Avis juridique important

|

32002L0053

Council Directive 2002/53/EC of 13 June 2002 on the common catalogue of varieties of agricultural plant species

Official Journal L 193 , 20/07/2002 P. 0001 - 0011

Council Directive 2002/53/ECof 13 June 2002on the common catalogue of varieties of agricultural plant speciesTHE COUNCIL OF THE EUROPEAN UNION,Having regard to the Treaty establishing the European Community, and in particular Article 37 thereof,Having regard to the proposal from the Commission,Having regard to the Opinion of the European Parliament(1),Having consulted the Economic and Social Committee,Whereas:(1) Council Directive 70/457/EEC of 29 September 1970 on the common catalogue of varieties of agricultural plant species(2) has been frequently and substantially amended(3). For reasons of clarity and rationality the said Directive should be codified.(2) The production of agricultural seed and young plants occupies an important place in the agriculture of the Community.(3) For this reason, the Council has adopted Directives concerning respectively the marketing of beet seed (2002/54/EC)(4), fodder plant seed (66/401/EEC)(5), cereal seed(6), seed potatoes (2002/56/EC)(7) and seed of oil and fibre plants (2002/57/EC)(8).(4) A common catalogue of varieties needs to be compiled. This catalogue can be compiled only on the basis of national catalogues.(5) All Member States should therefore compile one or more national catalogues of the varieties accepted for certification and marketing in their territory.(6) These catalogues must be drawn up in accordance with uniform rules so that the varieties accepted will be distinct, stable and sufficiently uniform and that they will be of satisfactory value for cultivation and use.(7) It is appropriate to take into consideration internationally established rules for certain provisions relating to the acceptance of varieties at national level.(8) In order to carry out the examinations for the acceptance of a variety, a large number of uniform criteria and minimum requirements must be laid down.(9) Provisions relating to the length of time during which acceptance of a variety is to remain valid, to the grounds on which acceptance may be revoked and to practices for maintenance of the variety must be standardized and the Member States should inform one another of the acceptance and withdrawal of varieties.(10) It is desirable to adopt rules in relation to the suitability of varietal denominations and the exchange of information between Member States.(11) Seed covered by this Directive should be freely marketable within the Community once it has been published in the common catalogue.(12) However, Member States should be given the right to express by means of a special procedure any objections which they may have to a variety.(13) The Commission should publish in the Official Journal of the European Communities, C Series, the varieties which are being added to the common catalogue of varieties of agricultural plant species.(14) Provision should be made for measures recognizing the equivalence of examinations and checks of varieties carried out in third countries.(15) Community rules should not apply to varieties the seed or propagating material of which is shown to be intended for export to third countries.(16) In the light of scientific and technical developments, it is now possible to breed varieties through genetic modification. Therefore, when determining whether to accept genetically modified varieties within the meaning of Council Directive 90/220/EEC of 23 April 1990 on the deliberate release into the environment of genetically modified organisms(9) Member States should have regard to any risk related to their deliberate release into the environment. Furthermore, conditions under which such genetically modified varieties are accepted should be established.(17) The marketing of novel foods and novel food ingredients is regulated at Community level by Regulation (EC) No 258/97 of the European Parliament and of the Council(10). Therefore, it is appropriate for Member States also to have regard to any food health risks when determining whether to accept varieties. Furthermore, conditions under which these varieties are accepted should be established.(18) In the light of scientific and technical developments, rules under which chemically treated seed and propagating material may be marketed should be introduced.(19) It is essential to ensure that plant genetic resources are conserved. Conditions to that end should be introduced to permit, within the framework of legislation on the seed trade, the conservation, by use in situ of varieties threatened with genetic erosion.(20) The measures necessary for the implementation of this Directive should be adopted in accordance with Council Decision 1999/468/EC of 28 June 1999 laying down the procedures for the exercise of implementing powers conferred on the Commission(11).(21) This Directive should not affect the obligations of the Member States concerning the deadlines for transposition of the Directives set out in Annex I, Part B.HAS ADOPTED THIS DIRECTIVE:Article 11. This Directive concerns the acceptance for inclusion in a common catalogue of varieties of agricultural plant species of those varieties of beet, fodder plant, cereal, potato and oil and fibre plant the seed of which may be marketed under provisions of the Directives concerning respectively the marketing of beet seed (2002/54/EC), fodder plant seed (66/401/EEC), cereal seed (66/402/EEC), seed potatoes (2002/56/EC) and seed of oil and fibre plants (2002/57/EC).2. The common catalogue of varieties shall be compiled on the basis of the national catalogues of the Member States.3. This Directive shall not apply to varieties, the seed or propagating material of which are shown to be, intended for export to third countries.Article 2For the purposes of this Directive "official measures" means measures taken:(a) by State authorities; or(b) by any legal person whether governed by public or by private law, acting under the responsibility of the State; or(c) in the case of ancillary activities which are also under State control, by any natural person duly sworn for that purpose;provided that the persons mentioned under (b) and (c) derive no private gain from such measures.Article 31. Each Member States shall establish one or more catalogues of the varieties officially accepted for certification and marketing in its territory. Any person may consult the catalogues.2. In the case of varieties (inbred lines, hybrids) which are intended solely as components for final varieties, the provisions of paragraph 1 apply only to the extent that the seeds which belong to them are to be marketed under their names.The conditions under which the provisions of paragraph 1 shall also apply to other component varieties may be determined in accordance with the procedure referred to in Article 23(2). In the meantime, in the case of cereals other than maize, Member States may themselves apply those provisions to other component varieties in respect of seed intended for certification in their territories.Component varieties shall be indicated as such.3. Member States may provide that the acceptance of a variety for inclusion in the common catalogue or in the catalogue of another Member State is equivalent to acceptance for inclusion in their own catalogues. If such provision is made, the Member State shall be released from the obligations provided in Article 7, Article 9(4) and Article 10(2) to (5).Article 41. Member States shall ensure that a variety is accepted only if it is distinct, stable and sufficiently uniform. The variety must be of satisfactory value for cultivation and use.2. Examination of the value for cultivation and use shall not be required:(a) for the acceptance of varieties of grasses if the breeder declares that the seed of his variety is not intended for the production of fodder plants;(b) for the acceptance of varieties whose seed is to be marketed in another Member State which has already accepted the varieties, having regard to their value for cultivation and use;(c) for the acceptance of varieties (inbred lines, hybrids) which are intended solely as components for hybrid varieties satisfying the requirements of paragraph 1.3. In the case of varieties to which point (a) of paragraph 2 applies, it may be decided, in accordance with the procedure referred to in Article 23(2), and to the extent that this is justified in the interest of free circulation of seed within the Community, that the varieties have to be shown by appropriate examination to be suitable for the purpose for which they are declared to be intended. In such cases, the conditions for the examination shall be determined.4. In the case of a genetically modified variety within the meaning of Article 2(1) and (2) of Directive 90/220/EEC the deliberate release into the environment of the variety shall be accepted only if all appropriate measures have been taken to avoid adverse effects on human health and the environment.5. However, where material derived from a plant variety is intended to be used as a food or food ingredient falling within the scope of Regulation (EC) No 258/97, these foods or food ingredients must not:- present a danger for the consumer,- mislead the consumer,- differ from foods or food ingredients which they are intended to replace to such an extent that their normal consumption would be nutritionally disadvantageous for the consumer.6. In the interest of conserving plant genetic resources as specified in Article 20(2), the Member States may depart from the acceptance criteria set out in the first sentence of paragraph 1 in so far as specific conditions are established in accordance with the procedure referred to in Article 23(2) considering the requirements of Article 20(3)(a) and (b).Article 51. A variety shall be regarded as distinct if, whatever the origin, artificial or natural, of the initial variation from which it has resulted, it is clearly distinguishable on one or more important characteristics from any other variety known in the Community.The characteristics of a variety must be capable of precise recognition and precise definition.A variety known in the Community shall be any variety which, at the time when the application for the acceptance of the variety to be assessed is duly made, is:- either listed in the common catalogue of varieties of agricultural plant species or the catalogue of varieties of vegetable species; or- without being listed in one of those catalogues, has been accepted or submitted fro acceptance in the Member State in question or in another Member State, either for certification and marketing, or for certification for other countries,unless the conditions are no longer fulfilled in all the Member States concerned before the decision on the application for acceptance of the variety to be assessed is taken.2. A variety shall be regarded as stable if, after successive propagation or multiplications or at the end of each cycle (where the breeder has defined a particular cycle of propagation or multiplications) it remains true to the description of its essential characteristics.3. A variety shall be regarded as sufficiently uniform if, apart from a very few aberrations, the plants of which it is composed are, account being taken of the distinctive features of the reproductive systems of the plants, similar or genetically identical as regards the characteristics, taken as a whole, which are considered for this purpose.4. The value of a variety for cultivation or use shall be regarded as satisfactory if, compared to other varieties accepted in the catalogue of the Member State in question, its qualities, taken as a whole, offer, at least as far as production in any given region is concerned, a clear improvement either for cultivation or as regards the uses which can be made of the crops or the products derived therefrom. Where other, superior characteristics are present, individual inferior characteristics may be disregarded.Article 6Member States shall ensure that varieties coming from other Member States are subject to the same requirements, in particular as regards the acceptance procedure, as those which apply to domestic varieties.Article 71. Member States shall provide that the acceptance of varieties be based on the results of official examinations, particularly growing trials, covering a sufficient number of characteristics for the variety to be described. The methods used for determining characteristics must be exact and reliable. In order to establish distinctness, the growing trials shall include at least the available comparable varieties which are varieties known in the Community within the meaning of Article 5(1). For the purpose of applying Article 9, other available comparable varieties shall be included.2. The following shall be fixed in accordance with the procedure referred to in Article 23(2), account being taken of current scientific and technical knowledge:(a) the characteristics to be covered as a minimum by the examinations of the various species;(b) the minimum requirements for carrying out the examination;(c) the necessary arrangements for the growing trials to be carried out with a view to assessing the value for cultivation or use; these arrangements may determine:- the procedures and conditions under which all or several Member States may agree to include in the growing trials, by way of administrative assistance, varieties for which a request for acceptance has been introduced in another Member State,- the terms of cooperation between the authorities of the participating Member States,- the impact of the results of the growing trials,- the standards relating to information on growing trials for assessment of the value for cultivation or use.3. Where examination of the genealogical components is necessary in order to study hybrids and synthetic varieties, Member States shall ensure that the results of the examination and the description of the genealogical components are, if the breeder so requests, treated as confidential.4. (a) In the case of a genetically modified variety referred to in Article 4(4), an environmental risk assessment equivalent to that laid down in Directive 90/220/EEC shall be carried out.(b) The procedures ensuring that the environmental risk assessment and other relevant elements shall be equivalent to those laid down in Directive 90/220/EEC shall be introduced on a proposal from the Commission, in a council Regulation based on the appropriate legal basis in the Treaty. Until this Regulation enters into force genetically modified varieties shall only be accepted for inclusion in a national catalogue after having been accepted for marketing in accordance with Directive 90/220/EEC.(c) Articles 11 to 18 of Directive 90/220/EEC shall no longer apply to genetically modified varieties once the Regulation referred to in point (b) above has entered into force.(d) The technical and scientific details of the implementation of the environmental risk assessment shall be adopted in accordance with the procedure referred to in Article 23(2).5. (a) The Member States shall ensure that a variety intended to be used for the purpose laid down in this paragraph is accepted only if:- the food or the food ingredient has already been authorised pursuant to Regulation (EC) No 258/97, or- the authorisation decisions referred to in Regulation (EC) No 258/97 are taken in accordance with the procedure referred to in Article 23(2).(b) In the case laid down in the second indent of paragraph (a), the criteria set out in Article 4(5) and the assessment principles laid down in Regulation (EC) No 258/97 shall be taken into account.