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31993L0039

Council Directive 93/39/EEC of 14 June 1993 amending Directives 65/65/EEC, 75/318/EEC and 75/319/EEC in respect of medicinal products

Official Journal L 214 , 24/08/1993 P. 0022 - 0030 Finnish special edition: Chapter 13 Volume 24 P. 0178  Swedish special edition: Chapter 13 Volume 24 P. 0178

COUNCIL DIRECTIVE 93/39/EEC of 14 June 1993 amending Directives 65/65/EEC, 75/318/EEC and 75/319/EEC in respect of medicinal productsTHE COUNCIL OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community, and in particular Article 100a thereof,  Having regard to the proposal from the Commission (1),  In cooperation with the European Parliament (2),  Having regard to the opinion of the Economic and Social Committee (3),  Whereas it is important to adopt measures with the aim of progressively establishing the internal market over a period expiring on 31 December 1992; whereas the internal market shall comprise an area without internal frontiers in which the free movement  of goods, persons, services and capital is ensured;  Whereas Article 15 (2) of Second Council Directive 75/319/EEC of 20 May 1975 on the approximation of provisions laid down by law, regulation or administrative action relating to proprietary medicinal products (4) provides that the Commission shall  submit to the Council a proposal containing appropriate measures leading towards the abolition of any remaining barriers to the free movement of proprietary medicinal products;  Whereas, in the interest of public health and of the consumer of medicinal products, it is necessary that decisions on the authorization to place medicinal products on the market be exclusively based on the criteria of quality, safety and efficacy;  whereas these criteria have been extensively harmonized by Council Directive 65/65/EEC of 26 January 1965 on the approximation of provisions laid down by law, regulation or administration action relating to medicinal products (5), by Council Directive  75/319/EEC, and by Council Directive 75/318/EEC of 20 May 1975 on the approximation of the laws of the Member States relating to analytical, pharmacotoxicological and clinical standards and protocols in respect of the testing of medicinal products (6);  whereas, however, Member States should exceptionally be able to prohibit the use on their territory of medicinal products which infringe objectively defined concepts of public order or public morality;  Whereas, with the exception of those medicinal products which are subject to the centralized Community authorization procedure established by Council Regulation (EEC) No 2309/93 of 22 July 1993 laying down Community procedures for the authorization and  supervision of medicinal products for human and veterinary use and establishing a European Agency for the Evaluation of Medicinal Products (7), an authorization to place a medicinal product on the market in one Member State ought in principle to be  recognized by the competent authorities of the other Member States unless there are serious grounds for supposing that the authorization of the medicinal product concerned may present a risk to public health; whereas, in the event of a disagreement  between Member States about the quality, the safety or the efficacy of a medicinal product, a scientific evaluation of the matter should be undertaken by the Committee for Proprietary Medicinal Products attached to the European Agency for the Evaluation  of Medicinal Products, leading to a single decision on the area of disagreement binding on the Member States concerned; whereas this decision should be adopted by a rapid procedure ensuring close cooperation between the Commission and the Member States;   Whereas in order better to protect public health and avoid any unnecessary duplication of effort during the examination of application for authorization to place medicinal products on the market, Member States should systematically prepare assessment  reports in respect of each medicinal product which is authorized by them, and exchange the reports upon request; whereas, furthermore, a Member State should be able to suspend the examination of an application for authorization to place a medicinal  product on the market which is currently under active consideration in another Member State with a view to recognizing the decision reached by the latter Member State;  Whereas following the establishment of the internal market, specific controls to guarantee the quality of medicinal products imported from third countries can be waived only if appropriate arrangements have been made by the Community to ensure that the  necessary controls are carried out in the exporting country;  Whereas it is desirable to codify and improve the cooperation and exchange of information between Member States relating to the supervision of medicinal products and in particular the monitoring of adverse reactions under practical conditions of use  through the national pharmacovigilance systems,  HAS ADOPTED THIS DIRECTIVE:  Article 1  Directive 65/65/EEC is hereby amended as follows:  1. Article 3 is replaced by the following:  'Article 3 No medicinal product may be placed on the market of a Member State unless a marketing authorization has been issued by the competent authorities of that Member State in accordance with this Directive or an authorization has been granted in accordance  with Regulation (EEC) No 2309/93 of 22 July 1993 laying down Community procedures for the authorization and supervision of medicinal products for human and veterinary use and establishing a European Agency for the Evaluation of Medicinal Products (*).  The provisions of this Directive shall not affect the powers of the Member States' authorities either as regards the setting of prices for medicinal products or their inclusion in the scope of national health insurance schemes, on the basis of health,  economic and social conditions.  (*) OJ No L 214, 24. 8. 1993, p. 1';  2. the following subparagraph is added between the first and second subparagraphs of Article 4:  'The person responsible for placing medicinal products on the market shall be established in the Community. In respect of medicinal products authorized on the date of implementation of this Directive, the Member State shall if necessary apply this  provision at the time of the five-yearly renewal of the marketing authorization provided for in Article 10.';  3. in the second paragraph of Article 4, points 6 and 11 are replaced by the following:  ' 6. Posology, pharmaceutical form, method and route of administration and expected shelf life.  If applicable, reasons for any precautionary and safety measures to be taken for the storage of the medicinal product, its administration to patients and for the disposal of waste products, together with an indication of any potential risks presented by  the medicinal product for the environment.';  '11. Copies of any authorization obtained in another Member State or in a third country to place the relevant medicinal product on the market, together with a list of those Member States in which an application for authorization submitted in accordance  with this Directive is under examination. Copies of the summary of the product characteristics proposed by the applicant in accordance with Article 4a or approved by the competent authorities of the Member State in accordance with Article 4b. Copies of  the package leaflet proposed in accordance with Article 6 of Directive 92/27/EEC or approved by the competent authorities of the Member State in accordance with Article 10 of the same Directive. Details of any decision to refuse authorization, whether  in the Community or in a third country, and the reasons for such decision.  This information shall be updated on a regular basis';  4. Article 4b is replaced by the following:  'Article 4b When the marketing authorization referred to in Article 3 is issued, the person responsible for placing that product on the market shall be informed, by the competent authorities of the Member State concerned, of the summary of the product  characteristics as approved by it. The competent authorities shall take all necessary measures to ensure that the information given in the summary is in conformity with that accepted when the marketing authorization is issued or subsequently. The  competent authorities shall forward to the European Agency for the Evaluation of Medicinal Products a copy of the authorization together with the summary of the product characteristics referred to in Article 4a.  Furthermore, the competent authorities shall draw up an assessment report and comments on the dossier as regards the results of the analytical and pharmacotoxicological tests and the clinical trials of the medicinal product concerned. The assessment  report shall be udapted whenever new information becomes available which is of importance for the evaluation of the quality, safety or efficacy of the medicinal product concerned.';  5. Article 6 is replaced by the following:  'Article 6 This Directive shall not affect the application of national legislation prohibiting or restricting the sale, supply or use of medicinal products as contraceptives or abortifacients. The Member States shall communicate the national legislation concerned  to the Commission';  6. Article 7 is replaced by the following:  'Article 7 1. Member States shall take all appropriate measures to ensure that the procedure for granting an authorization to place a medicinal product on the market is completed within 210 days of the submission of a valid application.  2. Where a Member State notes that an application for authorization submitted after 1 January 1995 is already under active examination in another Member State in respect of that medicinal product, the Member State concerned may decide to suspend the  detailed examination of the application in order to await the assessment report prepared by the other Member State in accordance with Article 4b.  The Member State concerned shall inform the other Member State and the applicant of its decision to suspend detailed examination of the application in question. As soon as it has completed the examination of the application and reached a decision, the  other Member State shall forward a copy of its assessment report to the Member State concerned.  Within 90 days of the receipt of the assessment report, the Member State concerned shall either recognize the decision of the other Member State and the summary of the product characteristics as approved by it, or, if it considers that there are grounds  for supposing that the authorization of the medicinal product concerned may present a risk to public health (*), it shall apply the procedures set out in Articles 10 to 14 of Directive 75/319/EEC.  (*) The expression "risk to public health " refers to the quality, safety and efficacy of the medicinal product.';  7. insert the following Article 7a:  'Article 7a With effect from 1 January 1998, where a Member State is informed in accordance with point 11 of the second paragraph of Article 4 that another Member State has authorized a medicinal product which is the subject of an application for authorization in  the Member State concerned, that Member State shall forthwith request the authorities of the Member State which has granted the authorization to forward to it the assessment report referred to in the second paragraph of Article 4b.  Within 90 days of the receipt of the assessment report, the Member State concerned shall either recognize the decision of the first Member State and the summary of the product characteristics as approved by it or, if it considers that there are grounds  for supposing that the authorization of the medicinal product concerned may present a risk to public health (*), it shall apply the procedures set out in Articles 10 to 14 of Directive 75/319/EEC.  (*) The expression "risk to public health " refers to the quality, safety and efficacy of the medicinal product';  8. Article 9a is replaced by the following:  'Article 9a After an authorization has been issued, the person responsible for placing the product on the market must, in respect of the methods of preparation and control provided for in points 4 and 7 of the second paragraph of Article 4, take account of  technical and scientific progress and introduce any changes that may be required to enable that medicinal product to be manufactured and checked by means of generally accepted scientific methods. These changes shall be subject to the approval of the  competent authority of the Member State concerned';  9. Article 10 is replaced by the following:  'Article 10 1. Authorization shall be valid for five years and shall be renewable for five-year periods, on application by the holder at least three months before the expiry date and after consideration by the competent authority of a dossier containing in  particular details of the data on pharmacovigilance and other information relevant to the monitoring of the medicinial product.  2. In exceptional circumstances, and following consultation with the applicant, an authorization may be granted subject to certain specific obligations, including:  - the carrying out of further studies following the granting of authorization,  - the notification of adverse reactions to the medicinal product.  These exceptional decisions may be adopted only for objective and verifiable reasons and shall be based on one of the causes referred to in Part 4 (G) of the Annex to Directive 75/318/EEC.' Article 2  In Directive 75/318/EEC, the Committee referred to in Article 2b shall be called 'the Standing Committee on Medicinal Products for Human Use'.  Article 3  Directive 75/319/EEC is hereby amended as follows:  1. Chapter III is replaced by the following:  'CHAPTER III Committee for Proprietary Medicinal Products Article 8 1. In order to facilitate the adoption of common decisions by Member States on the authorization of medicinal products for human use on the basis of the scientific criteria of quality, safety and efficacy, and to achieve thereby the free movement of  medicinal products within the Community, a Committee for Proprietary Medicinal Products, hereinafter referred to as "the Committee ", is hereby set up. The Committee shall be part of the European Agency for the Evaluation of Medicinal Products  established by Council Regulation (EEC) No 2309/93 of 22 July 1993 laying down Community procedures for the authorization and supervision of medicinal products for human and veterinary use and establishing a European Agency for the Evaluation of  Medicinal Products (*), hereinafter referred to as "the Agency ".  2. In addition to the other responsibilities conferred upon it by Community law, the Committee shall examine any question relating to the granting, variation, suspension or withdrawal of marketing authorization for a medicinal product which is submitted  to it in accordance with this Directive.  (*) OJ No L 214, 24. 8. 1993, p. 1.  Article 9 1. In order to obtain the recognition according to the procedures laid down in this Chapter in one or more of the Member States of an authorization issued by a Member State in accordance with Article 3 of Directive 65/65/EEC, the holder of the  authorization shall submit an application to the competent authorities of the Member State or Member States concerned, together with the information and particulars referred to in Articles 4, 4a and 4b of Directive 65/65/EEC. He shall testify that the  dossier is identical to that accepted by the first Member State, or shall identify any additions or amendments it may contain. In the latter case, he shall certify that the summary of the product characteristics proposed by him in accordance with  Article 4a of Directive 65/65/EEC is identical to that accepted by the first Member State in accordance with Article 4b of Directive 65/65/EEC. Moreover he shall certify that all the dossiers filed as part of the procedure are identical.  2. The holder of the marketing authorization shall notify the Committee of this application, inform it of the Member States concerned and of the dates of submission of the application and send it a copy of the authorization granted by the first Member  State. He shall also send the Committee copies of any such authorization which may have been granted by the other Member States in respect of the medicinal product concerned, and shall indicate whether any application for authorization is currently  under consideration in any Member State.  3. Except in cases referred to in Article 7a of Directive 65/65/EEC, before submitting the application, the holder of the authorization shall inform the Member State which granted the authorization on which the application is based that an application  is to be made in accordance with this Directive and shall notify it of any additions to the original dossier; that Member State may require the applicant to provide it with all the particulars and documents necessary to enable it to check that the  dossiers filed are identical.  In addition the holder of the authorization shall request the Member State which granted the initial authorization to prepare an assessment report in respect of the medicinal product concerned, or, if necessary, to update any existing assessment report.  That Member State shall prepare the assessment report, or update it, within 90 days of the receipt of the request.  At the same time as the application is submitted in accordance with paragraph 1 the Member State which granted the initial authorization shall forward the assessment report to the Member State or Member States concerned by the application.  4. Save in the exceptional case provided for in Article 10 (1), each Member State shall recognize the marketing authorization granted by the first Member State within 90 days of receipt of the application and the assessment report. It shall inform the  Member State which granted the initial authorization, the other Member States concerned by the application, the Committee, and the person responsible for placing the medicinal product on the market.  Article 10 1. Notwithstanding Article 9 (4), where a Member State considers that there are grounds for supposing that the authorization of the medicinal product concerned may present a risk to public health (*), it shall forthwith inform the applicant, the Member  State which granted the initial authorization, any other Member States concerned by the application and the Committee. The Member State shall state its reasons in detail and shall indicate what action may be necessary to correct any defect in the  application.  2. All the Member States concerned shall use their best endeavours to reach agreement on the action to be taken in respect of the application. They shall provide the applicant with the opportunity to make his point of view known orally or in writing.  However, if the Member States have not reached agreement within the time limit referred to in Article 9 (4) they shall forthwith refer the matter to the Committee for the application of the procedure laid down in Article 13.  3. Within the time limit referred to in paragraph 2, the Member States concerned shall provide the Committee with a detailed statement of the matters on which they have been unable to reach agreement and the reasons for their disagreement. The applicant  shall be provided with a copy of this information.  4. As soon as he is informed that the matter has been referred to the Committee, the applicant shall forthwith forward to the Committee a copy of the information and particulars referred to in Article 9 (1).  (*) The expression "risk to public health " refers to the quality, safety and efficacy of the medicinal product.  Article 11 If several applications submitted in accordance with Article 4 and 4a of Directive 65/65/EEC have been made for marketing authorization for a particular medicinal product, and Member States have adopted divergent decisions concerning the authorization  of the medicinal product or its suspension or withdrawal from the market, a Member State, or the Commission, or the person responsible for placing the medicinal product on the market may refer the matter to the Committee for application of the procedure  laid down in Article 13.  The Member State concerned, the person responsible for placing the medicinal product on the market or the Commission shall clearly identify the question which is referred to the Committee for consideration and, where appropriate, shall inform the  aforementioned person thereof.  