title: Council Directive 2007/61/EC of 26 September 2007 amending Directive 2001/114/EC relating to certain partly or wholly dehydrated preserved milk for human consumption

text:
               4.10.2007

               EN

               Official Journal of the European Union

               L 258/27

      COUNCIL DIRECTIVE 2007/61/EC
   of 26 September 2007
   amending Directive 2001/114/EC relating to certain partly or wholly dehydrated preserved milk for human consumption
   THE COUNCIL OF THE EUROPEAN UNION,
   Having regard to the Treaty establishing the European Community, and in particular Article 37 thereof,
   Having regard to the proposal from the Commission,
   Having regard to the opinion of the European Parliament (1),
   Whereas:

               (1)

               In view of the growing need for harmonisation in the international trade in milk and milk products, provision should be made to allow the standardisation of the protein content of certain partly or wholly dehydrated preserved milk to a minimum content of 34 %, by weight, expressed on fat-free dry matter.

               (2)

               While allowing standardisation, it is necessary to define raw materials as well as the composition of raw materials used for protein adjustment.

               (3)

               Regulation (EC) No 1925/2006 of the European Parliament and of the Council of 20 December 2006 on the addition of vitamins and minerals and of certain other substances to foods (2) aims at regulating the addition of such substances to food and establishes the list of vitamins and minerals that may be added to food. Council Directive 2001/114/EC (3) should therefore be amended to allow the addition of vitamins and minerals as provided for by Regulation (EC) No 1925/2006.

               (4)

               Directive 2001/114/EC should be amended accordingly,

         HAS ADOPTED THIS DIRECTIVE:
   Article 1
   Directive 2001/114/EC is hereby amended as follows:

               1.

               Article 2 shall be deleted.

               2.

               Annexe I shall be amended in accordance with the Annex to this Directive.

         Article 2
   1.   Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive by 31 August 2008. They shall forthwith communicate to the Commission the text of such laws, regulations and administrative provisions together with a table showing the correlation between them and this Directive.
   When they are adopted by Member States, these measures shall contain a reference to this Directive or shall be accompanied by such a reference on the occasion of their official publication. The methods for making such reference shall be laid down by the Member States.
   2.   Member States shall communicate to the Commission the text of the main provisions of national law which they adopt in the field covered by this Directive.
   Article 3
   This Directive shall enter into force on the third day following its publication in the Official Journal of the European Union.
   Article 4
   This Directive is addressed to the Member States.

      Done at Brussels, 26 September 2007.

            For the Council

            The President

         J. SILVA

      (1)  Opinion of 5 September 2007 (not yet published in the Official Journal).

      (2)  OJ L 404, 30.12.2006, p. 26.

      (3)  OJ L 15, 17.1.2002, p. 19. Directive as amended by the 2003 Act of Accession.

      ANNEX
      Annex I to Directive 2001/114/EC is hereby amended as follows:

                  1.

                  In point 1 ‘Partly dehydrated milk’, the first subparagraph shall be replaced by the following:
                  ‘This means the liquid product, whether or not sweetened, obtained by the partial removal of water from milk, from wholly or partly skimmed milk or from a mixture of these products, which may have an admixture of cream or of wholly dehydrated milk or both, the addition of wholly dehydrated milk not to exceed, in the finished products, 25 % of total milk solids.’.

                  2.

                  In point 2 ‘Totally dehydrated milk’, the first subparagraph shall be replaced by the following:
                  ‘This means the solid product, where the water content does not exceed 5 % by weight of the finished product, obtained by the removal of water from milk, from wholly or partly skimmed milk, from cream or from a mixture of these products.’.

                  3.