(c) The technical and scientific details of the implementation of the measures laid down in point (b) shall be adopted in accordance with the procedure referred to in Article 23(2).Article 8Member States shall require that when lodging an application for the acceptance of a variety, the applicant indicate whether acceptance has already been applied for in another Member State, which Member State was concerned and whether the application was granted.Article 91. Each Member State shall arrange for official publication of the catalogue of varieties accepted in its territory and of the name of the person or persons responsible for maintenance of the variety in its country. When several persons are responsible for the maintenance of a variety, the names need not be published. If the names are not published, the catalogue shall indicate the authority holding the list of names of persons responsible for maintenance of the variety.2. Member States shall, as far as possible, ensure at the time of acceptance that the variety is known by the same name in all Member States.If it is known that seed or propagating material of a given variety are marketed in another country under a different name, that name shall also be indicated in the catalogue.3. In taking into account the information available, Member States shall also ensure that a variety which is not clearly distinguishable:- from a variety previously accepted in the Member State in question or in another Member State, or- from another variety which has been assessed with regard to distinctness, stability and uniformity in accordance with rules corresponding to those of this Directive, without, however, being a variety known in the Community within the meaning of Article 5(1),bears the name of that variety. This provision shall not apply if this name is likely to mislead or cause confusion concerning the variety in question, or if, pursuant to all the provisions of the Member State concerned governing the names of varieties, other facts prevent its utilisation, or if the rights of third parties impede the free use of that name in connection with the variety in question.4. Member States shall compile a file on each variety accepted, containing a description of the variety and a clear summary of all the facts on which the acceptance was based. The description of the varieties shall relate to plants produced directly from seed and young plants of the category "certified seed and propagating material".5. Member States shall ensure that genetically modified varieties which have been accepted are clearly indicated as such in the catalogue of varieties. They shall further ensure that any person marketing such a variety clearly indicates in his sales catalogue that the variety is genetically modified.6. So far as the suitability of the denomination of a variety is concerned, Article 63 of Council Regulation (EC) No 2100/94 of 27 July 1994 on Community plant variety rights(12) shall apply.Detailed implementing rules as to the suitability of denominations of varieties may be adopted in accordance with the procedure referred to in Article 23(2).Article 101. Any application or withdrawal of an application for acceptance of a variety, any entry in a catalogue of varieties as well as any amendment thereto shall be notified forthwith to the other Member States and the Commission.2. Member States shall, for each new variety accepted, send the other Member States and the Commission a brief description of its most important characteristics for use. This provision shall not apply in the case of varieties (inbred lines, hybrids) which are intended solely as components for final varieties. They shall, on request, also communicate the special qualities which enable the variety to be distinguished from other similar varieties.3. Each Member State shall make available to the other Member States and the Commission the files referred to in Article 9(4) on the varieties which are accepted or which have ceased to be accepted. Information exchanged concerning these files shall be treated as confidential.4. Member States shall ensure that the acceptance files are made available for the personal and exclusive use of any person able to show a legitimate interest. These provisions shall not apply where the information must, under Article 7(3), be treated as confidential.5. Where acceptance of a variety is refused or revoked, the results of the examinations shall be made available to persons affected by such decision.Article 111. Member States shall provide that the varieties accepted must be maintained according to accepted practices for the maintenance of the variety.2. It must at all times be possible to check maintenance from the records kept by the person or persons responsible for the variety. These records shall also cover the production of all generations prior to basic seed or propagating material.3. Samples may be requested from the person responsible for the variety. Such samples may if necessary be taken officially.4. Where maintenance takes place in a Member State other than the one in which the variety was accepted, the Member States concerned shall assist each other administratively as regards verification.Article 121. Acceptance shall be valid until the end of the tenth calendar year following acceptance.Acceptance of the varieties by the authorities of the former German Democratic Republic prior to German unification shall be valid until the end of the tenth calendar year at the latest following their entry in the catalogue of varieties drawn up by the Federal Republic of Germany in accordance with Article 3(1).2. Acceptance of a variety may be renewed at given intervals if it is still cultivated on such a scale as to justify this, or should be retained in the interest of conserving plant genetic resources, and providing that the requirements as to distinctness, uniformity and stability, or the criteria determined under Article 20(2) and (3), are still satisfied. Except in the case of plant genetic resources within the meaning of Article 20 applications for renewal shall be submitted not later than two years before expiry of acceptance.3. The period of validity of acceptance shall be extended provisionally until a decision is taken on the application for renewal.Article 131. Member States shall ensure that any doubts which arise after the acceptance of a variety concerning the appraisal of its distinctness or of its name at the time of acceptance are clarified.2. Where, after acceptance of a variety, it is established that the condition concerning distinctness within the meaning of Article 5 was not fulfilled at the time of acceptance, acceptance shall be replaced by another decision or, where appropriate, a revocation, which conforms with this Directive.By this other decision, the variety shall, with effect from the date of its initial acceptance, no longer be regarded as a variety known in the Community within the meaning of Article 5(1).3. Where, after acceptance of a variety, it is established that its name within the meaning of Article 9 was not acceptable when the variety was accepted, the name shall be adapted in such a way that it conforms with this Directive. Member States may permit the previous name to be used temporarily as an additional name. The detailed arrangements in accordance with which the previous name may be used as an additional name may be laid down in accordance with the procedure referred to in Article 23(2).4. In accordance with the procedure referred to in Article 23(2) rules may be established for the application of paragraphs 1 and 2.Article 141. Member States shall ensure that acceptance of a variety is revoked:(a) if it is proved, on examination, that the variety is no longer distinct, stable or sufficiently uniform;(b) if the person or persons responsible for the variety so request, unless there is maintenance of the variety.2. Member States may revoke the acceptance of a variety:(a) if the laws, regulations and administrative provisions adopted in pursuance of this Directive are not complied with;(b) if, at the time of the application for acceptance or during examination, false or fraudulent particulars were supplied concerning the factors on the basis of which acceptance was granted.Article 151. Member States shall ensure that a variety is deleted from their catalogues if acceptance of the variety has been revoked or if the period of validity of the acceptance has expired.2. Member States may, in respect of their own territory, allow a period for the certification and marketing of seed or propagating material up to 30 June of the third year at the most after expiry of the acceptance.In the case of varieties that were listed pursuant to Article 16(1) in the common catalogue of varieties referred to in Article 17, the period which expires last among those granted by the various Member States of acceptance under the first subparagraph shall apply to marketing in all the Member States, provided that the seed or propagating material of the variety concerned has not been subject to any marketing restriction as regards the variety.Article 161. Member States shall ensure that, with effect from the publication referred to in Article 17, seed of varieties accepted in accordance with this Directive or in accordance with principles corresponding to those of this Directive is not subject to any marketing restrictions relating to variety.2. A Member State may, upon application which shall be dealt with under the procedure referred to in Article 23(2) or in Article 23(3) in the case of genetically modified varieties, be authorised to prohibit the use of the variety in all or in part of its territory or to lay down appropriate conditions for cultivating the variety in accordance, in cases provided for in subparagraph (c), with the conditions for using the products resulting from such cultivation:(a) where it is established that the cultivation of the variety could be harmful from the point of view of plant health to the cultivation of other varieties or species; or(b) where official growing trials carried out in the applicant Member States, Article 5(4) being applied correspondingly, show that the variety does not, in any part of its territory, produce results corresponding to those obtained from a comparable variety accepted in the territory of that Member State or, where it is well known that the variety is not suitable for cultivation in any part of its territory because of its type of maturity class. The application shall be lodged before the end of the third calendar year following that of acceptance;(c) where it has valid reasons other than those already mentioned or which may have been mentioned during the procedure referred to in Article 10(2) for considering that the variety presents a risk for human health or the environment.Article 17The Commission shall, on the basis of the information supplied by the Member States and as this is received, publish in the C series of the Official Journal of the European Communities under the title "Common Catalogue of Varieties of Agricultural Plant Species" a list of all varieties of which the seed and propagating material, under Article 16, are not subject to any marketing restrictions as regards variety, and also the information required under Article 9(1) concerning the person or persons responsible for maintenance of the variety. The published notice shall indicate the Member States which have received an authorisation under Article 16(2) or Article 18.The published notice shall list those varieties for which a period has been applied in accordance with the second subparagraph of Article 15(2). This shall indicate the length of the period and, where appropriate, the Member States to which the period does not apply.The published notice shall clearly indicate those varieties which have been genetically modified.Article 18If it is established that the cultivation of a variety included in the common catalogue of varieties could in any Member State be harmful from the point of view of plant health to the cultivation of other varieties or species, or present a risk for the environment or for human health, that Member State may upon application, be authorised in accordance with the procedure referred to in Article 23(2) or in Article 23(3) in the case of a genetically modified variety to prohibit the marketing of the seed or propagating material of that variety in all or part of its territory. Where there is imminent danger of the spread of harmful organisms or imminent danger for human health or for the environment, that prohibition may be imposed by the Member State concerned as soon as its application has been lodged until such time as a final decision has been taken. That decision shall be taken within a period of three months in accordance with the procedure laid down in Article 23(2) or in Article 23(3) in the case of a genetically modified variety.Article 19Where a variety ceases to be accepted in the Member State which initially accepted it, one or more other Member States may continue to accept that variety provided that the requirements for acceptance continue to be met in their territory and that maintenance remains assured.Article 201. Specific conditions may be established in accordance with the procedure referred to in Article 23(2) to take account of developments in relation to the conditions under which chemically treated seed may be marketed.2. Without prejudice to Council Regulation (EC) No 1467/94 of 20 June 1994 on the conservation, characterisation, collection and utilisation of genetic resources in agriculture(13), specific conditions shall be established in accordance with the procedure referred to in Article 23(2) to take account of developments in relation to the conservation in situ and the sustainable use of plant genetic resources through growing and marketing of seed of landraces and varieties which are naturally adapted to the local and regional conditions and threatened by genetic erosion.3. The specific conditions referred to in paragraph 2 above shall include in particular the following points:(a) landraces and varieties shall be accepted in accordance with the provisions of this Directive. The procedure for official acceptance shall take into account specific quality characteristics and requirements. In particular the results of unofficial tests and knowledge gained from practical experience during cultivation, reproduction and use and the detailed descriptions of the varieties and their relevant denominations, as notified to the Member State concerned, shall be taken into account and, if sufficient, shall result in exemption from the requirement of official examination. Upon acceptance of such a landrace or variety, it shall be indicated as a "conservation variety" in the common catalogue;(b) appropriate quantitative restrictions.Article 21Specific conditions may be established in accordance with the procedure referred to in Article 23(2) to take account of developments in the area of the conservation of genetic resources.Article 221. The Council, acting by a qualified majority on a proposal from the Commission, shall determine whether:(a) the official examinations of varieties carried out in the third country afford the same assurances as those provided for in Article 7 and carried out in the Member States;(b) the checks on practices for the maintenance of varieties carried out in the third country afford the same assurances as those carried out by the Member States.2. Paragraph 1 shall also apply in respect of any new Member State from the date of its accession to the date on which it is to bring into force the laws, regulations or administrative provisions necessary to comply with this Directive.Article 231. The Commission shall be assisted by the Standing Committee on Seeds and Propagating Material for Agriculture, Horticulture and Forestry set up by Article 1 of Council Decision 66/399/EEC(14).2. Where reference is made to this paragraph, Articles 4 and 7 of Decision 1999/468/EC shall apply.The period laid down in Article 4(3) of Decision 199/468/EC shall be set at one month.3. Where reference is made to this paragraph, Articles 5 and 7 of Decision 1999/468/EC shall apply.The period laid down in Article 5(6) of Decision 1999/468/EC shall be set at one month.4. The Committee shall adopt its rules of procedure.Article 24Save as otherwise provided in Articles 16 and 18, this Directive shall be without prejudice to the provisions of national laws justified on grounds of the protection of health and life of humans, animals or plants or the protection of industrial or commercial property.Article 25The Member States shall communicate to the Commission the text of the main provisions of domestic law they adopt in the field covered by this Directive.The Commission shall inform the other Member States thereof.Article 261. Directive 70/457/EEC as amended by the Directives listed in Annex I part A, is hereby repealed without prejudice to the obligations of the Member States concerning the deadlines for transposition of the said Directives set out in Annex I part B.2. References to the Directive shall be construed as references to this Directive and shall be read in accordance with the correlation table in Annex II.Article 27This Directive shall enter into force on the twentieth day following that of its publication in the Official Journal of the European Communities.Article 28This Directive is addressed to the Member States.Done at Luxembourg, 13 June 2002.For the CouncilThe PresidentM. Rajoy Brey(1) Opinion delivered on 9 April 2002 (not yet published in the Official Journal).(2) OJ 225, 12.10.1970, p. 1. Directive as last amended by Directive 98/96/EC (OJ L 25, 1.2.1999, p. 27).(3) See Annex I, Part A.(4) See page 12 of this Official Journal.(5) OJ 125, 11.7.1966, p. 2298/66. Directive as last amended by Directive 2001/64/EC (OJ L 234, 1.9.2001, p. 60).(6) OJ 125, 11.7.1966, p. 2309/66. Directive as last amended by Directive 2001/64/EC.(7) See page 60 of this Official Journal.(8) See page 74 of this Official Journal.(9) OJ L 117, 8.5.1970, p. 15. Directive repealed by Directive 2001/18/EC of the European Parliament and of the Council (OJ L 106, 17.4.2001, p. 1).(10) OJ L 43, 14.2.1997, p. 1.(11) OJ L 184, 17.7.1999, p. 23.(12) OJ L 227, 1.9.1994, p. 1. Regulation as amended by Regulation (EC) No 2506/95 (OJ L 258, 28.10.1995, p. 3).(13) OJ L 159, 28.6.1994, p. 1.(14) OJ 125, 11.7.1966, p. 2289/66.ANNEX IPART AREPEALED DIRECTIVE AND ITS SUCCESSIVE AMENDMENTS(referred to by Article 26)>TABLE>PART BDEADLINES FOR TRANSPOSITION INTO NATIONAL LAW(referred to by Article 26)>TABLE>ANNEX IICORRELATION TABLE>TABLE>