The Member State and the person responsible for placing the medicinal product on the market shall forward to the Committee all available information relating to the matter in question.  Article 12 The Member States or the Commission or the applicant or holder of the marketing authorization may, in specific cases where the interests of the Community are involved, refer the matter to the Committee for the application of the procedure laid down in  Article 13 before reaching a decision on a request for a marketing authorization or on the suspension or withdrawal of an authorization, or on any other variation to the terms of a marketing authorization which appears necessary, in particular to take  account of the information collected in accordance with Chapter Va.  The Member State concerned or the Commission shall clearly identify the question which is referred to the Committee for consideration and shall inform the person responsible for placing the medicinal product on the market.  The Member States and the aforementioned person shall forward to the Committee all available information relating to the matter in question.  Article 13 1. When reference is made to the procedure described in this Article, the Committee shall consider the matter concerned and issue a reasoned opinion within 90 days of the date on which the matter was referred to it.  However, in cases submitted to the Committee in accordance with Articles 11 and 12, this period may be extended by 90 days.  In case of urgency, on a proposal from its Chairman, the Committee may agree to impose a shorter deadline.  2. In order to consider the matter, the Committee may appoint one of its members to act as rapporteur. The Committee may also appoint individual experts to advise it on specific questions. When appointing experts, the Committee shall define their tasks  and specify the time limit for the completion of these tasks.  3. In the cases referred to in Articles 10 and 11, before issuing its opinion, the Committee shall provide the person responsible for placing the medicinal product on the market with an opportunity to present written or oral explanations.  In the case referred to in Article 12, the person responsible for placing the medicinal product on the market may be asked to explain himself orally or in writing.  If it considers it appropriate, the Committee may invite any other person to provide information relating to the matter before it.  The Committee may suspend the time limit referred to in paragraph 1 in order to allow the person responsible for placing the medicinal product on the market to prepare explanations.  4. Where the opinion of the Committee is that:  - the application does not satisfy the criteria for authorization, or - the summary of the product characteristics proposed by the applicant in accordance with Article 4a of Directive 65/65/EEC should be amended, or - the authorization should be granted subject to conditions, with regard to conditions considered essential for the safe and effective use of the medicinal product including pharmacovigilance, or - a marketing authorization should be suspended, varied or withdrawn,  the Agency shall forthwith inform the person responsible for placing the medicinal product on the market. Within 15 days of the receipt of the opinion, the aforementioned person may notify the Agency in writing of his intention to appeal. In that case,  he shall forward the detailed grounds for appeal to the Agency within 60 days of receipt of the opinion. Within 60 days of receipt of the grounds for appeal, the Committee shall consider whether its opinion should be revised, and the conclusions reached  on the appeal shall be annexed to the assessment report referred to in paragraph 5.  5. Within 30 days of its adoption, the Agency shall forward the final opinion of the Committee to the Member States, the Commission and the person responsible for placing the medicinal product on the market together with a report describing the  assessment of the medicinal product and stating the reasons for its conclusions.  In the event of an opinion in favour of granting or maintaining an authorization to place the medicinal product concerned on the market, the following documents shall be annexed to the opinion.  (a) a draft summary of the product characteristics, as referred to in Article 4a of Directive 65/65/EEC;  (b) any conditions affecting the authorization within the meaning of paragraph 4.  Article 14 1. Within 30 days of the receipt of the opinion, the Commission shall prepare a draft of the decision to be taken in respect of the application, taking into account Community law.  In the event of a draft decision which envisages the granting of marketing authorization, the documents referred to in Article 13 (5) (a) and (b) shall be annexed.  Where, exceptionally, the draft decision is not in accordance with the opinion of the Agency, the Commission shall also annex a detailed explanation of the reasons for the differences.  The draft decision shall be forwarded to the Member States and the applicant.  2. A final decision on the application shall be adopted in accordance with the procedure laid down in Article 37b.  3. The rules of procedure of the Committee referred to in Article 37b shall be adjusted to take account of the tasks incumbent upon it in accordance with this Directive.  These adjustments shall involve the following:  - except in cases referred to in the third subparagraph of paragraph 1, the opinion of the Standing Committee shall be obtained in writing,  - each Member State is allowed at least 28 days to forward written observations on the draft decision to the Commission,  - each Member State is able to require in writing that the draft decision be discussed by the Standing Committee, giving its reasons in detail.  Where, in the opinion of the Commission, the written observations of a Member State raise important new questions of a scientific or technical nature which have not been addressed in the opinion of the Agency, the Chairman shall suspend the procedure  and refer the application back to the Agency for further consideration.  The provisions necessary for the implementation of this paragraph shall be adopted by the Commission in accordance with the procedure laid down in Article 37a.  4. A decision adopted in accordance with this Article shall be addressed to the Member States concerned by the matter and to the person responsible for placing the medicinal product on the market. The Member States shall either grant or withdraw  marketing authorization, or vary the terms of a marketing authorization as necessary to comply with the decision within 30 days of its notification. They shall inform the Commission and the Committee thereof.  5. The procedure referred to in Articles 8 to 14 shall not apply in the cases provided for in Article 9 (2) of Council Directive 92/73/EEC of 22 September 1992 widening the scope of Directive 65/65/EEC and 75/319/EEC on the approximation of the laws of  the Member States on medicinal products and laying down additional provisions on homeopathic medicinal products (*).  (*) OJ No L 297, 13. 10. 1992, p. 8.  Article 15 Any application by the person responsible for placing the medicinal product on the market to vary a marketing authorization which has been granted in accordance with the provisions of this Chapter shall be submitted to all the Member States which have  previously authorized the medicinal product concerned.  The Commission shall, in consultation with the Agency, adopt appropriate arrangements for the examination of variations to the terms of a marketing authorization.  These arrangements shall include a notification system or administration procedures concerning minor variations and define precisely the concept of "a minor variation ".  These arrangements shall be adopted by the Commission in the form of an implementing Regulation in accordance with the procedure laid down in Article 37a.  The procedure laid down in Articles 13 and 14 shall apply by analogy to variations made to marketing authorizations for products subject to the Commission's arbitration.  Article 15a 1. Where a Member State considers that the variation of the terms of a marketing authorization which has been granted in accordance with the provisions of this Chapter or its suspension or withdrawal is necessary for the protection of public health, the  Member State concerned shall forthwith refer the matter to the Committee for the application of the products laid down in Articles 13 and 14.  2. Without prejudice to the provisions of Article 12, in exceptional cases, where urgent action is essential to protect public health, until a definitive decision is adopted a Member State may suspend the marketing and the use of the medicinal product  concerned on its territory. It shall inform the Commission and the other Member States no later than the following working day of the reasons for its action.  Article 15b Articles 15 and 15a shall apply by analogy to medicinal products authorized by Member States following an opinion of the Committee given in accordance with Article 4 of Directive 87/22/EEC before 1 January 1995.  Article 15c 1. The Agency shall publish an annual report on the operation of the procedures laid down in this chapter and shall forward that report to the European Parliament and the Council for information.  2. By 1 January 2001, the Commission shall publish a detailed review of the operation of the procedures laid down in this chapter and shall propose any amendments which may be necessary to improve these procedures.  The Council shall decide, under the conditions provided for in the Treaty, on the Commission proposal within one year of its submission.';  2. the third subparagraph of Article 22 (1) is replaced by the following:  'In the case of medicinal products imported from a third country, where appropriate arrangements have been made by the Community with the exporting country to ensure that the manufacturer of the medicinal product applies standards of good manufacturing  practice at least equivalent to those laid down by the Community and to ensure that the controls referred to under (b) have been carried out in the exporting country, the qualified person may be relieved of responsibility for carrying out those  controls.';  3. the following Chapter Va is inserted after Article 29:  'CHAPTER Va Pharmacovigilance Article 29a In order to ensure the adoption of appropriate regulatory decisions concerning the medicinal products authorized within the Community, having regard to information obtained about adverse reactions to medicinal products under normal conditions of use,  the Member States shall establish a pharmacovigilance system. This system shall be used to collect information useful in the surveillance of medicinal products, with particular reference to adverse reactions in human beings, and to evaluate such  information scientifically.  Such information shall be collated with data on consumption of medicinal products.  This system shall also collate information on frequently observed misuse and serious abuse of medicinal products.  Article 29b For the purpose of this Directive, the following definitions shall apply:  - "adverse reaction " means a reaction which is harmful and unintended and which occurs at doses normally used in man for the prophylaxis, diagnosis or treatment of disease or the modification of physiological function,  - "serious adverse reaction " means an adverse reaction which is fatal, life-threatening, disabling, incapacitating, or which results in or prolongs hospitalization,  - "unexpected adverse reaction " means an adverse reaction which is not mentioned in the summary of product characteristics,  - "serious unexpected adverse reaction " means an adverse reaction which is both serious and unexpected.  Article 29c The person responsible for placing the medicinal product on the market shall have permanently and continuously at his disposal an appropriately qualified person responsible for pharmacovigilance.  That qualified person shall be responsible for the following:  (a) the establishment and maintenance of a system which ensures that information about all suspected adverse reactions which are reported to the personnel of the company, and to medical representatives, is collected and collated at a single point within  the Community;  (b) the preparation for the competent authorities of the reports referred to in Article 29d, in such form as may be laid down by those authorities, in accordance with the relevant national or Community guidelines;  (c) ensuring that any request from the competent authorities for the provision of additional information necessary for the evaluation of the benefits and risks afforded by a medicinal product is answered fully and promptly, including the provision of  information about the volume of sales or prescriptions of the medicinal product concerned.  Article 29d 1. The person responsible for placing the medicinal product on the market shall be required to record and to report all suspected serious adverse reactions which are brought to his attention by a health care professional to the competent authorities  immediately, and in any case within 15 days of their receipt at the latest.  2. In addition, the person responsible for placing the medicinal product on the market shall be required to maintain detailed records of all other suspected adverse reactions which are reported to him by a health care professional.  Unless other requirements have been laid down as a condition of the granting of authorization, these records shall be submitted to the competent authorities immediately upon request or at least every six months during the first two years following  authorization, and once a year for the following three years. Thereafter, the records shall be submitted at five-yearly intervals together with the application for renewal of the authorization, or immediately upon request. These records shall be  accompanied by a scientific evaluation.  Article 29e The Member States shall take all appropriate measures to encourage doctors and other health care professionals to report suspected adverse reactions to the competent authorities.  The Member States may impose specific requirements on medical practitioners, in respect of the reporting of suspected serious or unexpected adverse reactions, in particular where such reporting is a condition of the authorization.  Article 29f The Member States shall ensure that reports of suspected serious adverse reactions are immediately brought to the attention of the Agency and the person responsible for placing the medicinal product on the market, and in any case within 15 days of their  notification, at the latest.  Article 29g In order to facilitate the exchange of information about pharmacovigilance within the Community, the Commission, in consultation with the Agency, Member States and interested parties, shall draw up guidance on the collection, verification and  presentation of adverse reaction reports.  This guidance shall take account of international harmonization work carried out with regard to terminology and classification in the field of pharmacovigilance.  Article 29h Where as a result of the evaluation of adverse reaction reports a Member State considers that a marketing authorization should be varied, suspended or withdrawn, it shall forthwith inform the Agency and the person responsible for placing the medicinal  product on the market.  In case of urgency, the Member State concerned may suspend the marketing of a medicinal product, provided the Agency is informed at the latest on the following working day.  Article 29i Any amendments which may be necessary to update provisions of this Chapter to take account of scientific and technical progress shall be adopted in accordance with the procedure laid down in Article 37a.';  4. the following Chapter VIa is inserted after Article 37:  'CHAPTER VIa Standing Committee procedures Article 37a Where the procedure laid down in this Article is to be followed the Commission shall be assisted by the Standing Committee on Medicinal Products for Human Use.  The representative of the Commission shall submit to the Committee a draft of the measures to be taken. The Committee shall deliver its opinion on the draft within a time limit which the Chairman may lay down according to the urgency of the matter. The  opinion shall be delivered by the majority laid down in Article 148 (2) of the Treaty in the case of decisions which the Council is required to adopt on a proposal from the Commission. The votes of the representatives of the Member States within the  Committee shall be weighted in the manner set out in that Article. The Chairman shall not vote.  The Commission shall adopt the measures envisaged if they are in accordance with the opinion of the Committee.  If the measures envisaged are not in accordance with the opinion of the Committee, or if no opinion is delivered, the Commission shall, without delay, submit to the Council a proposal relating to the measures to be taken. The Council shall act by a  qualified majority.  If on the expiry of a period of three months from the date of referral to the Council, the Council has not acted, the proposed measures shall be adopted by the Commission.  Article 37b Where the procedure laid down in this Article is to be followed the Commission shall be assisted by the Standing Committee on Medicinal Products for Human Use.  The representative of the Commission shall submit to the Committee a draft of the measures to be taken. The Committee shall deliver its opinion on the draft within a time limit which the Chairman may lay down according to the urgency of the matter. The  opinion shall be delivered by the majority laid down in Article 148 (2) of the Treaty in the case of decisions which the Council is required to adopt on a proposal from the Commission. The votes of the representatives of the Member States within the  Committee shall be weighted in the manner set out in that Article. The Chairman shall not vote.  The Commission shall adopt the measures envisaged if they are in accordance with the opinion of the Committee.  If the measures envisaged are not in accordance with the opinion of the Committee, or if no opinion is delivered, the Commission shall, without delay, submit to the Council a proposal relating to the measures to be taken. The Council shall act by a  qualified majority.  If on the expiry of a period of three months from the date of referral to the Council, the Council has not acted, the proposed measures shall be adopted by the Commission, save where the Council has decided against the said measures by a simple  majority.';  5. in Article 19a of Directive 75/319/EEC the reference to Article 2c of Directive 75/318/EEC shall be replaced by a reference to Article 37a.  Article 4  Member States shall take all appropriate measures to comply with this Directive, with the exception of Article 1 (7), before 1 January 1995. They shall forthwith inform the Commission thereof.  Member States shall take all appropriate measures to comply with Article 1 (7) of this Directive before 1 January 1998. They shall forthwith inform the Commission thereof.  When Member States adopt these provisions, they shall contain a reference to this Directive or shall be accompanied by such reference at the time of their official publication. The methods of making such a reference shall be laid down by Member States.   Member States shall communicate to the Commission the text of the provisions of national law which they adopt in the field governed by this Directive.  Article 5  This Directive is addressed to the Member States.  Done at Luxembourg, 14 June 1993.  For the Council The President J. TROEJBORG (1) OJ No C 330, 31. 12. 1970, p. 18, and OJ No C 310, 30. 11. 1991, p. 22.(2) OJ No C 183, 15. 7. 1991, p. 187, and OJ No C 150, 31. 5. 1993.(3) OJ No C 269, 14. 10. 1991, p. 84.(4) OJ No L 147, 9. 6. 1975, p. 13. Directive last amended by  Directive 92/27/EEC (OJ No L 113, 30. 4. 1992, p. 8).(5) OJ No 22, 9. 2. 1965, p. 369/65. Directive last amended by Directive 92/27/EEC (OJ No L 113, 30. 4. 1992, p. 8).(6) OJ No L 147, 9. 6. 1975, p. 1. Directive last amended by Commission Directive  91/507/EEC (OJ No L 270, 26. 9. 1991, p. 32).(7) See page 1 of this Official Journal.


