title: Directive 2013/40/EU of the European Parliament and of the Council of 12 August 2013 on attacks against information systems and replacing Council Framework Decision 2005/222/JHA

text:
               14.8.2013

               EN

               Official Journal of the European Union

               L 218/8

         DIRECTIVE 2013/40/EU OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL
   of 12 August 2013
   on attacks against information systems and replacing Council Framework Decision 2005/222/JHA
   THE EUROPEAN PARLIAMENT AND THE COUNCIL OF THE EUROPEAN UNION,
   Having regard to the Treaty on the Functioning of the European Union, and in particular Article 83(1) thereof,
   Having regard to the proposal from the European Commission,
   After transmission of the draft legislative act to the national parliaments,
   Having regard to the opinion of the European Economic and Social Committee (1),
   Acting in accordance with the ordinary legislative procedure (2),
   Whereas:

               (1)

               The objectives of this Directive are to approximate the criminal law of the Member States in the area of attacks against information systems by establishing minimum rules concerning the definition of criminal offences and the relevant sanctions and to improve cooperation between competent authorities, including the police and other specialised law enforcement services of the Member States, as well as the competent specialised Union agencies and bodies, such as Eurojust, Europol and its European Cyber Crime Centre, and the European Network and Information Security Agency (ENISA).

               (2)

               Information systems are a key element of political, social and economic interaction in the Union. Society is highly and increasingly dependent on such systems. The smooth operation and security of those systems in the Union is vital for the development of the internal market and of a competitive and innovative economy. Ensuring an appropriate level of protection of information systems should form part of an effective comprehensive framework of prevention measures accompanying criminal law responses to cybercrime.

               (3)

               Attacks against information systems, and, in particular, attacks linked to organised crime, are a growing menace in the Union and globally, and there is increasing concern about the potential for terrorist or politically motivated attacks against information systems which form part of the critical infrastructure of Member States and of the Union. This constitutes a threat to the achievement of a safer information society and of an area of freedom, security, and justice, and therefore requires a response at Union level and improved cooperation and coordination at international level.

               (4)

               There are a number of critical infrastructures in the Union, the disruption or destruction of which would have a significant cross-border impact. It has become apparent from the need to increase the critical infrastructure protection capability in the Union that the measures against cyber attacks should be complemented by stringent criminal penalties reflecting the gravity of such attacks. Critical infrastructure could be understood to be an asset, system or part thereof located in Member States, which is essential for the maintenance of vital societal functions, health, safety, security, economic or social well-being of people, such as power plants, transport networks or government networks, and the disruption or destruction of which would have a significant impact in a Member State as a result of the failure to maintain those functions.

               (5)

               There is evidence of a tendency towards increasingly dangerous and recurrent large-scale attacks conducted against information systems which can often be critical to Member States or to particular functions in the public or private sector. This tendency is accompanied by the development of increasingly sophisticated methods, such as the creation and use of so-called ‘botnets’, which involves several stages of a criminal act, where each stage alone could pose a serious risk to public interests. This Directive aims, inter alia, to introduce criminal penalties for the creation of botnets, namely, the act of establishing remote control over a significant number of computers by infecting them with malicious software through targeted cyber attacks. Once created, the infected network of computers that constitute the botnet can be activated without the computer users’ knowledge in order to launch a large-scale cyber attack, which usually has the capacity to cause serious damage, as referred to in this Directive. Member States may determine what constitutes serious damage according to their national law and practice, such as disrupting system services of significant public importance, or causing major financial cost or loss of personal data or sensitive information.

               (6)

               Large-scale cyber attacks can cause substantial economic damage both through the interruption of information systems and communication and through the loss or alteration of commercially important confidential information or other data. Particular attention should be paid to raising the awareness of innovative small and medium-sized enterprises to threats relating to such attacks and their vulnerability to such attacks, due to their increased dependence on the proper functioning and availability of information systems and often limited resources for information security.

               (7)

               Common definitions in this area are important in order to ensure a consistent approach in the Member States to the application of this Directive.

               (8)

               There is a need to achieve a common approach to the constituent elements of criminal offences by introducing common offences of illegal access to an information system, illegal system interference, illegal data interference, and illegal interception.

               (9)

               Interception includes, but is not necessarily limited to, the listening to, monitoring or surveillance of the content of communications and the procuring of the content of data either directly, through access and use of the information systems, or indirectly through the use of electronic eavesdropping or tapping devices by technical means.

               (10)

               Member States should provide for penalties in respect of attacks against information systems. Those penalties should be effective, proportionate and dissuasive and should include imprisonment and/or fines.

               (11)

               This Directive provides for criminal penalties at least for cases which are not minor. Member States may determine what constitutes a minor case according to their national law and practice. A case may be considered minor, for example, where the damage caused by the offence and/or the risk to public or private interests, such as to the integrity of a computer system or to computer data, or to the integrity, rights or other interests of a person, is insignificant or is of such a nature that the imposition of a criminal penalty within the legal threshold or the imposition of criminal liability is not necessary.

               (12)

               The identification and reporting of threats and risks posed by cyber attacks and the related vulnerability of information systems is a pertinent element of effective prevention of, and response to, cyber attacks and to improving the security of information systems. Providing incentives to report security gaps could add to that effect. Member States should endeavour to provide possibilities for the legal detection and reporting of security gaps.

               (13)

               It is appropriate to provide for more severe penalties where an attack against an information system is committed by a criminal organisation, as defined in Council Framework Decision 2008/841/JHA of 24 October 2008 on the fight against organised crime (3), where a cyber attack is conducted on a large scale, thus affecting a significant number of information systems, including where it is intended to create a botnet, or where a cyber attack causes serious damage, including where it is carried out through a botnet. It is also appropriate to provide for more severe penalties where an attack is conducted against a critical infrastructure of the Member States or of the Union.

               (14)

               Setting up effective measures against identity theft and other identity-related offences constitutes another important element of an integrated approach against cybercrime. Any need for Union action against this type of criminal behaviour could also be considered in the context of evaluating the need for a comprehensive horizontal Union instrument.

               (15)

               The Council Conclusions of 27 to 28 November 2008 indicated that a new strategy should be developed with the Member States and the Commission, taking into account the content of the 2001 Council of Europe Convention on Cybercrime. That Convention is the legal framework of reference for combating cybercrime, including attacks against information systems. This Directive builds on that Convention. Completing the process of ratification of that Convention by all Member States as soon as possible should be considered to be a priority.

               (16)

               Given the different ways in which attacks can be conducted, and given the rapid developments in hardware and software, this Directive refers to tools that can be used in order to commit the offences laid down in this Directive. Such tools could include malicious software, including those able to create botnets, used to commit cyber attacks. Even where such a tool is suitable or particularly suitable for carrying out one of the offences laid down in this Directive, it is possible that it was produced for a legitimate purpose Motivated by the need to avoid criminalisation where such tools are produced and put on the market for legitimate purposes, such as to test the reliability of information technology products or the security of information systems, apart from the general intent requirement, a direct intent requirement that those tools be used to commit one or more of the offences laid down in this Directive must be also fulfilled.

               (17)

               This Directive does not impose criminal liability where the objective criteria of the offences laid down in this Directive are met but the acts are committed without criminal intent, for instance where a person does not know that access was unauthorised or in the case of mandated testing or protection of information systems, such as where a person is assigned by a company or vendor to test the strength of its security system. In the context of this Directive, contractual obligations or agreements to restrict access to information systems by way of a user policy or terms of service, as well as labour disputes as regards the access to and use of information systems of an employer for private purposes, should not incur criminal liability where the access under such circumstances would be deemed unauthorised and thus would constitute the sole basis for criminal proceedings. This Directive is without prejudice to the right of access to information as laid down in national and Union law, while at the same time it may not serve as a justification for unlawful or arbitrary access to information.

               (18)

               Cyber attacks could be facilitated by various circumstances, such as where the offender has access to security systems inherent in the affected information systems within the scope of his or her employment. In the context of national law, such circumstances should be taken into account in the course of criminal proceedings as appropriate.

               (19)

               Member States should provide for aggravating circumstances in their national law in accordance with the applicable rules established by their legal systems on aggravating circumstances. They should ensure that those aggravating circumstances are available for judges to consider when sentencing offenders. It remains within the discretion of the judge to assess those circumstances together with the other facts of the particular case.

               (20)

               This Directive does not govern conditions for exercising jurisdiction over any of the offences referred to herein, such as a report by the victim in the place where the offence was committed, a denunciation from the State of the place where the offence was committed, or the non-prosecution of the offender in the place where the offence was committed.

               (21)

               In the context of this Directive, States and public bodies remain fully bound to guarantee respect for human rights and fundamental freedoms, in accordance with existing international obligations.

               (22)

               This Directive strengthens the importance of networks, such as the G8 or the Council of Europe’s network of points of contact available on a 24 hour, seven-day-a-week basis. Those points of contact should be able to deliver effective assistance thus, for example, facilitating the exchange of relevant information available and the provision of technical advice or legal information for the purpose of investigations or proceedings concerning criminal offences relating to information systems and associated data involving the requesting Member State. In order to ensure the smooth operation of the networks, each contact point should have the capacity to communicate with the point of contact of another Member State on an expedited basis with the support, inter alia, of trained and equipped personnel. Given the speed with which large-scale cyber attacks can be carried out, Member States should be able to respond promptly to urgent requests from this network of contact points. In such cases, it may be expedient that the request for information be accompanied by telephone contact in order to ensure that the request is processed swiftly by the requested Member State and that feedback is provided within eight hours.

               (23)

               Cooperation between public authorities on the one hand, and the private sector and civil society on the other, is of great importance in preventing and combating attacks against information systems. It is necessary to foster and improve cooperation between service providers, producers, law enforcement bodies and judicial authorities, while fully respecting the rule of law. Such cooperation could include support by service providers in helping to preserve potential evidence, in providing elements helping to identify offenders and, as a last resort, in shutting down, completely or partially, in accordance with national law and practice, information systems or functions that have been compromised or used for illegal purposes. Member States should also consider setting up cooperation and partnership networks with service providers and producers for the exchange of information in relation to the offences within the scope of this Directive.