Avis juridique important

|

31982L0434

Second Commission Directive 82/434/EEC of 14 May 1982 on the approximation of the Laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products

Official Journal L 185 , 30/06/1982 P. 0001 - 0028 Finnish special edition: Chapter 13 Volume 12 P. 0071  Spanish special edition: Chapter 15 Volume 3 P. 0179  Swedish special edition: Chapter 13 Volume 12 P. 0071  Portuguese special edition Chapter 15 Volume 3 P. 0179

SECOND COMMISSION DIRECTIVE of 14 May 1982 on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products (82/434/EEC)  THE COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community,  Having regard to Council Directive 76/768/EEC of 27 July 1976 on the approximation of the laws of the Member States relating to cosmetic products (1), as amended by Directive 79/661/EEC (2), and in particular Article 8 (1) thereof,  Whereas Directive 76/768/EEC provides for the official testing of cosmetic products with the aim of ensuring that the conditions laid down by Community provisions concerning the composition of cosmetic products are satisfied;  Whereas all the necessary methods of analysis should be drawn up as quickly as possible ; whereas, the first step towards the attainment of this objective having already been taken by the definition of certain methods in Commission Directive 80/1335/EEC (3), the second step is to consist in the definition of methods for identification of some oxidizing agents and determination of hydrogen peroxide in cosmetic hair-care products, identification and semi-quantitative determination of certain oxidation colorants in hair dyes, identification and determination of nitrite, identification and determination of free formaldehyde, determination of resorcinol in shampoos and hair lotions, and determination of methanol in relation to ethanol or propan-2-ol;  Whereas the measures laid down in this Directive are in accordance with the opinion of the Committee on the adaptation of Directive 76/768/EEC to technical progress,  HAS ADOPTED THIS DIRECTIVE:    Article 1 Member States shall take all necessary steps to ensure that, during official testing of cosmetic products:    - identification of oxidizing agents and determination of hydrogen peroxide in hair-care products,       - identification and semi-quantitative determination of certain oxidation colorants in hair dyes,       - identification and determination of nitrite,       - identification and determination of free formaldehyde,  (1) OJ No L 262, 27.9.1976, p. 169. (2) OJ No L 192, 31.7.1979, p. 35. (3) OJ No L 383, 31.12.1980, p. 27.        - determination of resorcinol in shampoos and hair lotion,       - determination of methanol in relation to ethanol or propan-2-ol         are performed in accordance with the methods described in the Annex.   Article 2 Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive not later than 31 December 1983.  They shall forthwith inform the Commission thereof.   Article 3 This Directive is addressed to the Member States.     Done at Brussels, 14 May 1982.  For the Commission  Karl-Heinz NARJES  Member of the Commission     ANNEX I. IDENTIFICATION OF OXIDIZING AGENTS AND DETERMINATION OF HYDROGEN PEROXIDE IN HAIR-CARE PRODUCTS  PURPOSE AND SCOPE  The iodometric determination of hydrogen peroxide in cosmetics is only possible in the absence of other oxidizing agents that form iodine from iodides. Consequently, before the iodometric determination of hydrogen peroxide it is necessary to detect and identify any other oxidizing agents present This identification breaks down into two stages ; the first covers the persulphates the bromates and hydrogen peroxide and the second covers barium peroxide.  A. IDENTIFICATION OF PERSULPHATES, BROMATES AND HYDROGEN PEROXIDE     1. PRINCIPLE  Sodium persulphate, potassium persulphate and ammonium persulphate ; potassium bromate, sodium bromate and hydrogen peroxide - whether or not originating from barium peroxide - are identified by means of descending paper chromatography, use being made of two developing solvents.       2. REAGENTS  All reagents should be of analytical purity.      2.1. 0 75 % (m/v) aqueous reference solutions of the following compounds:        2.1.1. Sodium persulphate               2.1.2. Potassium persulphate               2.1.3. Ammonium persulphate               2.1.4. Potassium bromate               2.1.5. Sodium bromate               2.1.6. Hydrogen peroxide                          2.2. Developing solvent A, 80 % (v/v) ethanol           2.3. Developing solvent B, benzene - methanol - 3-methyl butan-1-ol - water (34 : 38 : 18 : 10 by vol)           2.4. Detecting agent A, 10 % (m/v) aqueous solution of potassium iodide           2.5. Detecting agent B, 1 % (m/v) aqueous solution of starch           2.6. Detecting agent C, 10 % (m/m) hydrochloric acid           2.7. 4N hydrochloric acid                  3. APPARATUS AND EQUIPMENT      3.1. Chromatography paper (Whatman paper No 3 and No 4 or their equivalents)           3.2. Micropipette, 1 ¶l           3.3. Standard flasks, 100 ml           3.4. Fluted filters           3.5. Apparatus for descending paper chromatography   4. SAMPLE PREPARATION        4.1. Water soluble products  Make two solutions of each sample by dissolving 1 g and 5 g of the product respectively in 100 ml of water. Use 1 ¶l of each of these solutions for carrying out the paper chromatography described in Section 5.               4.2. Products sparingly soluble in water          4.2.1. Weigh out 1 g and 5 g of the sample and disperse in 50 ml of water, make up to 100 ml with water in each case and mix. Filter the two dispersions over a fluted filter (3.4) and use 1 ¶l of each of the filtrates in order to carry out the paper chromatography described in Section 5.                   4.2.2. Prepare once again two dispersions of each sample by dispersing 1 g and 5 g in 50 ml of water, acidify with dilute hydrochloric acid (2.7), make up with water to 100 ml and mix. Filter the dispersions through a fluted filter (3.4) and use 1 ¶l of the two filtrates in order to carry out the paper chromatography described in Section 5.                                  4.3. Creams  Disperse 5 g and 20 g of each product in 100 ml of water and use the dispersions to carry out the paper chromatography described in Section 5.  5. METHOD          5.1. Put an appropriate quantity of solvents A (2.2) and B (2.3) into two separate chromatography tanks in order to carry out the descending paper chromatography. Saturate the chromatography tanks for at least 24 hours with solvent vapour.                   5.2. Apply 1 ¶l of one sample solution and of one reference solution prepared according to Sections 4 and 2.1 to each starting point on a strip of chromatography paper (Whatman No 3 or equivalent) 40 cm long and 20 cm wide (3.1) or another suitable format and evaporate the solution in air.                   5.3. Place the chromatography strip (5.2) in the chromatography tank filled with developing solvent A (5.1) and develop until the solvent front has advanced 35 cm (about 15 hours).                   5.4. Repeat the procedure described in Sections 5.2 and 5.3, using chromatography paper (Whatman No 4 or equivalent) (3.1) and developing solvent B. Chromatograph until the solvent front has advanced 35 cm (about five hours).                   5.5. After development remove the chromatograms and dry them in air.                   5.6. Reveal the spots in the chromatogram by spraying it successively with:            5.6.1. detecting agent A (2.4) followed shortly thereafter by detecting agent B (2.5). The spots of the persulphates will now appear first in the chromatogram and will be followed by the hydrogen peroxide spots. Mark the spots with a pencil;                       5.6.2. detecting agent C (2.6) on the chromatograms obtained in accordance with Section 5.6.1; the presence of bromates will now be indicated by greyish blue spots in the chromatogram.                                          5.7. Under the abovementioned conditions pertaining to developing solvents A (2.2) and B (2.3), the Rf values of the reference substances (2.1) are approximately as follows: >PIC FILE= "T0050747">                                       B. IDENTIFICATION OF BARIUM PEROXIDE     1. PRINCIPLE  Barium peroxide is identified by the formation of hydrogen peroxide after acidification of the sample (A.4.2), and by the presence of the barium ion:      - in the absence of persulphates (A), by adding dilute sulphuric acid to a portion of the acid sample solution (B.4.1), as a result of which a white precipitate of barium sulphate is formed. The presence of barium ions in the sample (B.4.1) is again confirmed by paper chromatography in the manner described below (B.5),           - where barium peroxide and persulphates are present simultaneously (B.4.2) by digesting the residue from the solution (B.4.2) in an alkali ; after dissolution in hydrochloric acid, the presence of barium ions is confirmed in the solution of the melt (B.4.2.3) by paper chromatography and/or by barium sulphate precipitation.                  2. REAGENTS      2.1. Methanol           2.2. 36 % (m/m) concentrated hydrochloric acid           2.3. 6N hydrochloric acid           2.4. 4N sulphuric acid           2.5. Rhodizonic acid disodium salt           2.6. Barium chloride (BaCl2 72H2O)           2.7. Anhydrous sodium carbonate           2.8. 1 % (m/v) aqueous solution of barium chloride           2.9. Developing solvent consisting of methanol, concentrated hydrochloric acid (concentration 36 %) and water (80 : 10 : 10 by vol)           2.10. Detecting agent, 0 71 % (m/v) aqueous solution of rhodizonic acid disodium salt, to be freshly prepared immediately before use.                  3. APPARATUS AND EQUIPMENT      3.1. Micropipette, 5 ¶l           3.2. Platinum crucibles           3.3. Standard flasks, 100 ml           3.4. Chromatography paper Schleicher and Schull 2043 b or equivalent. Clean the paper by developing it overnight in a descending chromatography tank (A.3.5) containing developing solvent (B.2.9) and then dry.           3.5. Fluted filter paper           3.6. The usual apparatus for carrying out ascending paper chromatography                  4. SAMPLE PREPARATION      4.1. Products in which persulphates are absent        4.1.1. Disperse 2 g of the product in 50 ml of water and bring the pH of the dispersion to about 1 with hydrochloric acid (B.2.3).                