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32001L0053

Commission Directive 2001/53/EC of 10 July 2001 amending Council Directive 96/98/EC on marine equipment (Text with EEA relevance)

Official Journal L 204 , 28/07/2001 P. 0001 - 0028

Commission Directive 2001/53/ECof 10 July 2001amending Council Directive 96/98/EC on marine equipment(Text with EEA relevance)THE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Community, and in particular Article 80(2) thereof,Having regard to Council Directive 96/98/EC of 20 December 1996 on marine equipment(1), as amended by Commission Directive 98/85/EC(2), and in particular Article 17, the first and second indents thereof,Whereas:(1) For the purposes of Directive 98/96/EC, the international conventions, including the 1974 SOLAS Convention, and testing standards are those, together with their amendments, in force on the date of the adoption of that Directive.(2) Amendments to the SOLAS Convention and to other international conventions and new testing standards have entered into force since the adoption of that Directive or will enter into force shortly.(3) New rules regarding the equipment to be placed on board ships have been laid down by those instruments.(4) Directive 96/98/EC should be amended accordingly.(5) The measures provided for in this Directive are in accordance with the opinion of the Committee set up by Article 12 of Council Directive 93/75/EEC(3),HAS ADOPTED THIS DIRECTIVE:Article 1Directive 96/98/EC is hereby amended as follows:1. Article 2 is amended as follows:In points (c), (d) and (n), the words "on 1 January 1999" are replaced by "on 1 January 2001".2. Annex A is replaced by the text in the Annex to this Directive.Article 2Equipment listed as "new item" under the heading "item designation" of Annex A.1, and manufactured before the date referred to in Article 3(1), may be placed on the market and on board a Community ship, the certificates of which were issued by or on behalf of a Member State in accordance with international conventions, during the two years following that date if it was manufactured in accordance with procedures for type-approval already in force within the territory of that Member State before the date of the adoption of this Directive.Article 31. Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive not later than six months after its date of entry into force. They shall forthwith notify the Commission thereof.When Member States adopt those 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.2. Member States shall communicate to the Commission the provisions of national law, which they adopt in the field covered by this Directive.Article 4This Directive shall enter into force on the 20th day following its publication in the Official Journal of the European Communities.Done at Brussels, 10 July 2001.For the CommissionLoyola De PalacioVice-President(1) OJ L 46, 17.2.1997, p. 25.(2) OJ L 315, 25.11.1998, p. 14.(3) OJ L 247, 5.10.1993, p. 19.ANNEX"ANNEX AANNEX A.1: EQUIPMENT FOR WHICH DETAILED TESTING STANDARDS ALREADY EXIST IN INTERNATIONAL INSTRUMENTSNotes applicable to the whole of Annex A.1General:in addition to the testing standards specifically mentioned, a number of provisions, which must be checked during type-examination (type-approval) as referred to in the modules for conformity assessment in Annex B, are to be found in the applicable requirements of the international conventions and the relevant resolutions and circulars of the IMO.Column 5:where IMO resolutions are cited, only the testing standards contained in relevant parts of the Annexes to the resolutions are applicable and exclude the provisions of the resolutions themselves.Column 5:for the purpose of identifying correctly the relevant standards, the test reports and the appropriate type-approval certificates shall specify the applied standard and its version as identified in the column.Column 5:where two sets of testing standards are indicated (separated by a ";"), each set fulfils all the testing requirements to meet IMO performance standards. Thus the testing of an item based on one of the sets is sufficient to demonstrate compliance with the requirements of the relevant international instruments.Column 6:where module H appears, module H plus design-examination certificate is to be understood.1. Life-saving appliances>TABLE>2. Marine-pollution prevention>TABLE>3. Fire protection>TABLE>4. Navigation equipmentNotes for Annex A.1, section 4, Navigation equipmentColumn 4:ITU recommendations cited are those referred to in the international conventions and the relevant resolutions and circulars of the IMO.Column 5:Wherever reference is made to EN/IEC 61162, the relevant product testing standard shall be verified to define the applicable part of EN/IEC 61162.>TABLE>5. Radio-communication equipmentNotes for Annex A.1, section 5, Radio-communication equipmentColumn 4:ITU recommendations cited are those referred to in the international conventions and the relevant resolutions and circulars of the IMO.Column 5:In case of conflicting requirements between IMO MSC/Circ. 862, cited for several items, and the product testing standards, the IMO MSC/Circ. 862 requirements shall take precedence.Column 5:Wherever reference is made to EN/IEC 61162, the relevant product testing standard shall be verified to define the applicable part of EN/IEC 61162.>TABLE>Annex A.2: EQUIPMENT FOR WHICH NO DETAILED TESTING STANDARDS EXIST IN INTERNATIONAL INSTRUMENTS1. Life-saving appliances>TABLE>2. Marine-pollution preventionp.m.3. Fire protection>TABLE>4. Navigation equipmentNotes for Annex A.2, section 4, Navigation equipmentColumns 3 and 4:References to SOLAS Chapter V are to SOLAS 1974 as amended by MSC 73 and entering into force on 1 July 2002.Column 4:ITU recommendations cited are those referred to in the international conventions and the relevant resolutions and circulars of the IMO.>TABLE>5. Radio-communication equipmentNotes for Annex A.2, section 5, Radio-communication equipmentColumn 4:ITU recommendations cited are those referred to in the international conventions and the relevant resolutions and circulars of the IMO.>TABLE>6. Equipment required under Colreg 72>TABLE>7. Bulk carrier safety equipment>TABLE>"


Avis juridique important

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31995L0008

Commission Directive 95/8/EC of 10 April 1995 amending Directive 77/535/EEC on the approximation of the laws of Member States relating to methods of sampling and analysis for fertilizers (Methods of analysis for trace elements at a concentration greater than 10 %)