               (24)

               There is a need to collect comparable data on the offences laid down in this Directive. Relevant data should be made available to the competent specialised Union agencies and bodies, such as Europol and ENISA, in line with their tasks and information needs, in order to gain a more complete picture of the problem of cybercrime and network and information security at Union level and thereby to contribute to formulating a more effective response. Member States should submit information on the modus operandi of the offenders to Europol and its European Cybercrime Centre for the purpose of conducting threat assessments and strategic analyses of cybercrime in accordance with Council Decision 2009/371/JHA of 6 April 2009 establishing the European Police Office (Europol) (4). Providing information can facilitate a better understanding of present and future threats and thus contribute to more appropriate and targeted decision-making on combating and preventing attacks against information systems.

               (25)

               The Commission should submit a report on the application of this Directive and make necessary legislative proposals which could lead to broadening its scope, taking into account developments in the field of cybercrime. Such developments could include technological developments, for example those enabling more effective enforcement in the area of attacks against information systems or facilitating prevention or minimising the impact of such attacks. For that purpose, the Commission should take into account the available analyses and reports produced by relevant actors and, in particular, Europol and ENISA.

               (26)

               In order to fight cybercrime effectively, it is necessary to increase the resilience of information systems by taking appropriate measures to protect them more effectively against cyber attacks. Member States should take the necessary measures to protect their critical infrastructure from cyber attacks, as part of which they should consider the protection of their information systems and associated data. Ensuring an adequate level of protection and security of information systems by legal persons, for example in connection with the provision of publicly available electronic communications services in accordance with existing Union legislation on privacy and electronic communication and data protection, forms an essential part of a comprehensive approach to effectively counteracting cybercrime. Appropriate levels of protection should be provided against reasonably identifiable threats and vulnerabilities in accordance with the state of the art for specific sectors and the specific data processing situations. The cost and burden of such protection should be proportionate to the likely damage a cyber attack would cause to those affected. Member States are encouraged to provide for relevant measures incurring liabilities in the context of their national law in cases where a legal person has clearly not provided an appropriate level of protection against cyber attacks.

               (27)

               Significant gaps and differences in Member States’ laws and criminal procedures in the area of attacks against information systems may hamper the fight against organised crime and terrorism, and may complicate effective police and judicial cooperation in this area. The transnational and borderless nature of modern information systems means that attacks against such systems have a cross-border dimension, thus underlining the urgent need for further action to approximate criminal law in this area. In addition, the coordination of prosecution of cases of attacks against information systems should be facilitated by the adequate implementation and application of Council Framework Decision 2009/948/JHA of 30 November 2009 on prevention and settlement of conflict of jurisdiction in criminal proceedings (5). Member States, in cooperation with the Union, should also seek to improve international cooperation relating to the security of information systems, computer networks and computer data. Proper consideration of the security of data transfer and storage should be given in any international agreement involving data exchange.

               (28)

               Improved cooperation between the competent law enforcement bodies and judicial authorities across the Union is essential in an effective fight against cybercrime. In this context, stepping up the efforts to provide adequate training to the relevant authorities in order to raise the understanding of cybercrime and its impact, and to foster cooperation and the exchange of best practices, for example via the competent specialised Union agencies and bodies, should be encouraged. Such training should, inter alia, aim at raising awareness about the different national legal systems, the possible legal and technical challenges of criminal investigations, and the distribution of competences between the relevant national authorities.

               (29)

               This Directive respects human rights and fundamental freedoms and observes the principles recognised in particular by the Charter of Fundamental Rights of the European Union and the European Convention for the Protection of Human Rights and Fundamental Freedoms, including the protection of personal data, the right to privacy, freedom of expression and information, the right to a fair trial, the presumption of innocence and the rights of the defence, as well as the principles of legality and proportionality of criminal offences and penalties. In particular, this Directive seeks to ensure full respect for those rights and principles and must be implemented accordingly.

               (30)

               The protection of personal data is a fundamental right in accordance with Article 16(1) TFEU and Article 8 of the Charter on Fundamental Rights of the European Union. Therefore, any processing of personal data in the context of the implementation of this Directive should fully comply with the relevant Union law on data protection.

               (31)

               In accordance with Article 3 of the Protocol on the position of the United Kingdom and Ireland in respect of the Area of Freedom, Security and Justice, annexed to the Treaty on European Union and to the Treaty on the Functioning of the European Union, those Member States have notified their wish to take part in the adoption and application of this Directive.

               (32)

               In accordance with Articles 1 and 2 of the Protocol on the position of Denmark annexed to the Treaty on European Union and to the Treaty on the Functioning of the European Union, Denmark is not taking part in the adoption of this Directive and is not bound by it or subject to its application.

               (33)

               Since the objectives of this Directive, namely to subject attacks against information systems in all Member States to effective, proportionate and dissuasive criminal penalties and to improve and encourage cooperation between judicial and other competent authorities, cannot be sufficiently achieved by the Member States, and can therefore, by reason of their scale or effects, be better achieved at Union level, the Union may adopt measures in accordance with the principle of subsidiarity as set out in Article 5 of the Treaty on European Union. In accordance with the principle of proportionality, as set out in that Article, this Directive does not go beyond what is necessary in order to achieve those objectives.

               (34)

               This Directive aims to amend and expand the provisions of Council Framework Decision 2005/222/JHA of 24 February 2005 on attacks against information systems (6). Since the amendments to be made are of substantial number and nature, Framework Decision 2005/222/JHA should, in the interests of clarity, be replaced in its entirety in relation to Member States participating in the adoption of this Directive,

         HAVE ADOPTED THIS DIRECTIVE:
   Article 1
   Subject matter
   This Directive establishes minimum rules concerning the definition of criminal offences and sanctions in the area of attacks against information systems. It also aims to facilitate the prevention of such offences and to improve cooperation between judicial and other competent authorities.
   Article 2
   Definitions
   For the purposes of this Directive, the following definitions shall apply:

               (a)

               ‘information system’ means a device or group of inter-connected or related devices, one or more of which, pursuant to a programme, automatically processes computer data, as well as computer data stored, processed, retrieved or transmitted by that device or group of devices for the purposes of its or their operation, use, protection and maintenance;

               (b)

               ‘computer data’ means a representation of facts, information or concepts in a form suitable for processing in an information system, including a programme suitable for causing an information system to perform a function;

               (c)

               ‘legal person’ means an entity having the status of legal person under the applicable law, but does not include States or public bodies acting in the exercise of State authority, or public international organisations;

               (d)

               ‘without right’ means conduct referred to in this Directive, including access, interference, or interception, which is not authorised by the owner or by another right holder of the system or of part of it, or not permitted under national law.

         Article 3
   Illegal access to information systems
   Member States shall take the necessary measures to ensure that, when committed intentionally, the access without right, to the whole or to any part of an information system, is punishable as a criminal offence where committed by infringing a security measure, at least for cases which are not minor.
   Article 4
   Illegal system interference
   Member States shall take the necessary measures to ensure that seriously hindering or interrupting the functioning of an information system by inputting computer data, by transmitting, damaging, deleting, deteriorating, altering or suppressing such data, or by rendering such data inaccessible, intentionally and without right, is punishable as a criminal offence, at least for cases which are not minor.
   Article 5
   Illegal data interference
   Member States shall take the necessary measures to ensure that deleting, damaging, deteriorating, altering or suppressing computer data on an information system, or rendering such data inaccessible, intentionally and without right, is punishable as a criminal offence, at least for cases which are not minor.
   Article 6
   Illegal interception
   Member States shall take the necessary measures to ensure that intercepting, by technical means, non-public transmissions of computer data to, from or within an information system, including electromagnetic emissions from an information system carrying such computer data, intentionally and without right, is punishable as a criminal offence, at least for cases which are not minor.
   Article 7
   Tools used for committing offences
   Member States shall take the necessary measures to ensure that the intentional production, sale, procurement for use, import, distribution or otherwise making available, of one of the following tools, without right and with the intention that it be used to commit any of the offences referred to in Articles 3 to 6, is punishable as a criminal offence, at least for cases which are not minor:

               (a)

               a computer programme, designed or adapted primarily for the purpose of committing any of the offences referred to in Articles 3 to 6;

               (b)

               a computer password, access code, or similar data by which the whole or any part of an information system is capable of being accessed.

         Article 8
   Incitement, aiding and abetting and attempt
   1.   Member States shall ensure that the incitement, or aiding and abetting, to commit an offence referred to in Articles 3 to 7 is punishable as a criminal offence.
   2.   Member States shall ensure that the attempt to commit an offence referred to in Articles 4 and 5 is punishable as a criminal offence.
   Article 9
   Penalties
   1.   Member States shall take the necessary measures to ensure that the offences referred to in Articles 3 to 8 are punishable by effective, proportionate and dissuasive criminal penalties.
   2.   Member States shall take the necessary measures to ensure that the offences referred to in Articles 3 to 7 are punishable by a maximum term of imprisonment of at least two years, at least for cases which are not minor.
   3.   Member States shall take the necessary measures to ensure that the offences referred to in Articles 4 and 5, when committed intentionally, are punishable by a maximum term of imprisonment of at least three years where a significant number of information systems have been affected through the use of a tool, referred to in Article 7, designed or adapted primarily for that purpose.
   4.   Member States shall take the necessary measures to ensure that offences referred to in Articles 4 and 5 are punishable by a maximum term of imprisonment of at least five years where:

               (a)

               they are committed within the framework of a criminal organisation, as defined in Framework Decision 2008/841/JHA, irrespective of the penalty provided for therein;

               (b)

               they cause serious damage; or

               (c)

               they are committed against a critical infrastructure information system.