4.1.2. Transfer the dispersion with water into a 100-ml standard flask, make up to the mark with water and mix. Use this dispersion for the paper chromatography analysis described in Section 5 and for identification of barium by precipitation of the sulphate.                          4.2. Products in which persulphates are present        4.2.1. Disperse 2 g of the product in 100 ml of water and filter.               4.2.2. Add to the dried residue seven to 10 times its weight of sodium carbonate (B.2.7), mix and melt the mixture in a platinum crucible (B.3.2) for half an hour.               4.2.3. Cool to room temperature, dissolve the melt in 50 ml of water and filter (B.3.5)               4.2.4. Dissolve the residue from the melt in hydrochloric acid (B.2.3) and make up to 100 ml with water. Use this solution for the paper chromatography analysis described in Section 5 and for the identification of barium by precipitation of the sulphate.                                 5. METHOD      5.1. Place an appropriate quantity of developing solvent (B.2.9) in a tank for ascending paper chromatography and saturate the tank for at least 15 hours.           5.2. On a piece of chromatography paper - pretreated as described in Section B. 3.4 - apply 5 ¶l of each of the solutions prepared in accordance with Sections B.4.1.2 and B. 4.2.4 and reference solution B.2.8 at three starting points.           5.3. Dry the sample and reference spots in air. Develop the chromatogram until the solvent front has ascended 30 cm.           5.4. Remove the chromatogram from the tank and dry in air.           5.5. Reveal the spots on the chromatogram by spraying the paper with detecting agent B.2.10. In the presence of the barium, red spots with an RF value of about 0 710 appear on the chromatogram.                   C. DETERMINATION OF HYDROGEN PEROXIDE     1. PRINCIPLE  The iodometric determination of hydrogen peroxide is based on the following reaction: >PIC FILE= "T0050748">   This conversion proceeds slowly but can be accelerated by the addition of ammonium molybdate. The iodine formed is determined titrimetrically against sodium thiosulphate and is a measure of the hydrogen peroxide content.       2. DEFINITION  The hydrogen peroxide content measured in the manner described below is expressed as a percentage by mass (% m/m) of the product.       3. REAGENTS  All reagents should be of analytical purity.      3.1. 2N sulphuric acid           3.2. Potassium iodide           3.3. Ammonium molybdate           3.4. 0 71 N sodium thiosulphate  3.5. 10 % (m/v) potassium iodide solution, to be freshly prepared immediately before use           3.6. 20 % (m/v) ammonium molybdate solution           3.7. 1 % (m/v) starch solution                  4. APPARATUS AND EQUIPMENT      4.1. Beakers, 100 ml           4.2. Burette, 50 ml           4.3. Standard flasks, 250 ml           4.4. Measuring cylinders, 25 and 100 ml           4.5. One-mark pipettes, 10 ml           4.6. Conical flasks, 250 ml                  5. METHOD      5.1. Into a 100-ml beaker weigh out 10 g (m gram) of the product, containing about 0 76 g of hydrogen peroxide. Transfer the contents with water into a 250-ml standard flask, make up to the mark with water and mix.           5.2. Pipette 10 ml of the sample solution (5.1) into a 250-ml conical flask (4.6) and add successively 100 ml of 2N sulphuric acid (3.1), 20 ml of potassium iodide solution (3.5) and three drops of ammonium molybdate solution (3.6).           5.3. Titrate the iodine formed immediately against 0 71N sodium thiosulphate solution (3.4) and just before the end point is reached add a few millilitres of starch solution as indicator (3.7). Record the consumption of 0 71N sodium thiosulphate (3.4) in millilitres (V).           5.4. In the manner described in Sections 5.2 and 5.3, carry out a blank determination, replacing the 10 ml of the sample solution by 10 ml of water. Record the consumption of 0 71N sodium thiosulphate in the blank determination (Vo ml).                  6. CALCULATION  Calculate the hydrogen peroxide content of the product as a percentage by mass (% m/m) with the aid of the following formula: >PIC FILE= "T0050749">        7. REPEATABILITY (1)  For a product containing about 6 % m/m hydrogen peroxide the difference between the results of two determinations in parallel carried out on the same sample should not exceed an absolute value of 0 72 %.  (1) See Norm ISO 5725.         II. IDENTIFICATION AND SEMI-QUANITTATIVE DETERMINATION OF CERTAIN OXIDATION COLORANTS IN HAIR DYES   1. PURPOSE AND SCOPE  This method is suitable for the identification and semi-quantitative determination of the following substances in hair dyes in cream or liquid form: >PIC FILE= "T0050750">    2. PRINCIPLE  Oxidation colorants are extracted at pH 10 with 96 % ethanol from dyes in cream or liquid form and identified by thin-layer chromatography, either one- or two-dimensional.  For semi-quantitative determination of these substances, the chromatogram of the samples is compared by means of four developing systems with those for reference substances produced at the same time and under as similar conditions as possible.   3. REAGENTS  All reagents should be of analytical purity.    3.1. Ethanol, anhydrous       3.2. Acetone       3.3. Ethanol, 96 % v/v       3.4. Ammonia solution, 25 % (d204 = 0 791)  3.5. L(+)-ascorbic acid       3.6. Chloroform       3.7. Cyclohexane       3.8. Nitrogen, technical grade       3.9. Toluene       3.10. Benzene       3.11. n-Butanol       3.12. Butan-2-ol       3.13. Hypophosphorous acid, 50 % v/v solution       3.14. Diazo reagent. Either:      - 3-Nitro-1-benzenediazonium chlorobenzenesulphonate (stabilized salt form) as in Red 2 JN - Francolor,           - 2-Chloro-4-nitro- 1-benzenediazonium naphthalenebenzoate, (stabilized salt form) as in NNCD Reagent - reference No 74 150 FLUKA,             or an equivalent.       3.15. Silver nitrate       3.16. p-Dimethylaminobenzaldehyde       3.17. 2,5-Dimethylphenol       3.18. Ferric chloride hexahydrate       3.19. Hydrochloric acid, 10 % m/v solution       3.20. Reference substances  The reference substances are those shown in paragraph 1 "Purpose and scope". In the case of amine compounds, the reference substance must be either the hydrochloride (mono or di) or the free base.       3.21. Reference solutions 0 75 % (m/v)  A 0 75 % (m/v) solution of each of the reference substances in Section 3.20 is prepared.  Weigh out 50 mg ± 1 mg of the reference substance in a standard 10-ml flask.  Add 5 ml of 96 % ethanol (3.3) and 250 mg of ascorbic acid (3.5).  Make the solution alkaline by addition of the ammonia solution (3.4) to give an apparent pH of 10 (test with indicator paper).  Make up to 10 ml with 96 % ethanol (3.3) and mix.  The solutions may be kept for a week in a cool place away from the light.  In certain cases, after the addition of the ascorbic acid and the ammonia, a precipitate may form. It should then be allowed to settle before proceeding.       3.22. Developing solvents      3.22.1. Acetone - chloroform - toluene (35 : 25 : 40 by vol)           3.22.2. Chloroform - cyclohexane - absolute ethanol - 25 % ammonia (80 : 10 : 10 : 1 by vol)           3.22.3. Benzene - butan-2-ol - water (50 : 25 : 25 by vol). Shake well and use the upper phase after separating at room temperature (20 to 25 °C).           3.22.4. n-Butanol - chloroform - reagent M (7 : 70 : 23 by vol). Separate carefully at room temperature (20 to 25 °C) and use the lower phase.              >PIC FILE= "T0050751">   Note  Developing solvents containing ammonia must be well shaken immediately before use.       3.23. Indicator sprays      3.23.1. Diazo reagent  Make a 5 % (m/v) aqueous solution of the chosen reagent (3.14). This solution must be freshly prepared just before use.           3.23.2. Ehrlich's reagent  Dissolve 2 g of p-diamethylaminobenzaldehyde (3.16) in 100 ml of hydrochloric acid 10 % (m/v) aqueous solution (3.19).           3.23.3. 2,5-dimethylphenol - ferric chloride hexahydrate  Solution 1 : Dissolve 1 g of dimethylphenol (3.17) in 100 ml of 96 % ethanol (3.3).  Solution 2 : Dissolve 4 g of ferric chloride hexahydrate (3.18) in 100 ml of 96 % ethanol (3.3).  For development, these solutions are sprayed separately, first solution 1 then solution 2.           3.23.4. Ammoniacal silver nitrate  25 % ammonia (3.4) is added to 5 % (m/v) aq. solution of silver nitrate (3.15) until the precipitate just dissolves. This reagent must be prepared immediately before use.  Do not keep.                     4. APPARATUS    4.1. Usual laboratory equipment for thin-layer chromatography.      4.1.1. Plastics or glass cover so constructed that the chromatographic plate can be surrounded with nitrogen during application of the spots and drying. This precaution is necessary because of the susceptibility to oxidation of certain colorants.           4.1.2. Micro-syringe, 10 ¶l, graduated in 0 72 ¶l divisions, with a square cut needle, or, better, a 50 ¶l repeating dispenser, mounted on a clamp stand in such a way that the plate can be kept under nitrogen.           4.1.3. Silica gel thin layer plates ready to use 0 725 mm thick, formed by 20 x 20 cm (Macherey and Nagel, Silica G-HR, which are on plastics support, or equivalent)                  4.2. Centrifuge, 4 000 rev./min.       4.3. Centrifuge tubes, 10 ml with PTFE-lined screw caps, or equivalent          5. PROCEDURE    5.1. Treatment of test samples  Discard the first 2 or 3 cm of cream extruded from the tube.  Put the following into a centrifuge tube (4.3) previously flushed out with nitrogen : 300 mg ascorbic acid with 3 g cream or 3 g homogenized liquid.  Add 25 % ammonia drop-wise (3.4) until the pH is 10. Make up to 10 ml with 96 % ethanol (3.3).  Homogenize under nitrogen (3.8), stopper and then centrifuge at 4 000 rev./min. for 10 minutes.  Use the supernatant liquid.        5.2. Chromatography      5.2.1. Spotting the plates  Under an atmosphere of nitrogen (3.8), apply to a chromatography plate (4.1.3) 1 ¶l of each of the above-described reference solutions at nine points situated about 1 75 cm apart along a line approximately 1 75 cm from the edge of the plate.  