release are placed in an artificial sweat test solution for 1 week. The concentration of dissolved nickel in the solution is determined by atomic absorption spectrometry, inductively-coupled plasma spectrometry or other appropriate analytical method. The nickel release is expressed in micrograms per square centimetre per week (µg/cm2/week). 3 Reagents Except where indicated, all reagents shall be of recognized pro analysis, p.a., grade or better and shall be free of nickel. 3.1 Deionized and aerated water

Fill a tall-form 2-l beaker with deionized water, specific conductivity max. 1 µS/cm. Saturate with air by attaching a gas distribution tube (porosity 1) to a cork and positioning the lower end of the tube on the bottom of the beaker. Allow grease-free air to flow at a rate of 150 ml/min. for 30 min. 3.2 Sodium chloride 3.3 3 DL-Lactic acid, ρ = 1,21 g/ml, >88 % (m/m) 3.4 Urea 3.5 Ammonia solution, ρ = 0,91 g/ml, 25 % (m/m) 3.6 Dilute ammonia solution, 1 % (m/m)

Transfer 10 ml of ammonia solution (3.5) into a 250-ml beaker containing 100 ml of deionized water. Stir and cool to room temperature. Transfer the solution to a 250-ml volumetric flask and make up to volume with deionized water. 3.7 Nitric acid, ρ = 1,40 g/ml, 65 % (m/m) 3.8 Dilute nitric acid, approximately 5 % (m/m)

Transfer 30 ml of nitric acid (3.7) into a 500-ml beaker containing 350 ml of deionized water. Stir and cool to kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 6 room temperature. Transfer the solution to a 500-ml volumetric flask and make up to volume with deionized water. 3.9 Degreasing solution

Dissolve 5 g of an anionic surface-active agent such as sodium dodecylbenzene sulfonate or sodium alkylaryl sulfonate in 1000 ml water. An appropriately-diluted, neutral, commercially-available detergent may be used. 3.10 Wax or lacquer (suitable for electroplating purposes) capable of protecting a surface from nickel release

The wax or lacquer shall be shown to prevent nickel release from a nickel-releasing surface when one or more coats of the wax or lacquer are applied in the same manner as on a test sample, and tested for nickel release according to Clause 6 (see Annex C). 4 Apparatus 4.1 A pH-meter, accurate to ± 0,02 pH 4.2 An analytical spectrometer capable of detecting a concentration of 0,01 mg nickel per litre. The instrument shall, after optimization, meet the performance criteria given in 4.2.1 and 4.2.2. It is recommended that either an inductively-coupled plasma − optical emission spectrometer or an electrothermal excitation atomic absorption spectrometer is used. 4.2.1 Minimum precision

The standard deviation of 10 measurements of the absorption of a full matrix calibration solution containing 0,05 mg nickel per litre shall not exceed 10 %. 4.2.2 Limit of detection

The limit of detection shall be considered as twice the standard deviation of 10 measurements of the absorbance of a full matrix solution containing nickel at a concentration level selected to give an absorbance just above that of the zero calibration solution. The limit of detection of nickel in a matrix similar to the final test solution shall be better than 0,01 mg/l. 4.3 Thermostatically controlled water-bath or oven, capable of maintaining a temperature of (30 ± 2) °C. 4.4 A vessel with lid, both composed of a non-metallic, nickel-free and nitric-acid-resistant material, such as glass and/or polypropylene and/or polytetrafluoroethylene and/or polystyrene. The sample shall be suspended in the liquid by a holder made from the same materials as listed above, so as to minimize contact of the sample area (5.1.1) with the walls and base of the vessel. The size and shape of vessel and holder shall be chosen so as to minimize the volume of test solution required to completely cover the object to be tested. In order to remove any trace of nickel, the vessel and holder shall be pre-treated by being stored in a solution of dilute nitric acid (3.8) for at least 4 h. After acid treatment, rinse the vessel and holder with deionized water and dry. kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 7 5 Samples 5.1 Sample area 5.1.1 Definition of sample area Only the surface(s) of those parts of spectacle frames or sunglasses (referred to hereafter as "frames") liable to come into direct and prolonged contact with the skin 1) shall be analyzed. In this standard such surfaces are defined as "sample area". 5.1.2 Determination of sample area Determination of the sample area (a) in square centimetres is achieved by marking the contour of the sample area defined in 5.1.1 (see Annex C). In order to achieve the required degree of analytical sensitivity, a minimum sample area of 0,2 cm2 shall be tested. If necessary, identical items may be treated together to obtain this minimum area. NOTE If a frame is being tested to ascertain its conformity with Directive 94/27/EC, the accuracy with which the sample area of the frame or part has to be determined is dependent on the nickel release of the frame or part. The closer the nickel release is to 0,5 µg/cm2/week, the limit laid down in the directive, the more accurately the surface area has to be determined. 5.1.3 Areas other than sample areas In order to prevent release of nickel from areas other than the sample area, such areas shall be removed or protected from the test solution. This may be achieved after degreasing (see 5.2) by, for example, the application of one or more coatings of a wax or lacquer which has been shown to protect from nickel release (3.10). Annex C gives guidance on the coating of protected areas prior to testing. Where it is not feasible to remove or protect all areas other than the sample area, for example with certain watch bracelets, such unprotected surfaces shall be considered as part of the sample area.

NOTE If, when non-significant surfaces are considered to be part of the sample area, the nickel release from the frame is found to be unacceptable, consideration should be given to dismantling the frame and testing any internal components for nickel release. If the nickel release from such internal components is significant it might be appropriate to test the external components on their own, assuming that they are available, or the materials from which the frame has been manufactured (see Annex D). 5.2 Sample preparation Gently swirl the sample for 2 min in degreasing solution (3.9) at room temperature. Rinse thoroughly with deionized water and dry. After degreasing, items should be handled with plastic forceps or clean protective gloves. NOTE This cleaning stage is intended to remove extraneous grease and skin secretions due to handling, but not any protective coatings. However, it will also substantially remove any nickel contamination that might be present on the surface of the sample. If there is a requirement to determine this nickel the cleaning stage should be omitted. However, it should be appreciated that omission of this cleaning stage might itself affect the nickel release from the sample. 5.3 Reference disc As a quality control check, the nickel release from a reference disc may be determined (see Annex A and Annex B).

1) See EN ISO 12870 for guidance. kSIST FprEN 16128:2010

FprEN 16128:2010 (E) 8 If used, it is important that both sides of a reference disc are abraded before each test. A minimum of 0,05 mm shall be abraded from each surface using wet emery paper No. 600 followed by No. 1200. The disc is then degreased in the same way as the sample (5.2). 6 Procedure 6.1 Preparation of test solution The test solution representing artificial sweat consists of deionized and aerated water (3.1) containing:  0,5 % (m/m) sodium chloride (3.2);

 0,1 % (m/m) lactic acid (3.3);
 0,1 % (m/m)
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