         5.   Member States shall take the necessary measures to ensure that when the offences referred to in Articles 4 and 5 are committed by misusing the personal data of another person, with the aim of gaining the trust of a third party, thereby causing prejudice to the rightful identity owner, this may, in accordance with national law, be regarded as aggravating circumstances, unless those circumstances are already covered by another offence, punishable under national law.
   Article 10
   Liability of legal persons
   1.   Member States shall take the necessary measures to ensure that legal persons can be held liable for offences referred to in Articles 3 to 8, committed for their benefit by any person, acting either individually or as part of a body of the legal person, and having a leading position within the legal person, based on one of the following:

               (a)

               a power of representation of the legal person;

               (b)

               an authority to take decisions on behalf of the legal person;

               (c)

               an authority to exercise control within the legal person.

         2.   Member States shall take the necessary measures to ensure that legal persons can be held liable where the lack of supervision or control by a person referred to in paragraph 1 has allowed the commission, by a person under its authority, of any of the offences referred to in Articles 3 to 8 for the benefit of that legal person.
   3.   The liability of legal persons under paragraphs 1 and 2 shall not exclude criminal proceedings against natural persons who are perpetrators or inciters of, or accessories to, any of the offences referred to in Articles 3 to 8.
   Article 11
   Sanctions against legal persons
   1.   Member States shall take the necessary measures to ensure that a legal person held liable pursuant to Article 10(1) is punishable by effective, proportionate and dissuasive sanctions, which shall include criminal or non-criminal fines and which may include other sanctions, such as:

               (a)

               exclusion from entitlement to public benefits or aid;

               (b)

               temporary or permanent disqualification from the practice of commercial activities;

               (c)

               placing under judicial supervision;

               (d)

               judicial winding-up;

               (e)

               temporary or permanent closure of establishments which have been used for committing the offence.

         2.   Member States shall take the necessary measures to ensure that a legal person held liable pursuant to Article 10(2) is punishable by effective, proportionate and dissuasive sanctions or other measures.
   Article 12
   Jurisdiction
   1.   Member States shall establish their jurisdiction with regard to the offences referred to in Articles 3 to 8 where the offence has been committed:

               (a)

               in whole or in part within their territory; or

               (b)

               by one of their nationals, at least in cases where the act is an offence where it was committed.

         2.   When establishing jurisdiction in accordance with point (a) of paragraph 1, a Member State shall ensure that it has jurisdiction where:

               (a)

               the offender commits the offence when physically present on its territory, whether or not the offence is against an information system on its territory; or

               (b)

               the offence is against an information system on its territory, whether or not the offender commits the offence when physically present on its territory.

         3.   A Member State shall inform the Commission where it decides to establish jurisdiction over an offence referred to in Articles 3 to 8 committed outside its territory, including where:

               (a)

               the offender has his or her habitual residence in its territory; or

               (b)

               the offence is committed for the benefit of a legal person established in its territory.

         Article 13
   Exchange of information
   1.   For the purpose of exchanging information relating to the offences referred to in Articles 3 to 8, Member States shall ensure that they have an operational national point of contact and that they make use of the existing network of operational points of contact available 24 hours a day and seven days a week. Member States shall also ensure that they have procedures in place so that for urgent requests for assistance, the competent authority can indicate, within eight hours of receipt, at least whether the request will be answered, and the form and estimated time of such an answer.
   2.   Member States shall inform the Commission of their appointed point of contact referred to in paragraph 1. The Commission shall forward that information to the other Member States and competent specialised Union agencies and bodies.
   3.   Member States shall take the necessary measures to ensure that appropriate reporting channels are made available in order to facilitate the reporting of the offences referred to in Article 3 to 6 to the competent national authorities without undue delay.
   Article 14
   Monitoring and statistics
   1.   Member States shall ensure that a system is in place for the recording, production and provision of statistical data on the offences referred to in Articles 3 to 7.
   2.   The statistical data referred to in paragraph 1 shall, as a minimum, cover existing data on the number of offences referred to in Articles 3 to 7 registered by the Member States, and the number of persons prosecuted for and convicted of the offences referred to in Articles 3 to 7.
   3.   Member States shall transmit the data collected pursuant to this Article to the Commission. The Commission shall ensure that a consolidated review of the statistical reports is published and submitted to the competent specialised Union agencies and bodies.
   Article 15
   Replacement of Framework Decision 2005/222/JHA
   Framework Decision 2005/222/JHA is hereby replaced in relation to Member States participating in the adoption of this Directive, without prejudice to the obligations of the Member States relating to the time limit for transposition of the Framework Decision into national law.
   In relation to Member States participating in the adoption of this Directive, references to the Framework Decision 2005/222/JHA shall be construed as references to this Directive.
   Article 16
   Transposition
   1.   Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive by 4 September 2015.
   2.   Member States shall transmit to the Commission the text of the measures transposing into their national law the obligations imposed on them under this Directive.
   3.   When Member States adopt those measures, they shall contain a reference to this Directive or shall be accompanied by such a reference on the occasion of their official publication. The methods of making such a reference shall be laid down by the Member States.
   Article 17
   Reporting
   The Commission shall, by 4 September 2017, submit a report to the European Parliament and the Council, assessing the extent to which the Member States have taken the necessary measures in order to comply with this Directive, accompanied, if necessary, by legislative proposals. The Commission shall also take into account the technical and legal developments in the field of cybercrime, particularly with regard to the scope of this Directive.
   Article 18
   Entry into force
   This Directive shall enter into force on the twentieth day following that of its publication in the Official Journal of the European Union.
   Article 19
   Addressees
   This Directive is addressed to the Member States in accordance with the Treaties.

      Done at Brussels, 12 August 2013.

            For the European Parliament

            The President

         M. SCHULZ

            For the Council

            The President

         L. LINKEVIČIUS

      (1)  OJ C 218, 23.7.2011, p. 130.

      (2)  Position of the European Parliament of 4 July 2013 (not yet published in the Official Journal) and decision of the Council of 22 July 2013.

      (3)  OJ L 300, 11.11.2008, p. 42.

      (4)  OJ L 121, 15.5.2009, p. 37.

      (5)  OJ L 328, 15.12.2009, p. 42.

      (6)  OJ L 69, 16.3.2005, p. 67.


Avis juridique important

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31985L0503

First Commission Directive 85/503/EEC of 25 October 1985 on methods of analysis for edible caseins and caseinates

Official Journal L 308 , 20/11/1985 P. 0012 - 0024 Finnish special edition: Chapter 13 Volume 14 P. 0208  Spanish special edition: Chapter 13 Volume 19 P. 0020  Swedish special edition: Chapter 13 Volume 14 P. 0208  Portuguese special edition Chapter 13 Volume 19 P. 0020