These reference solution spots are arranged as follows: >PIC FILE= "T0050752">   In addition, apply at points 10 and 11 respectively 2 ¶l of the test solution samples obtained according to Section 5.1.  Keep the plate under nitrogen (3.8) until the moment when it is chromatographed.           5.2.2. Development  Place the plate in a tank previously flushed out with nitrogen (3.8), saturated with one of the four solvents (3.22) and allow to develop at room temperature (20 to 25 °C) in the dark until the solvent front has moved about 15 cm from the baseline. Remove the plate and dry under nitrogen (3.8) at room temperature.           5.2.3. Spraying  Spray the plate immediately with one of the four solutions specified in 3.23.           5.2.4. Identification  Compare the Rf value and the colour obtained from the sample with those of the reference substances chromatographed.  Table I gives as examples the Rf values and colours for each substance depending on the solvent and indicator used.  Confirmation of doubtful identification may sometimes be achieved by a spiking method, adding the corresponding reference substance solution to the sample extract.           5.2.5. Semi-quantitative estimation  Compare visually the intensity of the spots for each substance identified in 5.2.4 with an appropriate range of concentrations of the reference substances.  If the concentration of one or more of the substances found in the sample is excessive, dilute the sample extract and repeat the measurement.   >PIC FILE= "T0050753">                  6. EXAMINATION BY TWO-DIMENSIONAL THIN-LAYER CHROMATOGRAPHY  This two-dimensional chromatographic procedure requires the use of additional standards and reagents.  6.1. Additional reference solutions and substances  6.1.1. >PIC FILE= "T0050754">   6.1.2. 2-aminophenol (OAP)  6.1.3. 3-aminophenol (MAP)  6.1.4. 4-aminophenol (PAP)  6.1.5. 2-nitro-1,4-phenylenediamine (2-NPPD)  6.1.6. 4-nitro-1,2-phenylenediamine (4-NOPD)  Prepare a 0 75 % m/v solution of each of the additional reference substances as described in 3.21.   6.2. Additional developing solvent    6.2.1. Ethyl acetate - cyclohexane - ammonia solution, 25 % (65 : 30 : 0 75 by vol)          6.3. Additional indication system  Place a glass vessel in a developing tank for thin-layer chromatography, add about 2 g crystallized iodine and close the tank with an adequate lid.    6.4. Chromatography    6.4.1. Draw two lines, at shown in Figure 1, on the absorbent surface of a thin-layer plate (4.1.3).       6.4.2. Under a nitrogen atmosphere (4.1.1), apply 1 to 4 ¶l extract (5.1) at base point 1 (Figure 1) which is at 2 cm from the two sides. The quantity of extract depends on the intensity of the spots on the chromatograms 5.2.       6.4.3. Divide between points 2 and 3 (Figure 1) the oxidation colorants identified or assumed to be identified by 5.2 (distance between points 1 75 cm). Apply 2 ¶l of each of the reference solutions - except DAP of which 6 ¶l must be applied. Conduct the operation under nitrogen (6.4.2).       6.4.4. Repeat the operation in 6.4.3 at base points 4 and 5 (Figure 1) and keep the plate under nitrogen until the moment it is chromatographed (distance between points 1 75 cm).       6.4.5. Flush out a chromatographic tank with nitrogen (3.8) and place in it a suitable quantity of developing solvent 3.22.2. Place the plate (6.4.4) in the tank and develop it in the first elution direction (Figure 1) in the dark.  Elute until the solvent front reaches the line marked on the plate (approximately 13 cm).       6.4.6. Remove the plate from the tank and place it in the chromatography tank previously flushed out with nitrogen to evaporate the elution solvent for at least 60 minutes.       6.4.7. With a graduated test-tube, place a suitable quantity of elution solvent (6.2) in a tank flushed out with nitrogen (3.8), place the plate rotated through 90° in the tank (6.4.6) and chromatograph in the second direction (also in the dark) until the solvent front reaches the line drawn on the absorbent surface. Remove the plate from the tank and evaporate the elution solvent in air.       6.4.8. Place the plate for 10 minutes in the chromatography tank with iodine vapour (6.3) and interpret the two-way chromatogram using the Rf and colour values of the reference substances chromatographed at the same time (Table II gives a guide to the Rf values and colours).  Note  To obtain maximum colouring of the spots leave the chromatogram exposed to the atmosphere for half an hour after developing.       6.4.9. The presence of the oxidation colorants found in 6.4.8 can be definitively confirmed by repeating the operations described in 6.4.1 to 6.4.8 and adding at base point 1 on top of the amount of extract specified in 6.4.2 1 ¶l of the reference substances identified in 6.4.8. if no other spot is found in comparison with the chromatogram obtained in 6.4.8, the interpretation of chromatogram 6.4.8 is correct.             >PIC FILE= "T0050755">    III. IDENTIFICATION AND DETERMINATION OF NITRITE  A. IDENTIFICATION   1. PURPOSE AND SCOPE  This method is suitable for the identification of nitrite in cosmetic products particularly creams and pastes.   2. PRINCIPLE  The presence of nitrite is indicated by the formation of coloured derivatives with >PIC FILE= "T0050756">    3. REAGENTS  All reagents should be of analytical purity.    3.1. Dilute sulphuric acid : dilute 2 ml concentrated sulphuric acid (d204 = 1 784) with 11 ml distilled water.       3.2. Dilute hydrochloric acid : dilute 1 ml concentrated hydrochloric acid (d204 = 1 719) with 11 ml distilled water.       3.3. Methanol  3.4.  >PIC FILE= "T0050757">   Add drop-wise 4 ml dilute hydrochloric acid (3.2) and shake. Fill up to the mark with methanol and mix until the solution is completely clear. Store the solution in a brown glass bottle (4.3).          4. APPARATUS    4.1. Beakers, 50 ml       4.2. Standard flask, 100 ml       4.3. Brown glass bottle, 125 ml       4.4. Glass plate, 10 x 10 cm       4.5. Plastics spatula       4.6. Filter paper, 10 x 10 cm          5. PROCEDURE    5.1. Spread part of the sample to be examined evenly over the glass plate (4.4) so as to cover the surface to a thickness of no more than 1 cm.       5.2. Soak a sheet of filter paper (4.6) in distilled water. Lay it on the sample and press the filter paper down with the plastics spatula (4.5).       5.3. Wait about one minute and apply to the centre of the filter paper:  - two drops of dilute sulphuric acid (3.1),  - >PIC FILE= "T0050758">        5.4. After five to 10 seconds, remove the filter paper and examine it against daylight. The presence of nitrite is indicated by a reddish purple coloration.   If the nitrite content is low, the reddish purple colour changes to yellow after five to 15 seconds. This change of colour takes place only after one to two minutes where large quantities of nitrite are present.          6. COMMENT  The intensity of the reddish purple colour and the time that elapses before the change to yellow may give an indication of the nitrite content of the sample.    B. DETERMINATION   1. PURPOSE  The method describes the determination of nitrite in cosmetic products.   2. DEFINITION  The nitrite content of the sample, determined according to this method, is expressed in % by mass of sodium nitrite.   3. PRINCIPLE  After diluting the sample with water and clarifying, the nitrite present is made to react with sulphanilamide and N-1-naphthylethylenediamine and the optical density of the colour obtained is measured at 538 nm.   4. REAGENTS  All reagents should be of analytical quality.    4.1. Clarification reagents : these reagents may not be used more than one week after preparation.      4.1.1. Carrez I reagent:  Dissolve 106 g of potassium cyanoferrate (II) K4Fe(CN)6 73H2O, in distilled water and dilute with water to 1 000 ml.           4.1.2. Carrez II reagent:  Dissolve 219 75 g of zinc acetate, Zn(CH3COO)2 72H2O and 30 ml of glacial acetic acid in distilled water and dilute with water to 1 000 ml.                  4.2. Sodium nitrite solution:  Dissolve 0 7500 g of sodium nitrite in distilled water in a 1 000-ml volumetric flask and dilute with water to the mark. Dilute 10 70 ml of this stock standard solution to 500 ml ; 1 ml of the latter solution = 10 micrograms of NaNO2.       4.3. 1N sodium hydroxide solution       4.4. 0 72 % sulphanilamide hydrochloride solution:  Dissolve 2 70 g of sulphanilamide in 800 ml of water by warming. Cool and add 100 ml of concentrated hydrochloric acid while stirring. Dilute with water to 1 000 ml.       4.5. 5N hydrochloric acid       4.6. N-1-naphthyl reagent:  This solution must be prepared on the day of use. Dissolve 0 71 g of N-1-naphthylethylenediamine dihydrochloride in water and dilute with water to 100 ml.          5. APPARATUS    5.1. Analytical balance       5.2. Volumetric flasks of 100, 250, 500 and 1 000 ml       5.3. Bulb or graduated pipettes  5.4. Measuring cylinders of 100 ml       5.5. Fluted filter papers, free of nitrite, diameter 15 cm       5.6. Water-bath       5.7. Spectrophotometer with optical cells of 1 cm path-length       5.8. pH meter       5.9. Microburette of 10 ml       5.10. Beakers of 250 ml          6. PROCEDURE    6.1. Weigh about 0 75 g (m gram) to a precision of 0 71 mg of the homogenized sample, transfer with hot distilled water quantitatively into a 250-ml beaker (5.10) and bring the volume to approximately 150 ml with hot distilled water. Place the beaker (5.10) in a water-bath (5.6) at 80 °C for half an hour. During this period, shake the contents occasionally.       6.2. Cool to room temperature and add successively, while stirring, 2 ml of the Carrez I reagent (4.1.1) and 2 ml of the Carrez II reagent (4.1.2).       6.3. Add 1N sodium hydroxide solution (4.3) to bring the pH to 8 73. (Use the pH meter (5.8)). Transfer the contents quantitatively to a 250-ml volumetric flask (5.2) and make up to the mark with distilled water.       6.4. Mix the contents and filter through a fluted filter paper (5.5).       