Official Journal L 086 , 20/04/1995 P. 0041 - 0057

COMMISSION DIRECTIVE 95/8/EC of 10 April 1995 amending Directive 77/535/EEC on the  approximation of the laws of Member States relating to methods of sampling and analysis for  fertilizers (Methods of analysis for trace elements at a concentration greater than 10  %) THE COMMISSION OF THE EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws  of the Member States relating to fertilizers  (1), as last amended by Council Directive 89/530/EEC   (2), and in particular Article 9 (2) thereof, Whereas Article 8a of the Treaty establishes an area without internal frontiers in which the free  movement of goods, persons, services and capital in ensured; Whereas Directive 89/530/EEC supplement and amends Directive 76/116/EEC in respect of the trace  elements boron, cobalt, copper, iron, manganese, molybdendum and zinc in fertilizers; Whereas Commission Directive 77/535/EEC  (3), as last amended by Directive 93/1/EEC  (4), provides  for official controls for Community fertilizers for the purpose of checking compliance with the  requirements imposed by the Community provisions concerning the quality and composition of  fertilizers; whereas Directive 77/535/EEC should be supplemented so that fertilizers to which  Council Directive 89/530/EEC should be supplemented so that fertilizers to which Council Directive  89/530/EEC relates, can also be checked; Whereas, in view of the scope and effects of the proposed action, the Community measures provided  for by this Directive are not only necessary but also indispensable for the attainment of the  stated objectives, whereas these objectives cannot be achieved by Member States individually and  whereas their attainment at Community level is, in fact, already provided for by Directive  76/116/EEC; Whereas the measures provided for in this Directive are in accordance with the opinion of the  Committee on the Adaptation to Technical Progress of the Directives for the Removal of Technical  Barriers to Trade in Fertilizers, HAS ADOPTED THIS DIRECTIVE: Article 1 The text set out in the Annex of this Directive is hereby added to  Annex II of Directive 77/535/EEC. The methods are applicable to Community fertilizers for the determination of each trace element,  the declared contant of which is more than 10  %. Article 2 1.  Member States shall bring into force the provisions necessary to comply with this  Directive by 31 December 1995. They shall immediately inform the Commission thereof. When Member States adopt these provisions, they shall contain a reference to this Directive or  shall be accompanied by such reference at the time of their official publication. The procedure for  such reference shall be adopted by Member States. 2.  Member States shall communicate to the Commission the texts of the provisions of national law  which they adopt in the field covered by the Directive. Article 3 This Directive shall enter into force on the third day following its publication in the  Official Journal of the European Communities. Done at Brussels, 10 April 1995. For the Commission Martin BANGEMANN Member of the Commission  ANNEX 'Methods 10: TRACE ELEMENTS AT A CONCENTRATION GREATER THAN 10  % Method 10.1 EXTRACTION OF TOTAL TRACE ELEMENTS 1. SCOPE This method defines the procedure for extracting the following trace elements: total boron, total  cobalt, total copper, total iron, total manganese, total molybdenum and total zinc. The aim is to  carry out the minimum number of extractions, making use wherever possible of the same extact to  determine the total level of each of the trace elements list above. 2. FIELD OF APPLICATION This procedure concerns Community fertilizers covered by Directive 89/530/EEC containing one or  more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc.  It is applicable to each trace element, the declared content of which is more than 10  %. 3. PRINCIPLE Dissolution in boiling diluted hydrochloric acid. Note:  The extraction is empirical and may not be quantitative depending on the product or the  other constituents of the fertilizer. In particular, in the case of certain manganese oxides, the  quantity extracted may be substantially smaller than the total quantity of manganese which the  product contains. It is the responsibility of the fertilizer manufacturers to ensure that the  declared content actually corresponds to the quantity extracted under the conditions pertaining to  the method. 4. REAGENTS 4.1. Diluted hydrochloric acid (HCI) solution, about 6 M Mix 1 volume of hydrochloric acid (ñ = 1,18 g/ml) with 1 volume of water. 4.2. Concentrated ammonia solution (NH4OH, ñ = 0,9 g/ml) 5. APPARATUS 5.1. Electric hotplate with variable temperature control. 5.2. pH meter Note:  Where the boron content of an extract is to be determined, do not use borosilicate  glassware. As the method involves boiling, teflon or silica is preferable. Rinse the glassware  thoroughly if it has been washed in detergents containing borates. 6. PREPARATION OF THE SAMPLE See Method 1 (Directive 77/535/EEC). 7. PROCEDURE 7.1. Test sample Take a quantity of fertilizer weighing 1 or 2 g depending on the declared content of element in the  product. The following table shall be used to obtain a final solution which, after appropriate  dilution, will be within the measuring rane for each method. Samples should be weighed to within 1  mg. >TABLE> Place the sample in a 250 ml beaker. 7.2. Preparation of the solution If necessary moisten the sample with a little water, add 10 ml of dilute hydrochloric acid (4.1)  per gram of fertilizer carefully, in small amounts, then add about 50 ml of water. Cover the beaker  with a watchglass and mix. Bring to the boil on the hotplate and boil for 30 minutes. Allow to  cool, stirring occasionally. Transfer quantitatively to a 500 ml volumetric flask. Make up to  volume with water and mix thoroughly. Filter through a dry filter into a dry container. Discard the  first portion. The extract must be perfectly clear. It is recommended that the determinations be carried out without delay on aliquot portions of the  clear filtrate, if not the containers should be stoppered. Note:  Extracts in which the boron content has to be determined. Adjust the pH to between 4 and 6 with concentrated ammonia solution (4.2). 8. DETERMINATION The determination of each trace element is to be carried out on the aliquot portions indicated in  the method for each individual trace element. Methods 10.5, 10.6, 10.7, 10.9 and 10.10 cannot be used to determine elements present in a chelated  or complexed form. In such cases Method 10.3 must be used prior to the determination. In the case of determinations by AAS (Methods 10.8 and 10.11) such treatment may not be necessary. Method 10.2 EXTRACTION OF WATER-SOLUBLE TRACE ELEMENTS 1. SCOPE This method defines the procedure for extracting water-soluble forms of the following trace  elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc. The aim is to carry out the  minimum number of extractions, making use wherever possible of the same extract to determine the  level of each of the elements listed above. 2. FIELD OF APPLICATION This procedure concerns Community fertilizers covered by Directive 89/530/EEC containing one or  more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc.  It is applicable to each trace element, the declared content of which is more than 10  %. 3. PRINCIPLE The trace elements are extracted by shaking the fertilizer in water at 20 ± 2  °C. Note:  The extraction is empirical and may or may not be quantitative. 4. REAGENTS 4.1. Diluted hydrochloric acid (HCI) solution, about 6 M Mix 1 volume of hydrochloric acid (ñ = 1,18 g/ml) with 1 volume of water. 5. APPARATUS 5.1. Rotary shaker set at about 35 to 40 rpm. Note:  Where the boron content of the extract is to be determined, do not use borosilicate  glassware. Teflon or silica is preferable for this extraction. Rinse the glassware thoroughly if it  has been washed in detergents containing borates. 6. PREPARATION OF THE SAMPLE See Method 1 (Directive 77/535/EEC). 7. PROCEDURE 7.1. Test sample Take a quantity of fertilizer weighing 1 or 2 g depending on the declared content of the product.  The following table shall be used to obtain final solution which, after appropriate dilution, will  be within the measuring range for each method. The samples should be weighed to within 1 mg. >TABLE> Place the sample in a 500 ml flask. 7.2 Preparation of the solution Add about 400 ml of water. Stopper the flask well. Shake vigorously by hand to disperse the sample, then place the flask on  the shaker and shake for 30 minutes. Make up to volume with water and mix thoroughly. 7.3 Preparation of the test solution Filter immediately into a clean, dry flask. Stopper the flask. Carry out the determination  immediately after filtering. Note:  If the filtrate gradually becomes cloudy, make another extraction following 7.1 and 7.2 in a  flask of volume Ve. Filter into a calibrated flask of volume W wich has previously been dried and  has received 5 ml of dilute hydrochloric acid (4.1). Stop the filtration at the exact moment when  the calibration mark is reached. Mix thoroughly. Under these conditions the value of V in the expression of results is: V = Ve × W/(W-5) The dilutions in the expression of results depend on this value of V. 8. DETERMINATION The determination of each trace element is carried out on the aliquot portions indicated in the  method for each individual trace element. Methods 10.5, 10.6, 10.7, 10.9 and 10.10 cannot be used to determine elements present in a chelated  or complexed form. In such cases Method 10.3 must be used prior to the determination. In the case of determinations by AAS (Methods 10.8 and 10.11) such treatment may not be necessary. Method 10.3 REMOVAL OF ORGANIC COMPOUNDS FROM FERTILIZER EXTRACTS 1. SCOPE This method defines a procedure for removing organic compounds from fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 10.1 and 10.2  for which a declaration of total and/or water-soluble element is required by Directive 89/530/EEC. Note:  The presence of small quantities of organic matter usually does not affect determinations by  means of atomic absorption spectrometry. 3. PRINCIPLE The organic compounds in an aliquot portion of the extract are oxidized with hydrogen peroxide. 4. REAGENTS 4.1 Diluted hydrochloric acid (HCI) solution, about 0,5 M Mix 1 volume of hydrochloric acid ( ñ=1,18 g/ml) with 20 volumes of water. 4.2 Hydrogen peroxide solution (30  % H2O2, ñ=1,11 g/ml), free from trace elements. 5. APPARATUS Electric hotplate with variable temperature control. 6. PROCEDURE Take 25 ml of the extract solution obtained by Method 10.1 or Method 10.2 and place in 100 ml  beaker. In the case of Method 10.2, add 5 ml of the dilute hydrochloric acid solution (4.1). Then  add 5 ml of the hydrogen peroxide solution (4.2). Cover with a watchglass. Allow oxidation to occur  at room temperature for about one hour, then bring gradually to boiling and boil for half an hour.  