*****FIRST  COMMISSION DIRECTIVE  of 25 October 1985  on methods of analysis for edible caseins and caseinates  (85/503/EEC)  THE COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community,  Having regard to Council Directive 83/417/EEC of 25 July 1983 on the approximation of the laws of the Member States relating to certain lactoproteins (caseins and caseinates) intended for human consumption (1), and in particular Article 9 (b) thereof;  Whereas Article 9 (b) of Directive 83/417/EEC requires that Community methods of analysis be determined for checking the composition of certain edible caseins and caseinates;  Whereas it is possible to adopt an initial series of methods in respect of which studies have been completed;  Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Foodstuffs,  HAS ADOPTED THIS DIRECTIVE:  Article 1  Member States shall take all measures necessary to ensure that the analyses necessary for verification of the criteria set out in Annex I are carried out in accordance with the methods described in Annex II.  Article 2  Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive by 1 May 1987 at the latest. They shall forthwith inform the Commission thereof.  Article 3  This Directive is addressed to the Member States.  Done at Brussels, 25 October 1985.  For the Commission  COCKFIELD  Vice-President  (1) OJ No L 237, 26. 8. 1983, p. 25.  ANNEX I  SCOPE OF THE FIRST COMMUNITY METHODS OF ANALYSIS DIRECTIVE FOR EDIBLE CASEINS AND CASEINATES  1.2 // I.   // General Provisions   // II.   // Determination of moisture in:   //   // - acid caseins using method 1, Annex II   //   // - rennet caseins using method 1, Annex II   //  // - caseinates using method 1, Annex II   // III.  // Determination of protein content in:   //   // - acid caseins using method 2, Annex II   //   // - rennet caseins using method 2, Annex II   //   // - caseinates using method 2, Annex II   // IV.   // Determination of titratable acidity in:  //   // - acid caseins using method 3, Annex II   // V.  // Determination of ash (including P2O5) in:   //   // - acid caseins using method 4, Annex II   //   // - rennet caseins using method 5, Annex II   // VI.   // Determination of pH in:  //   // - caseinates using method 6, Annex II  ANNEX II  METHODS OF ANALYSIS RELATING TO THE COMPOSITION OF EDIBLE CASEINS AND CASEINATES  GENERAL PROVISIONS  1.2 // 1.   // PREPARATION OF THE ANALYSIS SAMPLE   // 1.1.  // General   //   // The mass of the sample presented to the laboratory for analysis shall be at least 200 grams.   // 1.2.  // Preparation of the sample for analysis in the laboratory  // 1.2.1.   // Thoroughly mix and break down any lumps, etc., in the laboratory sample by repeatedly shaking and inverting the container (if necessary, after having transferred all of the laboratory sample to an air-tight container of sufficient capacity (twice volume of sample) to allow this operation to be carried out).   // 1.2.2.   // Transfer a representative portion of the sample, i. e. about 50 grams of the thoroughly mixed laboratory sample (1.2.1) to the test sieve (3.3).  // 1.2.3.   // If the 50 gram portion completely or almost completely passes (at least 95 % by weight) through the sieve (3.3), use for the determination the sample as prepared in 1.2.1.   // 1.2.4.   // Otherwise, grind the 50 gram portion, using the grinding device (3.4), until it satisfies the sieving criterion (1.2.3). Immediately transfer all the sieved sample to an air-tight container of sufficient capacity (twice volume of sample) and mix thoroughly by repeated shaking and inverting. During these operations, take precautions to avoid any change in the moisture content of the product.   // 1.2.5.  // After the test sample has been prepared, any determination should be proceeded with as soon as possible.   // 1.3.  // Containers   //   // The sample shall always be kept in an air-tight and moisture-tight container.   // 2.   // REAGENTS  // 2.1.   // Water   // 2.1.1.   // Wherever mention is made to water for solution, dilution or washing purposes, distilled water, or demineralized water of at least equivalent purity, shall be used.   // 2.1.2.   // Wherever reference is made to 'solution' or 'dilution' without further indication, 'solution in water' or 'dilution with water' is meant.   // 2.2.  // Chemicals   //   // All chemicals used shall be of recognized analytical reagent quality except where otherwise specified.   // 3.   // EQUIPMENT   // 3.1.   // Lists of equipment   //   // The lists of equipment contain only those items with a specialized use and items to a particular specification.   // 3.2.   // Analytical balance   //  // Analytical balance means a balance capable of weighing to at least 0,1 mg.   // 3.3.   // Test sieve   //   // The test sieves to be used are to be fitted with a lid, to be of diameter 200 mm, to be constructed of wire cloth with a nominal aperture size of 500 mm. The aperture tolerances and wire diameters to be permitted are as given in ISO 3310/1. (Test sieves - Technical requirements and testing - Part 1: Metal wire cloth. ISO 3310/1 - 1975).   //   // The sieves are to be fitted with a receiver.   // 3.4.   // Grinding device   //  // For grinding the laboratory sample if necessary (see 1.2.4), without development of undue heat and without loss or absorption of moisture, a hammer mill shall not be used.  // 4.   // EXPRESSION OF RESULTS   // 4.1.   // Results   //  // The result stated in the analytical report is to be the mean value obtained from two determinations which satisfy the repeatability criterion for that method.   // 4.2.  // Calculation of percentage   //   // Except where otherwise specified, the result shall be calculated as a percentage by mass of the sample.   // 5.   // TEST REPORT   //   // The test report shall identify the method of analysis used as well as the results obtained. In addition, it shall mention all details of procedure not specified in the method of analysis or which are optional, as well as any circumstances that may have influenced the results obtained. The test report shall give all the information necessary for the complete identification of the sample.  METHOD 1  DETERMINATION OF MOISTURE CONTENT  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method determines the moisture content in:   //   // - acid caseins   //   // - rennet caseins   //   // - caseinates  // 2.   // DEFINITION   //   // The moisture content of caseins and caseinates: the loss of mass as determined by the method specified.   // 3.   // PRINCIPLE   //   // The residual mass of a test portion is determined after drying at atmospheric pressure in an oven at 102 °C ± 1 °C to constant mass. The loss of mass is calculated as a percentage by mass of the sample.   // 4.   // APPARATUS   // 4.1.   // Analytical balance   // 4.2.   // Dishes, flat-bottomed and of material non-corrodible under the conditions of test e.g. nickel, aluminium, stainless steel or glass. The dishes must have lids which fit tightly but which can readily be removed. Suitable dimensions are: diameter 60 to 80 mm and depth about 25 mm.  // 4.3.   // Atmospheric pressure drying oven, well ventilated, thermostatically controlled with temperature regulation (at 102 °C ± 1 °C). The temperature should be uniform throughout the oven.   // 4.4.   // Desiccator, containing freshly activated silica gel with a water content indicator or an equivalent desiccant.   // 4.5.   // Suitable device for handling dishes, e.g. laboratory tongs.   // 5.  // PROCEDURE   // 5.1.   // Preparation of the test sample  //   // As described in Section 1.2 of the General Provisions.  METHOD 2  DETERMINATION OF PROTEIN CONTENT  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method determines the protein content of:   //   // - acid caseins,   //   // - rennet caseins,   //   // - caseinates,  //   // except those containing ammonium caseinate or other ammonium or nitrogenous non-protein compounds.  // 2.   // DEFINITION   //   // The protein content: the nitrogen content as determined by the method specified and then multiplied by 6,38 and expressed as a percentage by mass.  // 3.   // PRINCIPLE   //   // A test portion is digested with a mixture of potassium sulphate and sulphuric acid, in the presence of copper (II) sulphate as catalyst, to convert organic nitrogen to ammoniacal nitrogen. The ammonia is distilled and absorbed into boric acid solution and then titrated with standard hydrochloric acid solution. The nitrogen content is converted to protein content by multiplying by 6,38.   // 4.   // REAGENTS   // 4.1.   // Sulphuric acid, concentrated, S2O 1,84 g/ml.   // 4.2.   // Potassium sulphate, anhydrous (K2SO4).   // 4.3.   // Copper (II) sulphate pentahydrate (CuSO45H2O).   // 4.4.   // Sucrose (C12H22O11).  // 4.5.   // Boric acid, 40-g/l solution.   // 4.6.  // Sodium hydroxide, concentrated aqueous solution 30 % (m/m), carbonate free.   // 4.7.   // Hydrochloric acid, 0,1 mol/l.  // 4.8.   // Mixed indicator. Mix equal volumes of a 2 g/l solution of methyl red in at least 95 % (V/V) ethanol and a 1 g/l solution of methylene blue in at least 95 % (V/V) ethanol.  // 5.   // APPARATUS   // 5.1.   // Analytical balance  // 5.2.   // Kjeldahl flask, 500 ml capacity.   // 5.3.  // Digestion apparatus to hold the Kjeldahl flask (5.2) in an inclined position and with a heating device which will not heat the part of the flask above the surface of the liquid contents.   // 5.4.   // Condenser with straight inner tube.   // 5.5.  // Outlet tube with safety bulb connected to the lower end of the condenser (5.4) by a ground glass joint or a rubber tube. If rubber tubing is used, the glass ends must be near one another.   // 5.6.   // Splash-head connected to the Kjeldahl flask (5.2) and to the condenser (5.4) by soft, close-fitting rubber or other appropriate stoppers.   // 5.7.   // Conical flask, 500 ml capacity.   // 5.8.   // Graduated cylinders, 50 ml and 100 ml capacity.   // 5.9.   // Burette, 50 ml capacity, graduated in 0,1 ml.   // 5.10.   // Boiling aids:   // 5.10.1.   // For the digestion: small pieces of hard porcelain, or glass beads.   // 5.10.2.   // For the distillation; freshly calcined pieces of pumice.   // 6.   // PROCEDURE   // 6.1.  // Preparation of the test sample   //   // As described in Section 1.2 of the General Provisions.  // 6.2.   // Test for presence of ammoniacal nitrogen   //  // If the presence of ammonium caseinate or other ammonium compounds is suspected, carry out the following test. Add to 1 gram of sample in a small conical flask 10 ml of water and 100 mg of magnesium oxide. Rinse down any magnesium oxide adhering to the walls and close the flask with a cork stopper, inserting a piece of moistened red litmus paper between the stopper and the neck of the flask. Mix the contents of the flask carefully and heat the flask in a water bath at 60 to 65 °C. If the litmus paper colours blue within 15 minutes ammonia is present, and the method is not applicable (see Section 1).   // 6.3.  // Blank test   //   // At the same time as the determination of the nitrogen content of the sample perform a blank determination using 0,5 grams of the sucrose (4.4) instead of the test portion, using the same apparatus, the same quantities of all reagents and the same procedure as described in 6.5. If the titration in the blank determination exceeds 0,5 ml of 0,1 mol/l acid, the reagents shall be checked and the impure reagent or reagents purified or replaced.   // 6.4.   // Test portion   //   // Transfer to the Kjeldahl flask (5.2) 0,3 to 0,4 grams of the test sample (6.1), weighed to the nearest 0,1 mg.   // 6.5.   // Determination   // 6.5.1.   // Transfer to the flask a few pieces of porcelain or a few glass beads (5.10.1) and about 10 grams of the anhydrous potassium sulphate (4.2).   //   // Add 0,2 g of the copper (II) sulphate (4.3) and wash down the neck of the flask with a little water. Add 20 ml of the concentrated sulphuric acid (4.1). Mix the contents of the flask.   //   // Heat gently on the digestion apparatus (5.3) until any frothing has ceased, boil gently until the solution is clear and a pale green-blue colour persists. During heating, swirl the flask occasionally.   //   // Continue the boiling, regulating the heating so as to condense the vapours in the middle of the flask neck. Continue the heating for 90 minutes avoiding local overheating.   //   // Allow to cool to room temperature. Carefully add about 200 ml of water and a few pieces of pumice (5.10.2). Mix and cool again.   // 6.5.2.  // Transfer into the conical flask (5.7) 50 ml of the boric acid solution (4.5) and four drops of the indicator (4.8). Mix. Place the conical flask under the condenser (5.4) so that the tip of the outlet tube (5.5) is immersed in the boric acid solution. Using a graduated cylinder (5.8), add to the Kjeldahl flask 80 ml of the sodium hydroxide solution (4.6). During this operation, hold the flask in an inclined position so that the sodium hydroxide solution runs down the side of the flask to form a bottom layer.   //   // Immediately connect the Kjeldahl flask to the condenser by means of the splash-head (5.6).   //  // Gently rotate the Kjeldahl flask to mix its contents. Boil gently at first, avoiding any frothing. Continue the distillation so that 150 ml of distillate are collected in approximately 30 minutes. The distillate should have a temperature below 25 °C. About two minutes before the end of the distillation, lower the conical flask so that the tip of the outlet tube is no longer immersed in the acid solution, and rinse the tip with a little water. Stop heating, remove the outlet tube and rinse its outer and inner walls with a little water, collecting the washings in the conical flask.  // 6.5.3.   // Titrate the distillate in the conical flask, using the standard volumetric hydrochloric acid solution (4.7).   // 7.   // EXPRESSION OF RESULTS   // 7.1.   // Formula and method of calculation   //   // The protein content of the sample, expressed as a percentage by mass, is given by: 1.2.3.4.5 //   //   // (V1 - V2) × T × 14 × 100 × 6,38 m × 1 000   // =   // 8,932 (V1 - V2) × T m  1.2 //  // where:   //   //  1.2.3 //   // V1   // is the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4.7) used in the determination (6.5);   //  // V2   // is the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4.7) used in the blank test (6.3);   //   // T   // is the strength of the standard volumetric hydrochloric acid solution (4.7) in mol/l;   //  // m   // is the mass, in grams, of the test portion.  1.2 //  // Calculate the protein content to the nearest 0,1 %.  // 7.2.   // Repeatability   //   // The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst under the same conditions shall not exceed 0,5 grams of protein per 100 grams of product.   //   // This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.  METHOD 3  DETERMINATION OF TITRATABLE ACIDITY  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // The method determines the titratable acidity of:   //   // - acid caseins.   // 2.   // DEFINITION   //   // The titratable acidity of acid caseins: the volume in millilitres, of a 0,1 mol/l standard sodium hydroxide solution required to neutralize an aqueous extract of 1 gram of the product.   // 3.  // PRINCIPLE   //   // An aqueous extract of the sample at 60 °C is obtained and filtered. The filtrate is titrated against standard sodium hydroxide using phenolphtalein indicator.  // 4.   // REAGENTS   //   // Any water used in the method procedure or in the preparation of reagents shall be freed from carbon dioxide by boiling for 10 minutes before use.   // 4.1.  // Sodium hydroxide solution: 0,1 Mol/l.   // 4.2.  // Phenolphtalein indicator solution, 10 g/l in ethanol (95 % V/V) neutralized to the indicator.   // 5.   // APPARATUS  // 5.1.   // Analytical balance   // 5.2.   // Conical flask, 500 ml capacity, with ground neck and fitted with a ground glass stopper.   // 5.3.   // One-mark pipette, 100 ml capacity.   // 5.4.   // Pipette, suitable for measuring 0,5 ml of indicator solution (4.2).   // 5.5.   // Conical flask, 250 ml capacity.   // 5.6.   // Measuring cylinder, 250 ml capacity.   // 5.7.   // Burette, graduated in 0,1 ml.  // 5.8.   // Water bath, capable of being controlled at a temperature of 60 °C ± 2 °C.   // 5.9.   // Appropriate filter  // 6.   // PROCEDURE   // 6.1.   // Preparation of the test sample   //   // As described in Section 1.2 of the General Provisions.  // 6.2.   // Test portion   //   // Weigh about 10 grams of the test sample (6.1) to the nearest 10 mg and transfer it to the conical flask (5.2).   // 6.3.   // Determination   //  // Using the 250 ml measuring cylinder (5.6), add 200 ml of freshly boiled and cooled water, previously heated to 60 °C. Stopper the flask, mix by swirling and place in the water bath at 60 °C (5.8) for 30 minutes. Shake the flask at intervals of about 10 minutes.   //   // Filter, and cool the filtrate to about 20 °C. The filtrate must be clear.   //   // Transfer 100 ml of the cooled filtrate into the conical flask (5.5), using the pipette (5.3). Add 0,5 ml of the phenolphtalein indicator solution (4.2), using the pipette (5.4). Titrate with the standard volumetric sodium hydroxide solution (4.1), until the appearance of a faint pink colour, persisting for at least 30 seconds. Determine and record the volume used to the nearest 0,01 ml.   // 7.   // EXPRESSION OF RESULTS   // 7.1.  // Formula and method of calculation   //   // The titratable acidity of the acid casein is given by:  1.2.3 //   //   // 20 × V × T m  1.2 //   // where:  1.2.3 //   // V   // is the volume, in millilitres, of the standard volumetric sodium hydroxide solution (4.1) used;   //   // T   // is the strength of the standard volumetric sodium hydroxide solution (4.1) in mol/l;   //   // m   // is the mass, in grams, of the test portion.  