6.5. Pipette (5.3) a suitable aliquot (V ml) of the clear filtrate, but not more than 25 ml, into a 100-ml volumetric flask (5.2) and add distilled water to a volume of 60 ml.       6.6. After mixing, add 10.0 ml of sulphanilamide hydrochloride solution (4.4) and then 6 70 ml of 5N hydrochloric acid (4.5). Mix and allow to stand for five minutes. Add 2 70 ml of N-1-naphthyl reagent (4.6), mix and allow to stand for three minutes. Dilute with water to the mark and mix.       6.7. Prepare a blank test by repeating the operations 6.5 and 6.6 without addition of the N-1-naphthyl reagent (4.6).       6.8. Measure (5.7) the optical density at 538 nm of the solution obtained under 6.6 using the blank solution (6.7) as a reference.       6.9. Read from the calibration graph (6.10) the sodium nitrite content in micrograms per 100 ml of the solution (m1 micrograms) that corresponds to the optical density measured in 6.8.       6.10. Using the 10 ¶g per ml sodium nitrite solution (4.2), prepare a calibration graph for concentrations of 0, 20, 40, 60, 80, 100 ¶g of sodium nitrite per 100 ml.          7. CALCULATION  Calculate the sodium nitrite content of the sample in percent by mass with the aid of the following formula:  >PIC FILE= "T0050759">    8. REPEATABILITY (1)  For a content of about 0 72 % m/m of sodium nitrite the difference between the results of two determinations in parallel carried out on the same sample should not exceed an absolute value of 0.005 %.    IV. IDENTIFICATION AND DETERMINATION OF FREE FORMALDEHYDE   1. PURPOSE AND SCOPE  This method describes the identification and the determination of free formaldehyde. It is applicable to all cosmetic products and comprises three parts:  1.1. Identification   1.2. Determination by pentane-2,4-dione colorimetry  This method is inadequate when the formaldehyde is combined or polymerized, as in the case of formaldehyde donors. If the result exceeds the maximum permitted concentration, the following method must be used.   1.3. Determination with bisulphite  With this method, formaldehyde in most combined or polymeric compounds is not taken into account. However, certain unstable combinations (hexamethylene tetramine, for example) are determined. Moreover, the alkalinity measurement is difficult in the presence of a buffer solution.      2. DEFINITION  The free formaldehyde content of the sample determined according to this method is expressed as percentage by mass.   3. PRINCIPLE  3.1. Part I - Identification  Formaldehyde in a sulphuric acid medium turns Schiff's reagent pink or mauve.   3.2. Part II - Determination by pentane-2,4-dione  Formaldehyde reacts with pentane-2,4-dione in the presence of ammonium acetate to form 3,5-diacetyl-1,4-dihydrolutidine. This is extracted with butan-1-ol and the absorbance of the extract is measured at 410 nm.  (1) See Norm ISO 5725.    3.3. Part III - Determination with bisulphite  Formaldehyde reacts with the sulphite in an acid medium at 0 °C to form an addition compound. The excess protons are titrated with sodium hydroxide. The protons consumed form the basis of the calculation for determining the quantity of formaldehyde. A blank test without sulphite enables the alkalinity or acidity of the medium to be measured.      4. REAGENTS  All the reagents should be of analytical purity.  4.1. Glacial acetic acid   4.2. Anhydrous ammonium acetate   4.3. Butan-1-ol   4.4. Sulphuric acid, about 2N   4.5. Freshly prepared 0 71 M sodium sulphite solution   4.6. Schiff's reagent 100 mg of fuchsine is weighed into a beaker and dissolved in 75 ml of water at 80 °C.  After cooling, add 2 75 g of sodium sulphite heptahydrate (Na2SO3 77H2O) and 1 75 ml of concentrated hydrochloric acid (d204 = 1 719) Make up to 100 ml.  (This reagent is unsuitable for use after two weeks.)   4.7. Pentane-2,4-dione reagent  In a 1 000-ml volumetric flask dissolve: >PIC FILE= "T0050760">   Make up to 1 000 ml with water (pH of solution : about 6 74)  This reagent must be freshly prepared.   4.8. Standard sulphuric acid solution, 0 71N   4.9. Standard sodium hydroxide solution, 0 71N   4.10. Iodine solution, 0 71N   4.11. Sodium thiosulphate, 0 71N   4.12. Formaldehyde stock solution  Pour 5 g of 37 to 40 % formaldehyde solution into 1 000-ml volumetric flask and make up to 1 000 ml.  Determine the strength of this solution as follows : Remove 10 700 ml ; add 25 700 ml of a standard 0 71N iodine solution (4.10) and 10 ml of a 1N sodium hydroxide solution.  Allow to stand for five minutes.  Add 11 ml of 1N HCl and titrate the excess standard 0 71N iodine solution (4.10) with standard 0 71N sodium thiosulphate solution (4.11), using starch solution as indicator.  1 ml of 0 71N iodine solution (4.10) is equivalent to 1 75 mg formaldehyde.   4.13. Formaldehyde reference solution  Pipette 5 700 ml of stock solution (4.12) into a 100-ml graduated flask and make up to 100 ml with demineralized water.  Pipette 5 700 ml of the above solution into a 500-ml graduated flask and make up to 500 ml with demineralized water.  1 ml of this solution contains about 1 ¶g of formaldehyde.  Calculate the exact content.   4.14. Thymolphthalein solution, 0 71 g/100 ml of 50 % ethanol   4.15. Reference reagent solution : as reagent 4.7 but without the pentane-2,4-dione      5. APPARATUS  5.1. Standard laboratory apparatus   5.2. Phase separation filter, Whatman 1 PS (or equivalent)   5.3. Centrifuge  5.4. Spectrophometer   5.5. Glass cells with an optical path of 1 cm   5.6. Potentiometer with chart recorder   5.7. Glass/calomel electrodes (it is recommended that special low-temperature electrodes be used).      6. PROCEDURE  6.1. Identification    6.1.1. Weigh 2 g of the test sample into a 10-ml beaker.       6.1.2. Add two drops of 2N sulphuric acid (4.4) and 2 ml of Schiff's reagent (4.6) (this reagent must be absolutely colourless when it is used).  Shake and leave to stand for five minutes.       6.1.3. If a pink or mauve tint is observed within the five minutes, the formaldehyde is present in excess of 0 701 % and is to be determined by the procedure 6.2 and, if necessary, by procedure 6.3.          6.2. Determination by pentane-2,4-dione colorimetry    6.2.1. Sample solution      6.2.1.1. Into a 100-ml volumetric flask, weigh, to within 0 7001 g, a quantity (m in grams) of the test sample corresponding to a presumed quantity of formaldehyde of about 150 micrograms.           6.2.1.2. Make up to 100 ml with demineralized water and mix.           6.2.1.3. To a 50-ml Erlenmeyer flask add:  10 700 ml solution from 6.2.1.2, 5 700 ml pentane-2,4-dione reagent (4.7), demineralized water to a final volume of 30 ml.                  6.2.2. Reference solution  Possible interference due to background colour in the test sample is eliminated by the use of this reference solution.  To a 50-ml Erlenmeyer flask add:  10 700 ml solution from 6.2.1.2, 5 700 ml reference reagent solution (4.15), demineralized water to a final volume of 30 ml.       6.2.3. Blank solution  To a 50-ml Erlenmeyer flask add:  5 700 ml pentane-2,4-dione reagent (4.7), demineralized water to a final volume of 30 ml.       6.2.4. Determination      6.2.4.1. Shake the flasks from 6.2.1.3, 6.2.2 and 6.2.3 and immerse in a water-bath at 60 °C for exactly 10 minutes. Allow to cool for two minutes in a bath of iced water.            6.2.4.2. Transfer into 50-ml separating funnels containing 10 700 ml of butan-1-ol (4.3). Rinse each flask with 3 to 5 ml of water and add the rinsings to the funnels. Shake the mixture vigorously for exactly 30 seconds. Allow it to separate.           6.2.4.3. Filter into the measurement cells through a phase-separation filter. Centrifuging (5 000 rev./min. for five minutes) is less practical and takes longer.           6.2.4.4. Measure the optical density A1 at 410 nm of the extract of the sample solution from 6.2.1.3 against the extract of the reference solution 6.2.2.           6.2.4.5. Similarly measure the extract of the blank solution from 6.2.3 against butan-1-ol (A2).  Note  All these operations must be carried out within 25 minutes from the moment when the Erlenmeyer flasks are placed in the water-bath at 60 °C                  6.2.5. Calibration curve      6.2.5.1. Into a 50-ml Erlenmeyer flask place:  5 700 ml of the standard solution (4.13), 5 700 ml of the pentane-2,4-dione reagent (4.7), demineralized water to a final volume of 30 ml.           6.2.5.2. Continue as described in Section 6.2.4.5, measure the optical density against butan-1-ol (4.3).           6.2.5.3. Repeat the procedure with 10, 15, 20 and 25 ml of the standard solution.           6.2.5.4. To obtain the zero value proceed as in 6.2.4.5.           6.2.5.5. Construct the calibration curve after subtraction of the zero value (6.2.4.5) from each of the optical densities obtained in 6.2.5.2 and 6.2.5.3. Beers Law is valid up to 30 ¶g of formaldenyde.                     6.3. Determination with bisulphite    6.3.1. Preparation of the test sample      6.3.1.1. For the test  Into a tared beaker weigh to the nearest 0 7001 g a quantity of test sample (m grams) corresponding to a presumed quantity of between 3 and 20 mg of formaldehyde.           6.3.1.2. For the reference test  In a similar manner, weigh a reference test sample (m grams).                  6.3.2. Determination      6.3.2.1. Place 50 700 ml of 0 71M sodium sulphite (4.5) in a 100-ml beaker and add 10 700 ml of 0 71N sulphuric acid (4.8). Shake.           6.3.2.2. Immerse the beaker in a mixture of ice and salt for the purpose of maintaining the temperature of the whole at +2 °C. Pour in test sample 6.3.1.1.           6.3.2.3. Titrate rapidly by potentiometry with 0 71N sodium hydroxide (4.9), shaking continuously and maintaining the temperature between +2 and +4 °C (the neutral point lies between pH 9 and 11). Let V1 be the volume of 0 71N sodium hydroxide (4.9) taken.                   6.3.3. Blank test  Nitrate an additionally prepared solution as in 6.3.2.1 under the conditions described in 6.3.2.  Let V2 be the volume of 0 71N sodium hydroxide (4.9) taken.       6.3.4. Reference test  Determine the acidity or alkalinity of the sample by potentiometric titration with 0 71N sodium hydroxide (4.9) or 0 71N sulphuric acid (4.8) in test sample m'. Let v' be the volume of 0 71N sodium hydroxide taken or sulphuric acid 0 71N.       6.3.5. Notes  Strict observance of the test conditions is important.  It is possible to perform the determination in the presence of thymolphthalein (4.14) as indicator.           