If necessary, add a further 5 ml of the hydrogen peroxide to the solution once it has cooled. Then  boil to remove the excess hydrogen peroxide. Allow to cool and transfer quantitatively to a 50 ml  volumetric flask and make up to volume. Filter where necessary. Account should be taken of this dilution when taking aliquot portions and calculating the  percentage of trace element in the product. Method 10.4 DETERMINATION OF TRACE ELEMENTS IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY (GENERAL PROCEDURE) 1. SCOPE This document defines a general procedure for determining the levels of iron and zinc in fertilizer  extracts by atomic absorption spectrometry. 2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 10.1 and 10.2  for which a declaration of total and/or water-soluble iron or zinc is required by Directive  89/530/EEC. Adaptations of this procedure for the various trace elements are detailed in the  methods defined specifically for each element. Note:  In most cases the presence of small quantities of organic matter will not affect  determinations by means of atomic absorption spectrometry. 3. PRINCIPLE After the extract has been treated where necessary to reduce or eliminate interfering chemical  species, the extract is diluted so that its concentration is in the optimum range of the  spectrometer at a wavelength suitable for the trace element to be determined. 4. REAGENTS 4.1 Diluted hydrochloric acid solution (HCI), about 6 M Mix one volume of hydrochloric acid ( ñ=1,18 g/ml) with 1 volume of water. 4.2 Diluted hydrochloric acid solution (HCI), about 0,5 M Mix one volume of hydrochloric acid ( ñ=1,18 g/ml) with 20 volumes of water. 4.3 Lanthanum salt solutions (10g of La per litre) This reagent is used for determinations of iron and zinc. It can be prepared either: (a)  with lanthanum oxide dissolved in hydrochloric acid (4.1). Place 11,73 g of lanthanum oxide  (La2O3) in 150 ml of water in a 1 litre volumetric flask and add 120 ml of 6 M hydrochloric acid  (4.1). Allow to dissolve and then make up to 1 litre with water and mix thoroughly. This solution  is approximately 0,5 M in hydrochloric acid; or (b)  with solutions of lanthanum chloride, sulfate or nitrate. Dissolve 26,7 g of lanthanum chloride heptahydrate (LaCl37H2O) or 31,2 g of lanthanum nitrate  hexahydrate (La (NO3)36H2O) or 26,2 g of lanthanum sulfate nonahydrate (La2(SO4)39H2O) in 150 ml of  water, then add 85 ml of 6 M hydrochloric acid (4.1). Allow to dissolve and then make up to 1 litre  with water. Mix thoroughly. This solution is approximately 0,5 M in hydrochloric acid. 4.4 Calibration solutions For the preparation of these, see the individual determination method for each trace element. 5. APPARATUS Atomic absorption spectrometer fitted with sources emitting radiation characteristic of the trace  elements to be determined. The analyst must follow the manufacturer's instructions and be familiar with the apparatus. The  apparatus must allow background correction so that it can be used whenever necessary (e.g. Zn). The  gases to be used are air and acetylene. 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of extract solutions containing the elements to be determined See Method 10.1 and/or 10.2 and, if appropriate, 10.3. 6.2. Treatment of the test solution Dilute an aliquot portion of the extract obtained by Method 10.1, 10.2 or 10.3 with water and/or  hydrochloric acid (4.1) or (41.2) so as to obtain, in the final solution for measurement, a  concentration of the element to be determined that is appropriate to the calibration range used  (7.2) and a hydrochloric acid concentration of at least 0,5 M and not more than 2,5 M. This  operation may require one or more successive dilutions. The final solution has to be obtained by placing an aliquot portion of the diluted extract in a 100  ml volumetric flask. Let the volume of this aliquot portion be (a) ml. Add 10 ml of the lanthanum  salt solution (4.3). Make up to volume with 0,5 M hydrochloric acid solution (4.2) and mix  thoroughly. Let D be the dilution factor. 7. PROCEDURE 7.1. Preparation of a blank solution Prepare a blank solution by repeating the whole procedure from the extraction stage, omitting only  the test sample of fertilizer. 7.2. Preparation of calibration solutions From the working calibration solution prepared using the method given for each individual trace  element, prepare in 100 ml volumetric flasks a series of at least five calibration solutions of  increasing concentration within the optimum measuring range of the spectrometer. If necessary,  adjust the concentration of hydrochloric acid to bring it as close as possible to that of the  diluted test solution (6.2). When determining iron or zinc add 10 ml of the same lanthanum salt  solution (4.3) as used in (6.2). Make up to volume with the 0,5 hydrochloric acid solution (4.2)  and mix thoroughly. 7.3. Determination Prepare the spectrometer (5) for the determination and adjust to the wavelength given in the method  for the individual trace element concerned. Spray three times in succession the calibration solutions (7.2), the test solution (6.2) and the  blank solution (7.1), noting each result and flushing the instrument with distilled water between  individual sprayings. Construct the calibration curve by plotting the average spectrometer reading for each calibration  solution (7.2) along the ordinate and the corresponding concentration of the element, expressed in  ìg/ml, along the abscissa. From this curve, determine the concentrations of the relevant trace element in the test solution Xs  (6.2) and in the blank solution Xb (7.1), expressing these concentrations in ìg per ml. 8. EXPRESSION OF RESULTS The percentage of trace element (E) in the fertilzer is given by: E (%) = [(Xs - Xb)  ×  V  ×  D] / (M  ×  104) If Method 10.3 has been used: E (%) = [(X5 - Xb)  ×  V  ×  2D] / (M  ×  104) where: E is the amount of the trace element determined, expressed as a percentage of the fertilizer; Xs is the concentration in the test solution (6.2), in ìg/ml; Xb is the concentration in the blank solution (7.1) in ìg/ml; V is the volume of the extract obtained by Method 10.1 or 10.2, in ml; D is the factor corresponding to the dilution carried out in (6.2); M is the mass of the test sample taken in accordance with Method 10.1 or 10.2, in grams. Calculation of dilution factor D: If (a1), (a2), (a3), .  .  .  ., (a1) and (a) are the aliquot portions and (v1), (v2), (v3), .  .   .  ., (v1) and (100) are the volumes in ml corresponding to their respective dilutions, the  dilution factor D will be equal to: D = (v1/a1)  ×  (v2/a2)  ×  (v3/a3) × .  .  . × (v1/a1)  ×  (100/a) Method 10.5 DETERMINATION OF BORON IN FERTILIZER EXTRACTS BY MEANS OF ACIDIMETRIC TITRATION 1. SCOPE This document defines a procedure for determining the boron content of fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Method 10.1 or  Method 10.2 and for which a declaration for the total boron content and/or of the water-soluble  boron content is required by Directive 89/530/EEC. 3. PRINCIPLE A mannitoboric complex is formed by the following reaction of the borate in with mannitol: C6H8(OH)6  +  H3BO3  - C6H15O8B  +  H2O The complex is titrated with sodium hydroxide solution to a pH of 6,3. 4. REAGENTS 4.1. Methyl red indicator solution Dissolve 0,1 g of methyl red (C15H15N3O2) in 50 ml of ethanol (95  % in a 100 ml volumetric flask.  Make up the volume to 100 ml with water. Mix thoroughly. 4.2. Diluted hydrochloric acid solution, about 0,5 M Mix 1 volume of hydrochloric acid HCI, p: 1,18 g/ml) with 20 volumes of water. 4.3. Sodium hydroxide solution, about 0,5 M Must be free of carbon dioxide. Dissolve 20 g of sodium hydroxide (NaOH) in pellet form in a 1  litre volumetric flask containing about 800 ml of boiled water. When the solution has cooled, make  up to 1  000 ml with boiled water and mix thoroughly. 4.4. Standard sodium hydroxide solution, about 0,025 M Must be free of carbon dioxide. Dilute the 0,5 M sodium hydroxide solution (4.3) 20 times with  boiled water and mix thoroughly. The value of the solution expressed as boron (B) is to be  determined (see paragraph 9). 4.5. Boron calibration solution (100 ìg/ml B) Dissolve 0,5719 g of boric acid (H3BO3), weighed to the nearest 0,1 mg, in water in a 1  000 ml  volumetric flask. Make up to volume with water and mix thoroughly. Transfer to a plastic bottle for  storage in a refrigerator. 4.6. D-mannitol (C6H14O6) powder 4.7. Sodium chloride (NaC1) 5. APPARATUS 5.1. pH meter with glass electrode 5.2. Magnetic stirrer 5.3. 400 ml beaker with teflon rod 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of the boron solution See Methods 10.1, 10.2 and, where appropriate, 10.3. 7. PROCEDURE 7.1. Test Place in a 400 ml beaker (5.3) an aliquot (a) of the extract (6.1) containing 2 to 4 mg B. Add 150  ml of water. Add several drops of the methyl red indicator solution (4.1). In the case of extraction with Method 10.2, acidify by adding 0,5 M hydrochloric acid (4.2) up to  the point of change of the indicator solution, then add a further 0,5 ml of 0,5 M hydrochloric acid  (4.2). After adding 3 g of sodium chloride (4.7), bring to boiling to drive off the carbon dixoide. Allow  to cool. Place the beaker on the magnetic stirrer (5.2) and insert the precalibrated pH meter  electrodes (5.1). Adjust the pH to exactly 6,3, first with the 0,5 M sodium hydroxide solution (4.3), then with the  0,025 M solution (4.4). Add 20 g of D-mannitol (4.6), dissolve completely and mix thoroughly. Titrate with the 0,025 M  sodium hydroxide solution (4.4) to pH 6,3 (at least 1 minute stability). Let x1, be the volume  required. 8. BLANK SOLUTION Preparage a blank solution by repeating the whole procedure from the preparation of solution stage,  omitting only the fertilizer. Let x0 be the volume required. 9. BORON (B) VALUE OF THE SODIUM HYDROXIDE SOLUTION (4.4) Pipette 20 ml (2,0 mg B) of the calibration solution (4.5), into a 400 ml beaker and add several  drops of methyl red indicator solution (4.1). Add 3 of sodium chloride (4.7) and the hydrochloric  acid solution (4.2) up to the point of change of the indicator solution (4.1). Make up the volume to about 150 ml and bring gradually to the boil so as to eliminate carbon  dioxide. Allow to cool. Place the beaker on the magnetic stirrer (5.2), and insert the  precalibrated pH meter electrodes (5.1). Adjust the pH to exactly 6,3, first with the 0,5 m sodium  hydroxide solution (4.3), then with the 0,025 M solution (4.4). Add 20 g of D-mannitol (4.6), dissolve completely and mix thoroughly. Titrate with the 0,025 M  sodium hydroxide solution (4.4) to pH 6,3 (at least 1 minute stability). Let V1 be the volume  required. Prepare a blank solution in the same way, substituting 20 ml of water for the calibration solution.  