1.2 //   // Calculate the titratable acidity to two decimal places.   // 7.2.   // Repeatability   //   // The difference in results between two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,02 ml of 0,1 mol/l sodium hydroxide per 1 gram of product.  //   // This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.  METHOD 4  DETERMINATION OF ASH  (including P2O5)  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // The method determines the ash (including P2O5) content of:   //  // - acid caseins   // 2.   // DEFINITION   //   // The ash (including P2O5) content: the content of ash as determined by the method specified.   // 3.   // PRINCIPLE   //   // A portion of the sample is incinerated at 825 °C ± 25 °C in the presence of magnesium acetate to bind all phosphorus of organic origin. The final ash is calculated after the weighing of the residue and subtraction of the mass of ash originating from the magnesium acetate.   // 4.   // REAGENTS   // 4.1.  // Magnesium acetate tetrahydrate solution, 120 g/l. Dissolve 120 grams of magnesium acetate tetrahydrate [Mg (CH3 CO2)2 4 H2 O] in water and make up one litre with water.   // 5.  // APPARATUS   // 5.1.   // Analytical balance   // 5.2.  // One-mark pipette, 5 ml.   // 5.3.   // Silica or platinum dishes, about 70 mm diameter and 25 to 50 mm deep.   // 5.4.  // Drying oven, capable of being controlled at 102 °C ± 1 °C.  // 5.5.   // Electrical furnace, capable of being controlled at 825 °C ± 25 °C.   // 5.6.   // Boiling water bath  // 5.7.   // Desiccator containing freshly activated silica gel with a water content indicator or an equivalent desiccant.  // 6.   // PROCEDURE   // 6.1.   // Preparation of the test sample   //   // As described in Section 1.2 of the General Provisions.   // 6.2.   // Preparation of the dishes   //  // Heat two dishes (A,B) (5.3) in the electrical furnace (5.5), controlled at 825 °C ± 25 °C, for 30 minutes. Allow the dishes to cool somewhat and then place in the desiccator (5.7) to the temperature of the balance room and weigh to the nearest 0,1 mg.   // 6.3.   // Test portion   //   // Weigh, to the nearest 0,1 mg approximately 3 grams of the test sample (6.1), directly into one of the prepared dishes (A).   // 6.4.  // Determination   //   // Using the pipette (5.2), add to the dish (A) exactly 5 ml of the magnesium acetate solution (4.1) so as to wet all of the test portion, and allow to stand for 20 minutes.   //   // To the other prepared dish (B), add with the pipette (5.2) exactly 5 ml of the magnesium acetate solution (4.1).   //   // Evaporate the contents of both dishes (A and B) to dryness on the boiling water bath (5.6).   //   // Place both dishes in the oven (5.4), controlled at 102 °C ± 1 °C, for 30 minutes.   //   // Heat dish A with its contents on a low flame, a hot plate or under an I/R lamp, until the test portion is completely charred, taking care that it does not burst into flame.   //   // Transfer both dishes (A and B) to the electrical furnace (5.5), controlled at 825 °C ± 25 °C, and heat for at least one hour until all carbon has disappeared from dish A. Allow both dishes to cool somewhat and then place in the desiccator (5.7) to the temperature of the balance room and weigh to the nearest 0,1 mg.   //   // Repeat the operations of heating for approximately 30 minutes, in the electrical furnace (5.5), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass.   // 7.   // EXPRESSION OF RESULTS   // 7.1.  // Method of calculation   //   // The content of ash, including P2O5, in the sample, as a percentage by mass, is given by:  1.2.3.4 //   //   // (m1 - m2) - (m3 - m4) m0   // × 100  1.2 //   // where:   //   // m0 is the mass, in grams, of the test portion;   //   // m1 is the mass, in grams, of dish A and residue;   //   // m2 is the mass, in grams, of the prepared dish A;   //   // m3 is the mass, in grams, of dish B and residue;   //   // m4 is the mass, in grams, of the prepared dish B.   //   // Calculate the final result to the nearest 0,01 %.   // 7.2.   // Repeatability   //   // The difference in results between the determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,1 grams per 100 grams of product.   //   // The repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.  METHOD 5  DETERMINATION OF ASH  (including P2O5)  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method determines the ash (including P2O5) content of:   //  // - rennet casein   // 2.   // DEFINITION   //   // The ash (including P2O5) content: the content of ash as determined by the method specified.   // 3.   // PRINCIPLE   //   // A portion of the sample is incinerated at 825 °C ± 25 °C to constant mass. The residue is determined by weighing and calculated as a percentage by mass of the sample.   // 4.  // APPARATUS   // 4.1.   // Analytical balance   // 4.2.  // Silica or platinum dish, about 70 mm diameter and 25 to 50 mm deep.   // 4.3.   // Electrical furnace with air circulation, capable of being controlled at 825 °C ± 25 °C.  // 4.4.   // Desiccator, containing freshly activated silica gel with a water content indicator or an equivalent desiccant.  // 5.   // PROCEDURE   // 5.1.   // Preparation of the test sample   //   // As described in Section 1.2 of the General Provisions.   // 5.2.   // Preparation of the dish   //  // Heat the dish (4.2) in the electrical furnace (4.3), controlled at 825 °C ± 25 °C, for 30 minutes. Allow the dish to cool somewhat and then place in the desiccator (4.4) to the temperature of the balance room and weigh to the nearest 0,1 mg.   // 5.3.   // Test portion   //   // Weigh, to the nearest 0,1 mg approximately 3 grams of the test sample (5.1) directly into the prepared dish.   // 5.4.   // Determination   //  // Heat the dish with its contents on a low flame, a hot plate or an I/R lamp until the test portion is completely charred, taking care that it does not burst into flame.   //  // Transfer the dish to the electrical furnace (4.3), controlled at 825 °C ± 25 °C, and heat for at least one hour until all carbon has disappeared from the dish. Allow the dish to cool somewhat and then place in the desiccator (4.4) to the temperature of the balance room and weigh to the nearest 0,1 mg.   //   // Repeat the operations of heating for approximately 30 minutes, in the electrical furnace (4.3), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass.   // 6.  // EXPRESSION OF RESULTS   // 6.1.   // Method of calculation and formula   //   // The ash content of the sample, including P2O5, as a percentage per mass, is given by:  1.2.3.4 //   //  // m1 - m2 m0   // × 100 1.2 //  // where:   //   // m0 is the mass, in grams, of the test portion;   //   // m1 is the mass, in grams, of the dish and residue;   //   // m2 is the mass, in grams, of the prepared dish.   //   // Calculate the final result to the nearest 0,01 %.   // 6.2.   // Repeatability   //   // The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,15 grams of ash per 100 grams of product.   //  // This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.  METHOD 6  DETERMINATION OF pH  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method determines the pH of:   //   // - caseinates.   // 2.  // DEFINITION   //   // The pH of caseinates: the pH, at 20 °C, of an aqueous solution of caseinates, as determined by the method specified.   // 3.   // PRINCIPLE   //   // The electrometric determination of pH of an aqueous solution of caseinate, using a pH meter.   // 4.   // REAGENTS   //  // Any water used in the preparation of the reagents or in the Procedure (6) shall be recently distilled water that has been protected from carbon dioxide absorption.   // 4.1.   // Buffer solutions, for calibration of the pH meter (5.2)   //   // Two standard buffer solutions with pH values at 20 °C which are known to the second decimal place and will bracket the pH value of the sample under test, for example phtalate buffer solution of pH approximately 4 and a borax buffer solution of pH approximately 9.   // 5.   // APPARATUS   // 5.1.   // Balance, accuracy 0,1 grams.   // 5.2.   // pH meter, minimum sensitivity 0,05 pH unit, with a suitably calibrated elecrode, e.g. glass electrode and a calomel or other reference electrode.   // 5.3.   // Thermometer, accuracy 0,5 °C.  // 5.4.   // Conical flask, capacity 100 ml, fitted with a ground glass stopper.   // 5.5.   // Beaker, capacity 50 ml.  // 5.6.   // Mixer   // 5.7.   // Beaker, for the mixer (5.6) of at least 250 ml capacity.   // 6.   // PROCEDURE   // 6.1.  // Preparation of the test sample   //   // As described in Section 1.2 of the General Provisions.  // 6.2.   // Determination   // 6.2.1.   // Calibration of pH meter   //   // Adjust the temperature of the buffer solutions (4.1) to 20 °C and calibrate the pH meter in accordance with the manufacturer's instructions.   //   // NOTES   //   // 1. The calibration should be carried out while the flasks are standing for 20 mintues (see 6.2.2).   //   // 2. If a series of samples is being tested, check the calibration of the pH meter with one or more of the standard buffer solutions at least every 30 minutes.   // 6.2.2.   // Preparation of the test solution   //   // Transfer to the beaker (5.7) 95 ml of water, add 5,0 grams of the test sample (6.1), and mix using the mixer (5.6) for 30 seconds.   //   // Allow to stand for 20 minutes at about 20 °C, covered with a watch glass.   // 6.2.3.   // Measurement of pH   // 6.2.3.1.   // Pour about 20 ml of the solution into the beaker (5.5) and immediately determine the pH of this liquid, using the pH meter (5.2) after having rinsed the glass electrode carefully with water.   // 6.2.3.2.  // Measure the pH.   // 7.   // EXPRESSION OF RESULTS  // 7.1.   // Recording of pH   //   // Record, as the pH of the aqueous solution of caseinate, the value read from the dial of the pH meter to at least two decimal places.   // 7.2.  // Repeatability   //   // The difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,05 pH unit.   //   // This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out.6.5.1 .  TRANSFER TO THE FLASK A FEW PIECES OF PORCELAIN OR A FEW GLASS BEADS ( 5.10.1 ) AND ABOUT 10 GRAMS OF THE ANHYDROUS POTASSIUM SULPHATE ( 4.2 ).   //  ADD 0,2 G OF THE COPPER ( II ) SULPHATE ( 4.3 ) AND WASH DOWN THE NECK OF THE FLASK WITH A LITTLE WATER . ADD 20 ML OF THE CONCENTRATED SULPHURIC ACID ( 4.1 ). MIX THE CONTENTS OF THE FLASK .   //  HEAT GENTLY ON THE DIGESTION APPARATUS ( 5.3 ) UNTIL ANY FROTHING HAS CEASED, BOIL GENTLY UNTIL THE SOLUTION IS CLEAR AND A PALE GREEN-BLUE COLOUR PERSISTS . DURING HEATING, SWIRL THE FLASK OCCASIONALLY .   //  CONTINUE THE BOILING, REGULATING THE HEATING SO AS TO CONDENSE THE VAPOURS IN THE MIDDLE OF THE FLASK NECK . CONTINUE THE HEATING FOR 90 MINUTES AVOIDING LOCAL OVERHEATING .   //  ALLOW TO COOL TO ROOM TEMPERATURE . CAREFULLY ADD ABOUT 200 ML OF WATER AND A FEW PIECES OF PUMICE ( 5.10.2 ). MIX AND COOL AGAIN .  6.5.2 .  TRANSFER INTO THE CONICAL FLASK ( 5.7 ) 50 ML OF THE BORIC ACID SOLUTION ( 4.5 ) AND FOUR DROPS OF THE INDICATOR ( 4.8 ). MIX . PLACE THE CONICAL FLASK UNDER THE CONDENSER ( 5.4 ) SO THAT THE TIP OF THE OUTLET TUBE ( 5.5 ) IS IMMERSED IN THE BORIC ACID SOLUTION . USING A GRADUATED CYLINDER ( 5.8 ), ADD TO THE KJELDAHL FLASK 80 ML OF THE SODIUM HYDROXIDE SOLUTION ( 4.6 ). DURING THIS OPERATION, HOLD THE FLASK IN AN INCLINED POSITION SO THAT THE SODIUM HYDROXIDE SOLUTION RUNS DOWN THE SIDE OF THE FLASK TO FORM A BOTTOM LAYER .   //  IMMEDIATELY CONNECT THE KJELDAHL FLASK TO THE CONDENSER BY MEANS OF THE SPLASH-HEAD ( 5.6 ).   //  GENTLY ROTATE THE KJELDAHL FLASK TO MIX ITS CONTENTS . BOIL GENTLY AT FIRST, AVOIDING ANY FROTHING . CONTINUE THE DISTILLATION SO THAT 150 ML OF DISTILLATE ARE COLLECTED IN APPROXIMATELY 30 MINUTES . THE DISTILLATE SHOULD HAVE A TEMPERATURE BELOW 25 *C . ABOUT TWO MINUTES BEFORE THE END OF THE DISTILLATION, LOWER THE CONICAL FLASK SO THAT THE TIP OF THE OUTLET TUBE IS NO LONGER IMMERSED IN THE ACID SOLUTION, AND RINSE THE TIP WITH A LITTLE WATER . STOP HEATING, REMOVE THE OUTLET TUBE AND RINSE ITS OUTER AND INNER WALLS WITH A LITTLE WATER, COLLECTING THE WASHINGS IN THE CONICAL FLASK .  6.5.3 .  TITRATE THE DISTILLATE IN THE CONICAL FLASK, USING THE STANDARD VOLUMETRIC HYDROCHLORIC ACID SOLUTION ( 4.7 ).  7 .  EXPRESSION OF RESULTS  7.1 .  FORMULA AND METHOD OF CALCULATION   //  THE PROTEIN CONTENT OF THE SAMPLE, EXPRESSED AS A PERCENTAGE BY MASS, IS GIVEN BY :  1.2.3.4.5 //  //  ( V1 - V2 ) X T X 14 X 100 X 6,38 M X 1 000  =  8,932 ( V1 - V2 ) X T M  1.2WHERE :   //  //  1.2.3 //  V1  IS THE VOLUME, IN MILLILITRES, OF THE STANDARD VOLUMETRIC HYDROCHLORIC ACID SOLUTION ( 4.7 ) USED IN THE DETERMINATION ( 6.5 );   //  V2  IS THE VOLUME, IN MILLILITRES, OF THE STANDARD VOLUMETRIC HYDROCHLORIC ACID SOLUTION ( 4.7 ) USED IN THE BLANK TEST ( 6.3 );  //  T  IS THE STRENGTH OF THE STANDARD VOLUMETRIC HYDROCHLORIC ACID SOLUTION ( 4.7 ) IN MOL/L;   //  M  IS THE MASS, IN GRAMS, OF THE TEST PORTION .  1.2 //  CALCULATE THE PROTEIN CONTENT TO THE NEAREST 0,1 %.  7.2 .  REPEATABILITY   //  THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS CARRIED OUT SIMULTANEOUSLY OR IN RAPID SUCCESSION ON THE SAME SAMPLE, BY THE SAME ANALYST UNDER THE SAME CONDITIONS SHALL NOT EXCEED 0,5 GRAMS OF PROTEIN PER 100 GRAMS OF PRODUCT .   //  THIS REPEATABILITY INTERVAL SHOULD BE ACHIEVED IN 95 % OF THE TIMES THAT THE METHOD IS CORRECTLY CARRIED OUT .  METHOD 3  DETERMINATION OF TITRATABLE ACIDITY  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THE METHOD DETERMINES THE TITRATABLE ACIDITY OF :   //  - ACID CASEINS .  2 .  DEFINITION   //  THE TITRATABLE ACIDITY OF ACID CASEINS : THE VOLUME IN MILLILITRES, OF A 0,1 MOL/L STANDARD SODIUM HYDROXIDE SOLUTION REQUIRED TO NEUTRALIZE AN AQUEOUS EXTRACT OF 1 GRAM OF THE PRODUCT .  3 .  PRINCIPLE   //  AN AQUEOUS EXTRACT OF THE SAMPLE AT 60 *C IS OBTAINED AND FILTERED . THE FILTRATE IS TITRATED AGAINST STANDARD SODIUM HYDROXIDE USING PHENOLPHTALEIN INDICATOR .  4 .  REAGENTS   //  ANY WATER USED IN THE METHOD PROCEDURE OR IN THE PREPARATION OF REAGENTS SHALL BE FREED FROM CARBON DIOXIDE BY BOILING FOR 10 MINUTES BEFORE USE .  4.1 .  SODIUM HYDROXIDE SOLUTION : 0,1 MOL/L .  4.2 .  PHENOLPHTALEIN INDICATOR SOLUTION, 10 G/L IN ETHANOL ( 95 % V/V ) NEUTRALIZED TO THE INDICATOR .  5 .  APPARATUS  5.1 .  ANALYTICAL BALANCE  5.2 .  CONICAL FLASK, 500 ML CAPACITY, WITH GROUND NECK AND FITTED WITH A GROUND GLASS STOPPER .  5.3 .  ONE-MARK PIPETTE, 100 ML CAPACITY .  5.4 .  PIPETTE, SUITABLE FOR MEASURING 0,5 ML OF INDICATOR SOLUTION ( 4.2 ).  5.5 .  CONICAL FLASK, 250 ML CAPACITY .  5.6 .  MEASURING CYLINDER, 250 ML CAPACITY .  5.7 .  BURETTE, GRADUATED IN 0,1 ML .  5.8 .  WATER BATH, CAPABLE OF BEING CONTROLLED AT A TEMPERATURE OF 60 *C  +/-  2 *C .  5.9 .  APPROPRIATE FILTER  6 .  PROCEDURE  6.1 .  PREPARATION OF THE TEST SAMPLE   //  AS DESCRIBED IN SECTION 1.2 OF THE GENERAL PROVISIONS .  6.2 .  TEST PORTION   //  WEIGH ABOUT 10 GRAMS OF THE TEST SAMPLE ( 6.1 ) TO THE NEAREST 10 MG AND TRANSFER IT TO THE CONICAL FLASK ( 5.2 ).  6.3 .  DETERMINATION   //  USING THE 250 ML MEASURING CYLINDER ( 5.6 ), ADD 200 ML OF FRESHLY BOILED AND COOLED WATER, PREVIOUSLY HEATED TO 60 *C . STOPPER THE FLASK, MIX BY SWIRLING AND PLACE IN THE WATER BATH AT 60 *C ( 5.8 ) FOR 30 MINUTES . SHAKE THE FLASK AT INTERVALS OF ABOUT 10 MINUTES .   //  FILTER, AND COOL THE FILTRATE TO ABOUT 20 *C . THE FILTRATE MUST BE CLEAR .   //  TRANSFER 100 ML OF THE COOLED FILTRATE INTO THE CONICAL FLASK ( 5.5 ), USING THE PIPETTE ( 5.3 ). ADD 0,5 ML OF THE PHENOLPHTALEIN INDICATOR SOLUTION ( 4.2 ), USING THE PIPETTE ( 5.4 ). TITRATE WITH THE STANDARD VOLUMETRIC SODIUM HYDROXIDE SOLUTION ( 4.1 ), UNTIL THE APPEARANCE OF A FAINT PINK COLOUR, PERSISTING FOR AT LEAST 30 SECONDS . DETERMINE AND RECORD THE VOLUME USED TO THE NEAREST 0,01 ML .  7 .  EXPRESSION OF RESULTS  7.1 .  FORMULA AND METHOD OF CALCULATION   //  THE TITRATABLE ACIDITY OF THE ACID CASEIN IS GIVEN BY :  1.2.3 //  //  20 X V X T M  1.2 //  WHERE :  1.2.3 //  V  IS THE VOLUME, IN MILLILITRES, OF THE STANDARD VOLUMETRIC SODIUM HYDROXIDE SOLUTION ( 4.1 ) USED;   //  T  IS THE STRENGTH OF THE STANDARD VOLUMETRIC SODIUM HYDROXIDE SOLUTION ( 4.1 ) IN MOL/L;   //  M  IS THE MASS, IN GRAMS, OF THE TEST PORTION .  1.2 //  CALCULATE THE TITRATABLE ACIDITY TO TWO DECIMAL PLACES .  7.2 .  REPEATABILITY   //  THE DIFFERENCE IN RESULTS BETWEEN TWO DETERMINATIONS CARRIED OUT SIMULTANEOUSLY OR IN RAPID SUCCESSION ON THE SAME SAMPLE, BY THE SAME ANALYST, UNDER THE SAME CONDITIONS, SHALL NOT EXCEED 0,02 ML OF 0,1 MOL/L SODIUM HYDROXIDE PER 1 GRAM OF PRODUCT .   //  THIS REPEATABILITY INTERVAL SHOULD BE ACHIEVED IN 95 % OF THE TIMES THAT THE METHOD IS CORRECTLY CARRIED OUT .  METHOD 4  DETERMINATION OF ASH  ( INCLUDING P2O5 )  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THE METHOD DETERMINES THE ASH ( INCLUDING P2O5 ) CONTENT OF :  //  - ACID CASEINS  2 .  DEFINITION   //  THE ASH ( INCLUDING P2O5 ) CONTENT : THE CONTENT OF ASH AS DETERMINED BY THE METHOD SPECIFIED .  3 .  PRINCIPLE   //  A PORTION OF THE SAMPLE IS INCINERATED AT 825 *C  +/-  25 *C IN THE PRESENCE OF MAGNESIUM ACETATE TO BIND ALL PHOSPHORUS OF ORGANIC ORIGIN . THE FINAL ASH IS CALCULATED AFTER THE WEIGHING OF THE RESIDUE AND SUBTRACTION OF THE MASS OF ASH ORIGINATING FROM THE MAGNESIUM ACETATE .  4 .  REAGENTS  4.1 .  MAGNESIUM ACETATE TETRAHYDRATE SOLUTION, 120 G/L . DISSOLVE 120 GRAMS OF MAGNESIUM ACETATE TETRAHYDRATE ( MG ( CH3 CO2)2 4 H2 O ) IN WATER AND MAKE UP ONE LITRE WITH WATER .  5 .  APPARATUS  5.1 .  ANALYTICAL BALANCE  5.2 .  ONE-MARK PIPETTE, 5 ML .  5.3 .  SILICA OR PLATINUM DISHES, ABOUT 70 MM DIAMETER AND 25 TO 50 MM DEEP .  5.4 .  DRYING OVEN, CAPABLE OF BEING CONTROLLED AT 102 *C  +/-  1 *C .  5.5 .  