7. PRESENTATION OF THE RESULTS  7.1. Calculation for the colorimetric method    7.1.1. Subtract A2 from A1 and read off from the calibration curve (6.2.5.5) the amount C, in micrograms, of formaldehyde in the test solution (6.2.1.3).       7.1.2. Calculate the formaldehyde content of the sample as a percentage by mass (% m/m) with the aid of the following formula: >PIC FILE= "T0050761">           7.2. Calculation for the bisulphite titration method  Relate the volume of 0 71N sodium hydroxide (4.9) or 0 71N sulphuric acid (4.8) taken in the reference test to the mass m: >PIC FILE= "T0050762">   For a neutral product v is, of course, zero.    7.2.1. In the case of an acid product: >PIC FILE= "T0050763">        7.2.2. In the case of an alkaline product: >PIC FILE= "T0050764">           7.3. Remark  If the results of the two methods differ, only the lower figure is to be taken.      8. REPEATABILITY (1)  For a formaldehyde content of 0 72 % the difference between the results of two determinations in parallel carried out on the same sample should not exceed 0 7005 % for the colorimetric method and 0 705 % for the bisulphite method.  (1) See Norm ISO 5725.      V. DETERMINATION OF RESORCINOL IN SHAMPOOS AND HAIR LOTIONS   1. PURPOSE AND SCOPE  This method specifies the gas chromatographic determination of resorcinol in shampoos and hair lotions. The method is suitable for concentrations of 0 71 up to 2 70 % by mass in the sample.   2. DEFINITION  The content of resorcinol in the sample as determined by this method is expressed as percentage by mass.   3. PRINCIPLE  Resorcinol and 3,5-dihydroxytoluene, (5-methylresorcinol) added as an internal standard, are separated from the sample by thin-layer chromatography. Both compounds are isolated by scraping their spots from the thin-layer plate and extracting with methanol. Finally the extracted compounds are dried, silylated and determined by gas chromatography.   4. REAGENTS  All reagents must be of analytical grade.  4.1. Hydrochloric acid 25 % (m/m)   4.2. Methanol   4.3. Ethanol 96 % (v/v)   4.4. Ready made silica gel TLC sheets (plastic or aluminium) with fluorescent indicator. Deactivate as follows : spray ordinary pre-coated silica sheets with water until glazed. Allow the sprayed plates to dry in air at room temperature for one to three hours.  Note  If plates are not deactivated losses of resorcinol can occur by irreversible adsorption on silica.   4.5. Developing solvent ; acetone - chloroform - acetic acid (20 : 75 : 5 by volume).   4.6. Resorcinol standard solution ; dissolve 400 mg resorcinol in 100 ml of 96 % ethanol (4.3) (1 ml corresponds to 4 000 ¶g resorcinol).   4.7. Internal standard solution ; dissolve 400 mg 3,5-dihydroxytoluene (DHT) in 100 ml of 96 % ethanol (4.3) (1 ml corresponds to 4 000 ¶g DHT).   4.8. Standard mixture ; mix 10 ml of solution 4.6 and 10 ml of solution 4.7 in a 100-ml volumetric flask, make up to the mark with 96 % ethanol (4.3) and mix (1 ml corresponds to 400 ¶g resorcinol and 400 ¶g DHT).   4.9 Silylating agents:  4.9.1. N, O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA)   4.9.2. Hexamethyldisilazane (HMDS)  4.9.3. Trimethylchlorosilane (TMCS)         5. APPARATUS  5.1. Usual thin-layer and gas chromatography equipment   5.2. Glassware      6. PROCEDURE  6.1. Preparation of the sample  6.1.1. Weigh accurately into a 150-ml beaker a test portion (m grams) of the product which contains approximately 20 to 50 mg resorcinol.   6.1.2. Acidify with hydrochloric acid (4.1) until the mixture is acid (approximately 2 to 4 ml are needed), add 10 ml (40 mg DHT) of the internal standard solution (4.7) and mix. Transfer to a 100-ml volumetric flask with ethanol (4.3) make up to the mark with ethanol and mix.   6.1.3. Apply 250 ¶l of the solution (6.1.2) to a deactivated silica sheet (4.4) as a continuous line of approximately 8 cm length. Take care to get the line as narrow as possible.   6.1.4. Apply 250 ¶l of the standard mixture (4.8) to the same plate in the same way (6.1.3).   6.1.5. Spot on two points of the starting line 5 ¶l of each of the solutions 4.6 and 4.7 to aid localizing after plate development.   6.1.6. Develop the plate in an unlined (unsaturated) tank filled with developing solvent 4.5 until the solvent front has reached a line 12 cm from the starting line ; usually this takes about 45 minutes. Air-dry the plate and localize the resorcinol/DHT-zone under short wave UV-light (254 nm). The two compounds have approximately the same Rf values. Mark the bands with a pencil at 2 mm distance from the outside dark borderline of the bands. Remove these zones and collect the adsorbent of each band in a 10-ml bottle.   6.1.7. Extract the adsorbent containing the sample and the absorbent containing the standard mixture each in the following way:  add 2 ml methanol (4.2) and extract for one hour with continuous stirring. Filter the mixture and repeat the extraction for another 15 minutes with 2 ml methanol.   6.1.8. Combine the extracts and evaporate the solvent by drying overnight in a vacuum desiccator filled with a suitable desiccant. Do not apply any heat.   6.1.9. Silylate the residues (6.1.8) either as indicated under 6.1.9.1 or 6.1.9.2.    6.1.9.1. Add 200 ¶l BSTFA (4.9.1) with a microsyringe and leave the mixture in a closed vessel for 12 hours at room temperature.       6.1.9.2. Add successively 200 ¶l HMDS (4.9.2) and 100 ¶l TMCS (4.9.3) with a microsyringe and heat the mixture for 30 minutes at 60 °C in a closed vessel. Cool the mixture.             6.2. Gas chromatography  6.2.1. Chromatographic conditions  The column must yield a resolution, R, equal to or better than 1 75, where: >PIC FILE= "T0050765">    The following column and gas chromatographic conditions have been found suitable: >PIC FILE= "T0050766">   For settings of hydrogen and air flow follow the manufacturer's instructions.   6.2.2. Inject 1 to 3 ¶l of the solutions obtained under 6.1.9 in the gas chromatograph. Carry out five injections for each solution (6.1.9), measure the peak areas, average these and calculate the peak area ratio : S = peak area resorcinol/peak area DHT.         7. CALCULATION  The concentration of resorcinol in the sample, expressed as % by mass (% m/m), is given by: >PIC FILE= "T0050767">    8. REPEATABILITY (1)  For a resorcinol content of about 0 75 % the difference between the results of two determinations in parallel carried out on the same sample should not exceed an absolute value of 0 7025 %.     VI. DETERMINATION OF METHANOL IN RELATION TO ETHANOL OR PROPAN-2-OL   1. PURPOSE AND SCOPE  This method describes the gas chromatographic analysis of methanol in all kinds of cosmetic products (including aerosols).  Relative levels of 0 to 10 % can be determined.   2. DEFINITION  The methanol content determined according to this method is expressed in % by mass of methanol in relation to ethanol or propan-2-ol.   3. PRINCIPLE  The determination is carried out by gas chromatography.  (1) See Norm ISO 5725.    4. REAGENTS  Use analytical grade reagents.  4.1. Methanol   4.2. Ethanol absolute   4.3. Propan-2-ol   4.4. Chloroform, freed from alcohols by washing with water      5. APPARATUS  5.1. Gas chromatograph:  with Katharometer detector for aerosol samples,  with flame ionization detector for non-aerosol samples.   5.2. Volumetric flasks, 100 ml   5.3. Pipettes, 2 ml, 20 ml, 0 to 1 ml   5.4. Microsyringes 0 to 100 ¶l and 0 to 5 ¶l  and (only for aerosol samples) special gas-tight syringe with sliding valve, (see sampling procedure Figure 5 (1).      6. PROCEDURE  6.1. Sample preparation  6.1.1. Aerosol products are sampled according to Chapter II of the Annex to Commission Directive 80/1335/EEC of 22 December 1980 (1) and then analyzed by gas chromatography under the conditions of 6.2.1.   6.1.2. Non-aerosol products sampled according to the abovementioned Chapter II are diluted with water to a level of 1 to 2 % ethanol or propan-2-ol, and then analyzed by gas chromatography under the conditions of 6.2.2.      6.2. Gas chromatography  6.2.1. For aerosol samples the katharometer detector is used.  6.2.1.1. The column is filled with 10 % Hallcomid M18 on Chromosorb WAW 100 to 200 mesh.   6.2.1.2. The column must yield a resolution, R, equal to or better than 1 75, where: >PIC FILE= "T0050768">    6.2.1.3. The following conditions allow this resolution to be achieved: >PIC FILE= "T0050769">   (1) OJ No L 383, 31.12.1980, p. 27.     >PIC FILE= "T0050770">                 6.2.2. For non-aerosol samples:  6.2.2.1. The column is filled with Chromosorb 105 or Porapak QS and the flame ionization detector is used.   6.2.2.2. The column must yield a resolution, R, equal to or better than 1 75, where: >PIC FILE= "T0050771">    6.2.2.3. This resolution has been achieved using the following conditions: >PIC FILE= "T0050772">       7. STANDARD GRAPH  7.1. For the gas chromatography procedure 6.2.1 (Hallcomid M18 column) use the following standard mixtures. Prepare these mixtures by measuring with pipettes but find the exact amount by immediate weighing of the pipette or flask after each addition. >PIC FILE= "T0050773">   Inject 2 to 3 ¶l into the chromatograph using conditions of 6.2.1.  Calculate peak areas ratio (methanol/ethanol) or (methanol/propan-2-ol) of each mixture. Plot standard graph using:  X-axis : % methanol in relation to ethanol or propan-2-ol,  Y-axis : peak area ratio (methanol/ethanol) or (methanol/propan-2-ol).    7.2. For the gas chromatography procedure 6.2.2 (Porapak QS or Chromosorb 105) use the following standard mixtures. Prepare these mixtures by measuring with microsyringe and pipette, but find the exact amount by immediate weighing of the pipette or flask after each addition. >PIC FILE= "T0050774">   Inject 2 to 3 ¶l into the chromatograph using conditions of 6.2.2.  Calculate peak area ratio (methanol/ethanol) or (methanol/propan-2-ol) of each mixture. Plot standard graph using:  X-axis : % methanol in relation to ethanol or propan-2-ol,  Y-axis : peak area ratio (methanol/ethanol) or (methanol/propan-2-ol).   7.3. The standard graph must be a straight line.      8. REPEATABILITY (1)  For a methanol content of 5 % relative to ethanol or propan-2-ol, the difference between the results of two determinations in parallel carried out on the same sample should not exceed 0 725 %.  (1) See Norm ISO 5725.