Let V0 be the volume required. The boron value (F) in mg/ml of the standard NaOH solution (4.4) is as follows: F (in mg/ml) = 2/(V1  P V0) 1 ml of exactly 0,025 M sodium hydroxide solution corresponds to 0,27025 mg B. 10. EXPRESSION OF RESULTS The percentage of boron in the fertilizer is given by: B  (%) = (X1  P X0) × F × V 10 × a × M where: B  (%) is the percentage of boron in the ferlizer; X1 is the volume, in ml, of the 0,025 M sodium hydroxide solution (4.4); X0 is the volume, in ml, of the 0,025 M sodium hydroxide solution M (4.4); F is the boron (B) value, in mg/ml, of the 0,025 M sodium hydroxide solution M (4.4); V is the volume, in ml, of the extract solution obtained in accordance with Method 10.1 or 10,2; a is the volume, in ml, of the aliquot (7.1) taken from the extract solution (6.1); M is the mass, in grams, of the test sample taken in accordance with Method 10.1 or 10.2. Method 10.6 DETERMINATION OF COBALT IN FERTILIZER EXTRACTS BY THE GRAVIMETRIC METHOD WITH 1-NITROSO-2-NAPHTHOL 1. SCOPE This document defines a procedure for determing cobalt in fertilzer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Method 10.1 or  Method 10.2 for which a declaration of cobalt content is required by Directive 89/530/EEC. 3. PRINCIPLE Cobalt III combines with 1-nitroso-2-naphthol to give a red precipitate Co (C10H6ONO)3, 2H2O. After  the cobalt present in the extract has been brought to the cobalt III state, the cobalt is  precipitated in an acetic acid medium by a solution of 1-nitroso-2-naphthol. After filtration, the  precipitate is washed and dried to constant weight and then weighed as Co (C10H6ONO)3, 2H2O. 4. REAGENTS 4.1. Hydrogen peroxide solution (H2O2 p=1,11 g/ml) 30  % 4.2. Sodium hydroxide solution, about 2 M Dissolve 8 g of sodium hydroxide in pellet form in 100 ml of water. 4.3. Diluted hydrochloric acid solution, about 6 M Mix one volume of hydrochloric acid (p=1,18 g/ml) with 1 volume of water. 4.4. Acetic acid (99,7  % CH3CO2H) (p=1,05 g/ml) 4.5. Acetic acid solution (1:  2), about 6 M Mix one volume of acetic acid (4.4) with 2 volumes of water. 4.6. Solution of 1-nitroso-2-naphthol in 100 ml of acetic acid (4.4). Add 100 ml of lukewarm water.  Mix thoroughly. Filter at once. The solution obtained must be used immediately. 5. APPARATUS 5.1. Filter crucible P 16/ISO 4793, porosity 4, capacity 30 or 50 ml 5.2. Drying oven at 130 ± 2  °C 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of the cobalt solution See Methods 10.1 or 10.2. 6.2. Preparation of the solution to be analysed Place an aliquot of the extract containing not more than 20 m Co in a 400 ml beaker. If the extract  is obtained according to Method 10.2, acidify with five drops of hydrochloric acid (4.3). Add about  10 ml of the hydrogen peroxide solution (4.1). Allow the oxidant to act in the cold state for 15  minutes, then make up to about 100 ml with water. Cover the beaker with a watchglass. Bring the  solution to boiling point and allow to boil for about 10 minutes. Cool. Make alkaline with the  sodium hydroxide solution (4.21) drop by drop until black cobalt hydroxide begins to precipitate. 7. PROCEDURE Add 10 ml of acetic acid (4.4) and make up the solution with water to about 200 ml. Heat until  boiling. Using a burette, add 20 ml of the 1-nitroso-2-naphthol solution (4.6) drop by drop,  stirring constantly. Complete by vigorous stirring to make the precipitate coagulate. Filter through a previously weighed filter curcible (5.1), taking care not to clog up the crucbile.  With this in mind, ensure that liquid is left above the precipitate throughout the filtration  process. Wash the beaker with dilute acetic acid (4.5) to remove all the precipitate, wash the precipitate  on the filter with dilute acetic acid (4.5) and then three times with hot water. Dry in a drying oven (5.2) at 130 ± 2  °C until constant weight is achieved. 8. EXPRESSION OF THE RESULTS 1 mg of Co (C10H6ONO)3, 2H2O precipitate corresponds to 0,096381 mg Co. The percentage of Cobalt (Co) in the fertilizer is given by: Co (%) = X × 0,0096381 × V × D a × M where: X is the mass in mg of the precipitate; V is the volume in ml of the extract solution obtained in accordance with Method 10.1 or Method  10.2; a is the volume in ml of the aliquot taken from the last dilution; D is the dilution factor of this aliquot; M is the mass in g of the test sample. Method 10.7 DETERMINATION OF COPPER IN FERTILIZER EXTRACTS BY THE TITRIMETRIC METHOD 1. SCOPE This document defines a procedure for determining copper in fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertlizers obtained by Method 10.1 or  Method 10.2 for which a declaration of copper content is required by Directive 89/530/EEC. 3. PRINCIPLE The cupric ions are reduced in an acidic medium with potassium iodide: 2 Cu+++ 4 I  P -2 CuI + I2 The iodine released in this way is titrated with a standard sodium thiosulphate solution in the  presence of starch as an indicator in accordance with: I2 + 2 Na2S2O3  - 2 NaI + Na2S4O6 4. REAGENTS 4.1, Nitric acid (HNO3, p = 1,40 g/ml) 4.2. Urea [(NH2)2 C=0] 4.3. Ammonium bifluoride (NH4HF2) solution 10  % w/v Keep the solution in a plastic container. 4.4. Ammonium hydroxyde solution (1+1) Mix 1 volume of ammonia (NH4OH, p: 0,9 g/ml) with 1 volume of water. 4.5. Sodium thiosulphate standard solution Dissolve 7,812 g of sodium thiosulphate pentahydrate (NA2S2O35H2O) with water in a 1 litre  volumetric flask. This solution must be prepared so that 1 ml = 2 mg Cu. For stabilization, add  several drops of chloroform. The solution must be kept in a glass container and protected from  direct light. 4.6. Potassium iodide (KI) 4.7. Potassium thiocyanate (KSCN) solution (25  % w/v) Keep this solution in a plastic flask. 4.8. Starch solution (about 0,5  %) Place 2,5 g of starch in a 600 ml beaker. Add about 500 ml of water. Boil while stirring. Cool to  ambient temperature. The solution has a short preservation period. Its preservation can be extended  by adding about 10 mg of mercury iodide. 5. PREPARATION OF THE SOLUTION TO BE ANALYSED Preparation of the copper solution See Methods 10.1 and 10.2. 6. PROCEDURE 6.1. Preparation of the solution for titration Place an aliquot portion of the solution containing not less than 20-40 mg Cu in a 500 ml  Erlenmeyer flask. Drive off any excess oxygen present by boiling briefly. Make up to a volume af about 100 ml water.  Add 5 ml of nitric acid (4.1), bring to boiling and allow to boil for about half a minute. Remove the Erlenmeyer flask from the heating apparatus, add about 3 g of urea (4.2) and resume  boiling for about half a minute. Remove from the heating apparatus and add 200 ml of cold water. Where necessary, cool the contents  of the Erlenmeyer flask to ambient temperature. Gradually add ammonia hydroxide solution (4.4) until the solution becomes blue, then add 1 ml in  excess. Add 50 ml of ammonium bifluoride solution (4.3) and mix. Add 10 g of potassium iodide (4.6) and dissolve. 6.2. Titration of the solution Place the Erlenmeyer flask on a magnetic stirrer. Insert the rod into the Erlenmeyer flask and  adjust the stirrer to the desired speed. Using a burette, add standard sodium thiosulphate solution (4.5) until the brown colour of the  iodine released from the solution becomes less intense. Add 10 ml of the starch solution (4.8). Continue to titrate with the sodium thiosulphate solution (4.5) until the purple colour has almost  disappeared. Add 20 ml of the potassium thiocyanate solution (4.7) and continue titration until the violet blue  colour has completely disappeared. Note the volume for thiosulphate solution employed. 7. EXPRESSION OF RESULTS 1 ml of standard sodium thiosulphate solution (4.5) corresponds to 2 mg Cu. The percentage of copper in the fertilizer is given by: Cu (%) = X V a × M × 5 where: X is the volume in ml of the sodium thiosulphate solution used; V is the volume in ml of the extract solution in accordance with Methods 10.1 and 10.2; a is the volume in ml of the aliquot portion; M is the mass in g of the test sample treated in accordance with Methods 10.1 and 10.2. Method 10.8 DETERMINATION OF IRON IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining iron in fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Methods 10.1 and  10.2 for which a declaration of total and/or water-soluble iron is required by Directive  89/530/EEC. 3. PRINCIPLE After suitable treatment and dilution of the extract, the iron content is determined by atomic  absorption spectrometry. 4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 10.4, (4.1). 4.2. Hydrochloric acid solution, about 0,5 M See Method 10.4, (4.2). 4.3 Hydrogen peroxide solution (30  % H2O2, d = 1,11 g/ml) free from trace elements 4.4. Lanthanum salt solutions (10 g of La per litre) See Method 10.4, (4.3). 4.5. Iron calibration solution 4.5.1. Iron stock solution (1  000 ìg/ml) In a 500 ml beaker, weigh to the nearest 0,1 mg, 1 g of pure iron wire, add 200 ml of 6 M  hydrochloric acid (4.1) and 15 ml of hydrogen peroxide solution (4.3). Heat on a hotplate until the  iron is completely dissolved. When cool, transfer quantitatively to a 1  000 ml volumetric flask.  Make up to volume with water and mix thoroughly. 4.5.2. Iron working solution (100 ìg/ml) Place 20 ml of the stock solution (4.5.1) in a 200 ml volumetric flask. Make up to volume with the  0,5 M hydrochloric acid solution (4.2) and mix thoroughly. 5. APPARATUS Atomic absorption spectrometer: see Method 10.4, (5). The instrument must be fitted with a source  of rays characteristic of iron (248,3 nm). 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Iron extract solution See Methods 10.1 and/or 10.2 and, if appropriate, 10.3. 6.2. reparation of the test solution See Method 10.4, (6.2). The test solution must contain 10  % (v/v) of a lanthanum salt solution. 7. PROCEDURE 7.1. Preparation of blank solution See Method 10.4 (7.1). The blank solution must contain 10  % (v/v) of the lanthanum salt solution  used in 6.2. 7.2. Preparation of calibration solutions See Method 10.4, (7.2). For an optimum determination range of 0 to 10 ìg/ml of iron, place 0, 2, 4, 6, 8 and 10 ml  respectively of working solution (4.5.2) in a series of 100 ml volumetric flasks. If necessary  adjust the hydrochloric acid concentration as closely as possible to that of the test solution. Add  10 ml of the lanthanum salt solution used in 6.2. Make up to volume with 0,5 M hydrochloric acid  solution (4.2) and mix thoroughly. These solutions contain 0, 2, 4, 6, 8 and 10 ìg/ml respectively  of iron. 7.3. Determination See Method 10.4, (7.3). Prepare the spectrometer (5) for measurement at a wavelength of 248,3 nm. 8. EXPRESSION OF RESULTS See Method 10.4, (8). The percentage of iron in the fertilizer is given by: Fe (%) = [(Xs - Xb) × V × D] / (M × 104) If Method 10.3 is used: FE (%) = [(Xs - Xb) × V × 2D] / (M × 104) where: Fe is the quantity of iron expressed as a percentage of the fertilizer; Xs is the concentration in ìg/ml of the test solution (6.2); Xb is the concentration in ìg-ml of the blank solution (7.1); V is the volume in ml of extract obtained in accordance with Method 10.1 or 10.2; D is the factor of the dilution carried oujt in 6.2; M is the mass in grams of the test sample taken in accordance with Method 10.1 or 10.2. Calculation of the dilution factor D: if (a1), (a2), (a3), .  .  ., (ai) and (a) are aliquot  portions and (v1) (v2) (v3), .  .  ., (vi) and (100) are the volumes in ml corresponding to their  respective dilutions, the dilution factor D is given by: D = (v1/a1) × (v2/a2) × (v3/a3) × .  .  . × (vi/ai) × (100/a) Method 10.9 DETERMINATION OF MANGANESE IN FERTILIZER EXTRACTS BY TITRATION 1. SCOPE This method describes a procedure for determining manganese in fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Methods 10.1 and  10.2 for which a declaration of manganese is required by Directive 89/530/EEC. 3. PRINCIPLE If chloride ions are present in the extract, they are driven off by boiling the extract with  sulfuric acid. The manganese is oxidized by sodium bismuthate in a nitric acid medium. The  permanganate formed is reduced by an excess of ferrous sulfate. This excess is titrated with a  potassium permanganate solution. 