ELECTRICAL FURNACE, CAPABLE OF BEING CONTROLLED AT 825 *C  +/-  25 *C .  5.6 .  BOILING WATER BATH  5.7 .  DESICCATOR CONTAINING FRESHLY ACTIVATED SILICA GEL WITH A WATER CONTENT INDICATOR OR AN EQUIVALENT DESICCANT .  6 .  PROCEDURE  6.1 .  PREPARATION OF THE TEST SAMPLE   //  AS DESCRIBED IN SECTION 1.2 OF THE GENERAL PROVISIONS .  6.2 .  PREPARATION OF THE DISHES   //  HEAT TWO DISHES ( A,B ) ( 5.3 ) IN THE ELECTRICAL FURNACE ( 5.5 ), CONTROLLED AT 825 *C  +/-  25 *C, FOR 30 MINUTES . ALLOW THE DISHES TO COOL SOMEWHAT AND THEN PLACE IN THE DESICCATOR ( 5.7 ) TO THE TEMPERATURE OF THE BALANCE ROOM AND WEIGH TO THE NEAREST 0,1 MG .  6.3 .  TEST PORTION   //  WEIGH, TO THE NEAREST 0,1 MG APPROXIMATELY 3 GRAMS OF THE TEST SAMPLE ( 6.1 ), DIRECTLY INTO ONE OF THE PREPARED DISHES ( A ).  6.4 .  DETERMINATION   //  USING THE PIPETTE ( 5.2 ), ADD TO THE DISH ( A ) EXACTLY 5 ML OF THE MAGNESIUM ACETATE SOLUTION ( 4.1 ) SO AS TO WET ALL OF THE TEST PORTION, AND ALLOW TO STAND FOR 20 MINUTES .   //  TO THE OTHER PREPARED DISH ( B ), ADD WITH THE PIPETTE ( 5.2 ) EXACTLY 5 ML OF THE MAGNESIUM ACETATE SOLUTION ( 4.1 ).   //  EVAPORATE THE CONTENTS OF BOTH DISHES ( A AND B ) TO DRYNESS ON THE BOILING WATER BATH ( 5.6 ).   //  PLACE BOTH DISHES IN THE OVEN ( 5.4 ), CONTROLLED AT 102 *C  +/-  1 *C, FOR 30 MINUTES .   //  HEAT DISH A WITH ITS CONTENTS ON A LOW FLAME, A HOT PLATE OR UNDER AN I/R LAMP, UNTIL THE TEST PORTION IS COMPLETELY CHARRED, TAKING CARE THAT IT DOES NOT BURST INTO FLAME .   //  TRANSFER BOTH DISHES ( A AND B ) TO THE ELECTRICAL FURNACE ( 5.5 ), CONTROLLED AT 825 *C  +/-  25 *C, AND HEAT FOR AT LEAST ONE HOUR UNTIL ALL CARBON HAS DISAPPEARED FROM DISH A . ALLOW BOTH DISHES TO COOL SOMEWHAT AND THEN PLACE IN THE DESICCATOR ( 5.7 ) TO THE TEMPERATURE OF THE BALANCE ROOM AND WEIGH TO THE NEAREST 0,1 MG .   //  REPEAT THE OPERATIONS OF HEATING FOR APPROXIMATELY 30 MINUTES, IN THE ELECTRICAL FURNACE ( 5.5 ), COOLING AND WEIGHING, UNTIL THE MASS REMAINS CONSTANT TO WITHIN 1 MG OR BEGINS TO INCREASE . RECORD THE MINIMUM MASS .  7 .  EXPRESSION OF RESULTS  7.1 .  METHOD OF CALCULATION   //  THE CONTENT OF ASH, INCLUDING P2O5, IN THE SAMPLE, AS A PERCENTAGE BY MASS, IS GIVEN BY :  1.2.3.4 //  //  ( M1 - M2 ) - ( M3 - M4 ) M0  X 100  1.2 //  WHERE :   //  M0 IS THE MASS, IN GRAMS, OF THE TEST PORTION;   //  M1 IS THE MASS, IN GRAMS, OF DISH A AND RESIDUE;   //  M2 IS THE MASS, IN GRAMS, OF THE PREPARED DISH A;   //  M3 IS THE MASS, IN GRAMS, OF DISH B AND RESIDUE;   //  M4 IS THE MASS, IN GRAMS, OF THE PREPARED DISH B .   //  CALCULATE THE FINAL RESULT TO THE NEAREST 0,01 %.  7.2 .  REPEATABILITY   //  THE DIFFERENCE IN RESULTS BETWEEN THE DETERMINATIONS CARRIED OUT SIMULTANEOUSLY OR IN RAPID SUCCESSION ON THE SAME SAMPLE, BY THE SAME ANALYST, UNDER THE SAME CONDITIONS, SHALL NOT EXCEED 0,1 GRAMS PER 100 GRAMS OF PRODUCT .   //  THE REPEATABILITY INTERVAL SHOULD BE ACHIEVED IN 95 % OF THE TIMES THAT THE METHOD IS CORRECTLY CARRIED OUT .  METHOD 5  DETERMINATION OF ASH  ( INCLUDING P2O5 )  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THIS METHOD DETERMINES THE ASH ( INCLUDING P2O5 ) CONTENT OF :  //  - RENNET CASEIN  2 .  DEFINITION   //  THE ASH ( INCLUDING P2O5 ) CONTENT : THE CONTENT OF ASH AS DETERMINED BY THE METHOD SPECIFIED .  3 .  PRINCIPLE   //  A PORTION OF THE SAMPLE IS INCINERATED AT 825 *C  +/-  25 *C TO CONSTANT MASS . THE RESIDUE IS DETERMINED BY WEIGHING AND CALCULATED AS A PERCENTAGE BY MASS OF THE SAMPLE .  4 .  APPARATUS  4.1 .  ANALYTICAL BALANCE  4.2 .  SILICA OR PLATINUM DISH, ABOUT 70 MM DIAMETER AND 25 TO 50 MM DEEP .  4.3 .  ELECTRICAL FURNACE WITH AIR CIRCULATION, CAPABLE OF BEING CONTROLLED AT 825 *C  +/-  25 *C .  4.4 .  DESICCATOR, CONTAINING FRESHLY ACTIVATED SILICA GEL WITH A WATER CONTENT INDICATOR OR AN EQUIVALENT DESICCANT .  5 .  PROCEDURE  5.1 .  PREPARATION OF THE TEST SAMPLE   //  AS DESCRIBED IN SECTION 1.2 OF THE GENERAL PROVISIONS .  5.2 .  PREPARATION OF THE DISH   //  HEAT THE DISH ( 4.2 ) IN THE ELECTRICAL FURNACE ( 4.3 ), CONTROLLED AT 825 *C  +/-  25 *C, FOR 30 MINUTES . ALLOW THE DISH TO COOL SOMEWHAT AND THEN PLACE IN THE DESICCATOR ( 4.4 ) TO THE TEMPERATURE OF THE BALANCE ROOM AND WEIGH TO THE NEAREST 0,1 MG .  5.3 .  TEST PORTION   //  WEIGH, TO THE NEAREST 0,1 MG APPROXIMATELY 3 GRAMS OF THE TEST SAMPLE ( 5.1 ) DIRECTLY INTO THE PREPARED DISH .  5.4 .  DETERMINATION   //  HEAT THE DISH WITH ITS CONTENTS ON A LOW FLAME, A HOT PLATE OR AN I/R LAMP UNTIL THE TEST PORTION IS COMPLETELY CHARRED, TAKING CARE THAT IT DOES NOT BURST INTO FLAME .   //  TRANSFER THE DISH TO THE ELECTRICAL FURNACE ( 4.3 ), CONTROLLED AT 825 *C  +/-  25 *C, AND HEAT FOR AT LEAST ONE HOUR UNTIL ALL CARBON HAS DISAPPEARED FROM THE DISH . ALLOW THE DISH TO COOL SOMEWHAT AND THEN PLACE IN THE DESICCATOR ( 4.4 ) TO THE TEMPERATURE OF THE BALANCE ROOM AND WEIGH TO THE NEAREST 0,1 MG .   //  REPEAT THE OPERATIONS OF HEATING FOR APPROXIMATELY 30 MINUTES, IN THE ELECTRICAL FURNACE ( 4.3 ), COOLING AND WEIGHING, UNTIL THE MASS REMAINS CONSTANT TO WITHIN 1 MG OR BEGINS TO INCREASE . RECORD THE MINIMUM MASS .  6 .  EXPRESSION OF RESULTS  6.1 .  METHOD OF CALCULATION AND FORMULA   //  THE ASH CONTENT OF THE SAMPLE, INCLUDING P2O5, AS A PERCENTAGE PER MASS, IS GIVEN BY :  1.2.3.4 //  //  M1 - M2 M0  X 100  1.2WHERE :   //  M0 IS THE MASS, IN GRAMS, OF THE TEST PORTION;   //  M1 IS THE MASS, IN GRAMS, OF THE DISH AND RESIDUE;   //  M2 IS THE MASS, IN GRAMS, OF THE PREPARED DISH .   //  CALCULATE THE FINAL RESULT TO THE NEAREST 0,01 %.  6.2 .  REPEATABILITY   //  THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS CARRIED OUT SIMULTANEOUSLY OR IN RAPID SUCCESSION ON THE SAME SAMPLE, BY THE SAME ANALYST, UNDER THE SAME CONDITIONS, SHALL NOT EXCEED 0,15 GRAMS OF ASH PER 100 GRAMS OF PRODUCT .   //  THIS REPEATABILITY INTERVAL SHOULD BE ACHIEVED IN 95 % OF THE TIMES THAT THE METHOD IS CORRECTLY CARRIED OUT .  METHOD 6  DETERMINATION OF PH  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THIS METHOD DETERMINES THE PH OF :   //  - CASEINATES .  2 .  DEFINITION   //  THE PH OF CASEINATES : THE PH, AT 20 *C, OF AN AQUEOUS SOLUTION OF CASEINATES, AS DETERMINED BY THE METHOD SPECIFIED .  3 .  PRINCIPLE   //  THE ELECTROMETRIC DETERMINATION OF PH OF AN AQUEOUS SOLUTION OF CASEINATE, USING A PH METER .4 .  REAGENTS   //  ANY WATER USED IN THE PREPARATION OF THE REAGENTS OR IN THE PROCEDURE ( 6 ) SHALL BE RECENTLY DISTILLED WATER THAT HAS BEEN PROTECTED FROM CARBON DIOXIDE ABSORPTION .  4.1 .  BUFFER SOLUTIONS, FOR CALIBRATION OF THE PH METER ( 5.2 )   //  TWO STANDARD BUFFER SOLUTIONS WITH PH VALUES AT 20 *C WHICH ARE KNOWN TO THE SECOND DECIMAL PLACE AND WILL BRACKET THE PH VALUE OF THE SAMPLE UNDER TEST, FOR EXAMPLE PHTALATE BUFFER SOLUTION OF PH APPROXIMATELY 4 AND A BORAX BUFFER SOLUTION OF PH APPROXIMATELY 9 .  5 .  APPARATUS  5.1 .  BALANCE, ACCURACY 0,1 GRAMS .  5.2 .  PH METER, MINIMUM SENSITIVITY 0,05 PH UNIT, WITH A SUITABLY CALIBRATED ELECRODE, E.G . GLASS ELECTRODE AND A CALOMEL OR OTHER REFERENCE ELECTRODE .  5.3 .  THERMOMETER, ACCURACY 0,5 *C .  5.4 .  CONICAL FLASK, CAPACITY 100 ML, FITTED WITH A GROUND GLASS STOPPER .  5.5 .  BEAKER, CAPACITY 50 ML .  5.6 .  MIXER  5.7 .  BEAKER, FOR THE MIXER ( 5.6 ) OF AT LEAST 250 ML CAPACITY .  6 .  PROCEDURE  6.1 .  PREPARATION OF THE TEST SAMPLE   //  AS DESCRIBED IN SECTION 1.2 OF THE GENERAL PROVISIONS .  6.2 .  DETERMINATION  6.2.1 .  CALIBRATION OF PH METER   //  ADJUST THE TEMPERATURE OF THE BUFFER SOLUTIONS ( 4.1 ) TO 20 *C AND CALIBRATE THE PH METER IN ACCORDANCE WITH THE MANUFACTURER'S INSTRUCTIONS .   //  NOTES   //  1 . THE CALIBRATION SHOULD BE CARRIED OUT WHILE THE FLASKS ARE STANDING FOR 20 MINTUES ( SEE 6.2.2 ).   //  2 . IF A SERIES OF SAMPLES IS BEING TESTED, CHECK THE CALIBRATION OF THE PH METER WITH ONE OR MORE OF THE STANDARD BUFFER SOLUTIONS AT LEAST EVERY 30 MINUTES .  6.2.2 .  PREPARATION OF THE TEST SOLUTION   //  TRANSFER TO THE BEAKER ( 5.7 ) 95 ML OF WATER, ADD 5,0 GRAMS OF THE TEST SAMPLE ( 6.1 ), AND MIX USING THE MIXER ( 5.6 ) FOR 30 SECONDS .   //  ALLOW TO STAND FOR 20 MINUTES AT ABOUT 20 *C, COVERED WITH A WATCH GLASS .  6.2.3 .  MEASUREMENT OF PH  6.2.3.1 .  POUR ABOUT 20 ML OF THE SOLUTION INTO THE BEAKER ( 5.5 ) AND IMMEDIATELY DETERMINE THE PH OF THIS LIQUID, USING THE PH METER ( 5.2 ) AFTER HAVING RINSED THE GLASS ELECTRODE CAREFULLY WITH WATER .  6.2.3.2 .  MEASURE THE PH .  7 .  EXPRESSION OF RESULTS  7.1 .  RECORDING OF PH   //  RECORD, AS THE PH OF THE AQUEOUS SOLUTION OF CASEINATE, THE VALUE READ FROM THE DIAL OF THE PH METER TO AT LEAST TWO DECIMAL PLACES .  7.2 .  REPEATABILITY   //  THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS CARRIED OUT SIMULTANEOUSLY OR IN RAPID SUCCESSION ON THE SAME SAMPLE, BY THE SAME ANALYST, UNDER THE SAME CONDITIONS, SHALL NOT EXCEED 0,05 PH UNIT .   //  THIS REPEATABILITY INTERVAL SHOULD BE ACHIEVED IN 95 % OF THE TIMES THAT THE METHOD IS CORRECTLY CARRIED OUT .