Avis juridique important

|

32002L0017

Commission Directive 2002/17/EC of 21 February 2002 amending Directive 90/128/EEC relating to plastic materials and articles intended to come into contact with foodstuffs (Text with EEA relevance)

Official Journal L 058 , 28/02/2002 P. 0019 - 0024

Commission Directive 2002/17/ECof 21 February 2002amending Directive 90/128/EEC relating to plastic materials and articles intended to come into contact with foodstuffs(Text with EEA relevance)THE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Community,Having regard to Council Directive 89/109/EEC of 21 December 1988 on the approximation of the laws of the Member States relating to materials and articles intended to come into contact with foodstuffs(1), and in particular Article 3 thereof,After consulting the Scientific Committee on Food,Whereas:(1) On the basis of the new information available to the Scientific Committee on Food, certain monomers provisionally permitted at national level as well as other monomers requested for use following the adoption of Commission Directive 90/128/EEC of 23 February 1990 relating to plastic materials and articles intended to come into contact with foodstuffs(2), as last amended by Directive 2001/62/EC(3), may be included in the Community list of permitted substances in Annex II to Directive 90/128/EEC.(2) Annex III to Directive 90/128/EEC contains an incomplete list of additives which may be used in the manufacture of plastics materials and articles. That list should be amended so as to include other additives evaluated by the Scientific Committee on Food.(3) For certain substances, the restrictions already established at Community level should be amended on the basis of the information available.(4) The current list of additives is an incomplete list inasmuch as it does not contain all the substances, which are currently accepted in one or more Member States. Accordingly, these substances continue to be regulated by national laws only pending a decision on inclusion in the Community list.(5) This Directive establishes specifications for only a few substances. The other substances, which may require specifications, therefore remain regulated in this respect by national laws only pending a decision at Community level.(6) Directive 90/128/EEC should therefore be amended accordingly.(7) The measures provided for in this Directive are in accordance with the opinion of the Standing Committee on Foodstuffs,HAS ADOPTED THIS DIRECTIVE:Article 1Annexes II, III, V and VI to Directive 90/128/EEC are amended as set out in the Annex to this Directive.Article 2Member States shall adopt and publish, by 28 February 2003 at the latest, the provisions necessary to comply with this Directive. They shall forthwith inform the Commission thereof.They shall apply those provisions in such a way as to:(a) permit the trade in and use of plastic materials and articles intended to come into contact with foodstuffs and complying with this Directive, from 1 March 2003;(b) prohibit the manufacture and importation into the Community of plastic materials and articles intended to come into contact with foodstuffs and which do not comply with this Directive, from 1 March 2004. However, for materials and articles which contain divinylbenzene and do not comply with the restriction set in this Directive, Member States shall prohibit their manufacture and importation into the Community as from 1 March 2003.When Member States adopt these provisions, they shall contain a reference to this Directive or be accompanied by such a reference on the occasion of their official publication. Member States shall determine how such reference is to be made.Article 3This Directive shall enter into force on the 20th day following its publication in the Official Journal of the European Communities.Article 4This Directive is addressed to the Member States.Done at Brussels, 21 February 2002.For the CommissionDavid ByrneMember of the Commission(1) OJ L 40, 11.2.1989, p. 38.(2) OJ L 75, 21.3.1990, p. 19.(3) OJ L 221, 17.8.2001, p. 18.ANNEXThe Annexes to Directive 90/128/EEC are amended as follows:1. Annex II is amended as follows:(a) In point 8:(i) The definition of QM(T) is replaced by the following: "QM(T) = Maximum permitted quantity of the "residual" substance in the material or article expressed as total of moiety or substance(s) indicated. For the purpose of this Directive the quantity of the substance in the material or article should be determined by a validated method of analysis. If such a method does not currently exist, an analytical method with appropriate performance characteristics at the specified limit may be used, pending the development of a validated method;"(ii) the following text is inserted after QM(T): "QMA = Maximum permitted quantity of the "residual" substance in the finished material or article expressed as mg per 6 dm2 of the surface in contact with foodstuffs. For the purpose of this Directive the quantity of the substance in the surface of the material or article should be determined by a validated method of analysis. If such a method does not currently exist, an analytical method with appropriate performance characteristics at the specified limit may be used, pending the development of a validated method;QMA(T) = Maximum permitted quantity of the "residual" substance in the material or article expressed as mg of total of moiety or substance(s) indicated per 6 dm2 of the surface in contact with foodstuffs. For the purpose of this Directive the quantity of the substance in the surface of the material or article should be determined by a validated method of analysis. If such a method does not currently exist, an analytical method with appropriate performance characteristics at the specified limit may be used, pending the development of a validated method;"(iii) The definitions of SML and SML(T) are replaced by the following: "SML = Specific migration limit in food or in food simulant, unless it is specified otherwise. For the purpose of this Directive the specific migration of the substance should be determined by a validated method of analysis. If such a method does not currently exist, an analytical method with appropriate performance characteristics at the specified limit may be used, pending the development of a validated method;SML(T) = Specific migration limit in food or in food simulant expressed as total of moiety or substance(s) indicated. For the purpose of this Directive the specific migration of the substances should be determined by a validated method of analysis. If such a method does not currently exist, an analytical method with appropriate performance characteristics at the specified limit may be used, pending the development of a validated method."(b) Section A is amended as follows:(i) The following monomers and other starting substances are inserted: >TABLE>(ii) For the following monomers and other starting substances the content of the column "Restrictions and/or specifications" is replaced by the following: >TABLE>(iii) The following monomers and other starting substances are transferred from Section B to Section A: >TABLE>2. Annex III is amended as follows:(a) The table of Section A is amended as follows:(i) The following additives are inserted: >TABLE>(ii) For the following additives the content of column "Restriction and/or specifications" is replaced by the following: >TABLE>(iii) The following additive is deleted >TABLE>(b) The table of Section B is amended as follows:(i) The following additives are inserted: >TABLE>(ii) For the following additives the content of column "Restriction and/or specifications" is replaced by the following: >TABLE>3. Annex V is amended as follows: The following specifications are inserted in the table of Part B: >TABLE>4. Annex VI is amended as follows:(a) The notes (12) and (13) are replaced by the following: "(12) SML(T) in this specific case means that the restriction shall not be exceeded by the sum of the migration levels of the following substances mentioned as PM/REF. Nos: 36720, 36800, 36840 and 92000.(13) SML(T) in this specific case means that the restriction shall not be exceeded by the sum of the migration levels of the following substances mentioned as PM/REF. Nos: 39090 and 39120."(b) The following notes are added: "(23) SML(T) in this specific case means that the restriction shall not be exceeded by the sum of the migration levels of the following substances mentioned as PM/REF. Nos: 13620, 36840, 40320 and 87040.(24) SML(T) in this specific case means that the restriction shall not be exceeded by the sum of the migration levels of the following substances mentioned as PM/REF. Nos: 13720 and 40580.(25) SML(T) in this specific case means that the restriction shall not be exceeded by the sum of the migration levels of the following substances mentioned as PM/REF. Nos: 16650 and 51570.(26) QM(T) in this specific case means that the restriction shall not be exceeded by the sum of the residual quantities of the following substances mentioned as PM/REF. Nos: 14950, 15700, 16240, 16570, 16600, 16630, 18640, 19110, 22332, 22420, 22570, 25210, 25240, 25270."