4. REAGENTS 4.1. Concentrated sulfuric acid (H2SO4, ñ =  1.84 g/ml) 4.2. Sulfuric acid, about 9 M Carefully mix 1 volume of concentrated sulphuric acid (4.1) with 1 volume of water. 4.3. Nitric acid, 6 M Mix 3 volumes of nitric acid (HNO3, ñ =  1,40 g/ml) with 4 volumes of water. 4.4. Nitric acid, 0,3 M Mix 1 volume of 6 M nitric acid with 19 volumes of water. 4.5. Sodium bismuthate (NaBiO3) (85  %) 4.6. Kieselguhr 4.7. Orthophosphoric acid, 15 M (H3PO4, ñ =  1,71 g/ml) 4.8. Ferrous sulphate solution, 0,15 M Dissolve 41,6 g of ferrous sulphate heptahydrate (FeSO4, 7H2O) in a 1-litre volumetric flask. Add 25 ml of concentrated sulphuric acid (4.1) and 25 ml phosphoric acid (4.7). Make up to 1  000  ml. Mix. 4.9. Potassium permanganate solution, 0,020 M Weigh out 3,160 g of potassium permanganate (KMnO4) to within 0,1 mg. Dissolve and make up to 1   000 ml with water. 4.10. Silver nitrate solution, 0,1 M Dissolve 1,7 g of silver nitrate (AgNO3) in water and make up to 100 ml. 5. APPARATUS 5.1. Filter crucible P16/ISO 4793, porosity 4, capacity 50 ml, mounted on a 500 ml filtration  flask. 5.2. Magnetic stirrer. 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Manganese extract solution See Methods 10.1 and 10.2. If it is not known whether chloride ions are present, perform a test on  the solution with one drop of the silver nitrate solution (4.10). 6.2. In the absence of chloride ions, place an aliquot of the extract containing 10 to 20 mg of  manganese in a tall form 400 ml beaker. Bring to a volume of about 25 ml either by evaporation or  by adding water. Add 2 ml of concentrated sulphuric acid (4.1). 6.3. If chloride ions are present, it is necessary to remove them as follows: Place an aliquot of the extract containing 10 to 20 mg of manganese in a tall form 400 ml beaker.  Add 5 ml of 9 M sulphuric acid (4.2.). Under a fume hood, bring to boiling on a hot-plate and allow  to boil until copious white fumes are released. Continue until the volume is reduced to about 2 ml  (thin film of syrupy liquid at the bottom of the beaker). Allow to cool to ambient temperature. Carefully add 25 ml of water and once again test for the presence of chlorides with one drop of the  silver nitrate solution (4.10). If chlorides still remain, repeat the operation after adding 5 ml  of 9 M sulphuric acid (4.2). 7. PROCEDURE Add 25 ml of 6 M nitric acid (4.3) and 2,5 g of sodium bismuthate (4.5) to the 400-ml beaker  containing the test solution. Stir vigorously for three minutes on the magnetic stirrer (5.2). Add 50 ml of 0,3 M nitric acid (4.4) and stir again. Filter in vacuo through a crucible (5.1), the  bottom of which is covered with Keiselguhr (4.6). Wash the crucible serveral times with the 0,3 M  nitric acid (4.4) until a colourless filtrate is obtained. Transfer the filtrate and the washing solution into a 500 ml beaker. Mix and add 25 ml of 0,15 M  ferrous sulphate solution (4.8). If the filtrate turns yellow after the addition of ferrous  sulphate, add 3 ml of 15 M orthophosphoric acid (4.7). Using a burette, titrate the excess ferrous sulphate with 0,02 M potassium permanganate solution  (4.9) until the mixture turns pink, the colour remaining stable for one minute. Perform a blank  test under the same conditions, omitting only the test sample. Note: The oxidized solution must not come into contact with rubber. 8. EXPRESSION OF RESULTS 1 ml of 0,02 M potassium permanganate solution corresponds to 1,099 mg of manganese (Mn) The percentage of manganese in the fertilizer is given by: Mn (%) where  =  (Xb-Xs)  ×  0,1099  ×    V a × M where: Xb is the volume in ml of the permanganate used for the blank; Xs is the volume in ml of the permanganate used for the test sample; V is the volume in ml of the extract solution in accordance with Methods 10.1 and 10.2; a is the volume in ml of the aliquot portion taken from the extract; M is the mass in g of the test sample. Method 10.10 DETERMINATION OF MOLYBDENUM IN FERTILIZER EXTRACTS BY THE GRAVIMETRIC METHOD WITH  8-HYDROXYQUINOLINE 1. SCOPE This document describes a procedure for determining molybdenum in ferilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Method 10.1 and  10.2 for which a declaration of molybdenum is required by Directive 89/530/EEC. 3. PRINCIPLE The molybdenum level is determined by precipitation as molybdenyl oxinate under specific  conditions. 4. REAGENTS 4.1. Sulphuric acid solution, approximately 1 M Carefully pour 55 ml of sulphuric acid (H2SO4, ñ = 1,84 g/ml) into a 1-litre volumetric flask  containing 800 ml of water. Mix. After cooling, make up to one litre. Mix. 4.2. Diluted ammonia solution (1:  3) Mix 1 volume of concentrated ammonia solution (NH4OH, ñ = 0,9 g/ml) with 3 volumes of water. 4.3. Diluted acetic acid solution (1:  3) Mix 1 volume of concentrated acetic acid (99,7  % CH3COOH, ñ = 1,049 g/ml) with 3 volumes of  water. 4.4. Solution of disodium salt of ethylene diamine tetraacetic acid (EDTA) Dissolve 5 g of Na2EDTA in water in a 100 ml volumetric flask. Make up to the calibration mark and  mix.4.5. Buffer solution In a 100-ml volumetric flask dissolve 15 ml of concentrated acetic acid and 30 g of ammonium  acetate in water. Make up to 100 ml. 4.6. 7-Hydroxyquinoline (oxine) solution In a 100-ml volumetric flask dissolve 3 g of 8-hydroxyquinoline in 5 ml of concentrated acetic  acid. Add 80 ml of water. Add the ammonia solution (4.2) drop by drop until the solution becomes  cloudy and then add the acetic acid (4.3) until the solution becomes clear again. Make up to 100 ml with water. 5. APPARATUS 5.1. Filter crucible P16/ISO4793, porosity 4, capacity 30 ml. 5.2. pH meter with glass electrode. 5.3. Drying oven at 130 to 135  °C. 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of the molybdenum solution. See Method 10.1 and Method 10.2. 7. PROCEDURE 7.1. Preparation of the test solution Place an aliquot portion containing 25 to 100 mg Mo in a 250-ml beaker. Make up the volume to 50 ml  with water. Adjust this solution to pH of 5 by adding the sulfuric acid solution (4.1) drop by drop. Add 15 ml  of EDTA solution (4.4) and then 5 ml of buffer solution (4.5). Make up to about 80 ml with water. 7.2. Obtaining and washing the precipitate Obtaining the precipitate Heat the solution slightly. Stirring constantly, add the oxine solution (4.6). Continue the  precipitation until formation of a deposit is no longer observed. Add further reagent until the  supernatant solution turns slightly yellow. A quantity of 20 ml should normally be sufficient.  Continue to heat the precipitate slightly for two to three minutes. Filtration and washing Filter through a filter crucible (5.1). Rinse several times with 20 ml of hot water. The rinse  water should gradually become colourless indicating that oxine is not longer present. 7.3. Weighing the precipitate Dry the precipitate at 130 to 135  °C to constant weight (at last one hour) Allow to cool in a desiccator and then weigh. 8. EXPRESSION OF THE RESULTS 1 mg of molybdenyl oxinate, MoO2(C9H6ON)2, corresponds to 0,2305 mg Mo. The percentage of molybdenum in the fertilizer is given by: Mo (%) = X × 0,02305 ×   V × D a × M where: X is the mass in mg of the molybdenyl oxinate precipitate; V is the volume in ml of the extract solution in accordance with Methods 10.1 or 10.2; a is the volume in ml of the aliquot taken from the last dilution; D is the dilution factor of the aliquot; M is the mass in g of the test sample. Method 10.11 DETERMINATION OF ZINC IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining zinc in fertilizer extracts. 2. FIELD OF APPLICATION This procedure is applicable to extracts from samples of fertilizers obtained by Methods 10.1 and  10.2 for which a declaration of zinc is required by Directive 89/530/EEC. 3. PRINCIPLE After suitable treatment and dilution of the extracts, the zinc level is determined by atomic  absorption spectrometry. 4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 10.4, (4.1). 4.2. Hydrochloric acid solution, about 0.5 M See Method 10.4, (4.2). 4.3. Lanthanum salt solutions (10 g of La per litre) See Method 10.4, (4.3). 4.4. Zinc calibration solutions 4.4.1. Zinc stock solution (1  000 ìg/ml) In a 1  000 ml volumetric flask dissolve 1 g of zinc powder or flakes weighed to within 0,1 mg in  25 ml of 6 M hydrochloric acid (4.1). When completely dissolved, make up to volume with water and  mix thoroughly. 4.4.2. Zinc working solution (100 ìg/ml) In a 200 ml volumetric flask, dilute 20 ml of the stock solution (4.4.1) in 0,5 M hydrochloric acid  solution (4.2). Make up to a volume with the 0,5 M hydrochloric acid solution and mix thoroughly. 5. APPARATUS Atomic absorption spectrometer See Method 10.4, (5). The apparatus must be fitted with a source of lines characteristic of zinc  (213,8  nm). The spectrometer must allow background correction to be made. 6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Zinc extract solution See Methods 10.1 and/or 10.2. 6.2. Preparation of the test solution See Method 10.4, (6.2). The test solution must contain 10  % by volume of lanthanum salt solution  (4.3). PROCEDURE 7.1. Preparation of the blank solution. See Method 10.4, (7.1). The blank solution must contain 10  % by volume of the lanthanum salt  solution used in 6.2. 7.2. Preparation of the calibration solutions See Method 10.4 (7.2). For an optimum interval of 0 to 5 ìg/ml of zinc, place 0, 0,5, 1, 2, 3, 4  and 5 ml, respectively, of the working solution (4.4.2) in a series of 100 ml volumetric flasks.  Where necessary, adjust the concentration of hydrochloric acid to bring it as close as possible to  that of the test solution. Add 10 ml of the lanthanum salt solution used in (6.2) to each  volumetric flask. Make up to 100 ml with the 0,5 M hydrochloric acid solution (4.2) and mix  thoroughly. These solutions contain, respectively: 0, 0,5, 1, 2, 3, 4 and 5 ìg/ml of zinc. 7.3. Determination See Method 10.4, (7.3). Prepare the spectrometer (5) for measurements at a wavelength of 213,8 nm. 8. EXPRESSION OF RESULTS See Method 10.4 (8) The percentage of zinc in the fertilizer is given by: Zn (%) = [(Xs-Xb) × V × D] / (M × 104) If method 10.3 has been used: Zn (%) = [(Xs-Xb) × V × 2D] / (M × 104) where: Zn is the quantity of zinc expressed as a percentage of the fertilizer; Xs is the concentration in ìg/ml of the test solution; Xb is the concentration in ìg/ml of the blank solution; V is the volume in ml of the extract solution obtained in accordance with Method 10.1 or 10.2; D is the factor corresponding to the dilution performed in (6.2); M is the mass in g of the test sample taken in accordance with Method 10.1 or 10.2. Calculation of the dilution factor D: where (a1), (a2), (a3), .  .  .,. (ai) and (a) are successive  aliquot portions and (v1), (v2), (v3), .  .  ., (vi) and (100) are the volumes corresponding to  their respective dillutions, the dilution factor D will be: D = (v1/a1) × (v2/a2) × (v3/a3) × .  .  . × (vi/ai) × (100/a).`


Avis juridique important

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32002L0028

Commission Directive 2002/28/EC of 19 March 2002 amending certain annexes to Council Directive 2000/29/EC on protective measures against the introduction into the Community of organisms harmful to plants or plant products and against their spread within the Community

Official Journal L 077 , 20/03/2002 P. 0023 - 0025

Commission Directive 2002/28/ECof 19 March 2002amending certain annexes to Council Directive 2000/29/EC on protective measures against the introduction into the Community of organisms harmful to plants or plant products and against their spread within the CommunityTHE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Community,Having regard to Council Directive 2000/29/EC of 8 May 2000 on protective measures against the introduction into the Community of organisms harmful to plants or plant products and against their spread within the Community(1), as last amended by Commission Directive 2001/33/EC(2) and in particular Article 14(c) thereof,Having regard to the agreement of the Member States concerned,Whereas:(1) From information supplied by the United Kingdom based on updated surveys it appears that the protected zone recognised for Dendroctonus micans Kugelan in the United Kingdom should be modified.(2) From information supplied by the United Kingdom on the presence of beet necrotic yellow vein virus it appears that it is no longer appropriate to maintain the protected zone for the whole of the United Kingdom in respect of beet necrotic yellow vein virus but should be restricted to Northern Ireland only.(3) From information supplied by Italy the description of the protected zones in respect of Erwinia amylovora (Burr.) Winsl. et al. should be modified to take into account the present distribution of the organism.(4) The description of the protected zones relating to host plants of Erwinia amylovora (Burr.) Winsl. et al. as regards the special requirements to be met should be modified to take into account the present distribution of the organism.(5) From information supplied by France on the presence of Matsucoccus feytaudi Duc. it appears that it is no longer appropriate to maintain the protected zone for this organism.(6) Therefore, Directive 2000/29/EC should be amended accordingly.(7) The measures provided for in this Directive are in accordance with the opinion of the Standing Committee on Plant Health,HAS ADOPTED THIS DIRECTIVE:Article 1Annexes I, II, III and IV to Directive 2000/29/EC are amended in accordance with the Annex to this Directive.Article 21. Member States shall adopt and publish, by 31 March 2002 at the latest, the laws, regulations and administrative provisions necessary to comply with this Directive. They shall forthwith inform the Commission thereof.They shall apply those provisions from 1 April 2002.When Member States adopt those provisions, they shall contain a reference to this Directive or shall be accompanied by such reference on the occasion of their official publication. Member States shall determine how such a reference is to be made.2. Member States shall immediately communicate to the Commission the text of the main provisions of national law which they adopt in the field covered by this Directive. The Commission shall inform the other Member States thereof.Article 3This Directive shall enter into force on the third day following that of its publication in the Official Journal of the European Communities.Article 4This Directive is addressed to the Member States.Done at Brussels, 19 March 2002.For the CommissionDavid ByrneMember of the Commission(1) OJ L 169, 10.7.2000, p. 1.(2) OJ L 127, 9.5.2001, p. 42.ANNEX1. In Annex I, Part B(b)(1), in the right-hand column "UK" is replaced by "UK (Northern Ireland)".2. Annex II, Part B is amended as follows:(a) under heading (a), in point 3, the entry in the third column is replaced by the following: >TABLE>;(b) under heading (a), point 7 is deleted;(c) under heading (b), in point 2, the entry in the third column is replaced by the following: >TABLE>;3. In Annex III, Part B(b)(1), the right-hand column is replaced by the following: >TABLE>;4. Annex IV, Part B is amended as follows:(a) in points 1, 7, and 14.1, the entry in the third column is replaced by the following: >TABLE>;(b) points 6.2, 14.7 are deleted;(c) in points 20.1, 20.2, 22, 23, 25.1, 25.2, 26, 27.1, 27.2, and 30 in the third column "UK" is replaced by "UK (Northern Ireland)";(d) in point 21, the entry in the second column at (a) is replaced by the following: >TABLE>;(e) in point 21, the entry in the third column is replaced by the following: >TABLE>.