                  Point 3 ‘Treatments’ shall be amended as follows:

                              (a)

                              In point (b), the introductory words shall be replaced by the following:
                              ‘Without prejudice to Regulation (EC) No 853/2004 of the European Parliament and of the Council of 29 April 2004 laying down specific hygiene rules for food of animal origin (1), the preservation of the products referred to in paragraphs 1 and 2 shall be achieved:

                              (b)

                              The following point shall be added:

                                          ‘(c)

                                          Without prejudice to the compositional requirements of points 1 and 2 of this Annex the protein content of milk may be adjusted to a minimum content of 34 % by weight (expressed on fat free dry matter), by the addition and/or withdrawal of milk constituents in such a way as not to alter the whey protein to casein ratio of the milk being adjusted.’.

                  4.

                  Point 4 ‘Authorised additions’ shall be replaced by the following:
                  ‘4.   Authorised additions and raw materials

                              (a)

                              Vitamins and minerals in accordance with Regulation (EC) No 1925/2006 of the European Parliament and of the Council of 20 of December 2006, on the addition of vitamins and minerals and of certain other substances to foods (2).

                              (b)

                              Authorised raw materials for protein adjustment purposes referred to in point 3(c) shall be as follows:

                                          (i)

                                          Milk retentate
                                          Milk retentate is the product obtained by concentrating milk protein by ultra filtration of milk, partly skimmed milk, or skimmed milk;

                                          (ii)

                                          Milk permeate
                                          Milk permeate is the product obtained by removing milk proteins and milk fat from milk, partly skimmed milk, or skimmed milk by ultra filtration; and

                                          (iii)

                                          Lactose
                                          Lactose is a natural constituent of milk normally obtained from whey with an anhydrous lactose content of not less than 99,0 % m/m on a dry basis. It may be anhydrous or contain one molecule of water of crystallisation or be a mixture of both forms.

         (1)  OJ L 139, 30.4.2004, p. 55. Corrected by OJ L 226, 25.6.2004, p. 22.’

         (2)  OJ L 404, 30.12.2006, p. 26.’.


title: Commission Directive 2005/26/EC of 21 March 2005 establishing a list of food ingredients or substances provisionally excluded from Annex IIIa of Directive 2000/13/EC of the European Parliament and of the CouncilText with EEA relevance

text:
               22.3.2005

               EN

               Official Journal of the European Union

               L 75/33

      COMMISSION DIRECTIVE 2005/26/EC
   of 21 March 2005
   establishing a list of food ingredients or substances provisionally excluded from Annex IIIa of Directive 2000/13/EC of the European Parliament and of the Council
   (Text with EEA relevance)
   THE COMMISSION OF THE EUROPEAN COMMUNITIES,
   Having regard to the Treaty establishing the European Community,
   Having regard to Directive 2000/13/EC of the European Parliament and of the Council of 20 March 2000 on the approximation of the laws of the Member States relating to the labelling, presentation and advertising of foodstuffs (1), and in particular second subparagraph of Article 6(11) thereof,
   Whereas:

               (1)

               Annex IIIa of Directive 2000/13/EC establishes a list of food ingredients to be indicated on the label as they are likely to cause adverse reactions in susceptible individuals.

               (2)

               In accordance with Directive 2000/13/EC the Commission may provisionally exclude certain ingredients or products of those ingredients from Annex IIIa to that Directive, while food manufacturers or their associations conduct scientific studies to establish that those ingredients or products comply with the conditions for definite exclusion from that Annex.

               (3)

               The Commission received 27 applications regarding 34 ingredients or products thereof, of which 32 fall within the scope of this Directive, and have been submitted to the European Food Safety Authority (EFSA) for a scientific opinion.

               (4)

               Based on the information provided by the applicant, and other information available, the EFSA has considered that certain products of ingredients are not likely, or not very likely, to cause adverse reactions in susceptible individuals. In certain cases, EFSA has concluded that it cannot draw a firm conclusion, though no reported cases were mentioned.

               (5)

               Those products or ingredients complying with these conditions should therefore provisionally be excluded from Annex IIIa of Directive 2000/13/EC,

         HAS ADOPTED THIS DIRECTIVE:
   Article 1
   The ingredients or substances listed in the Annex to this Directive shall be excluded from Annex IIIa of Directive 2000/13/EC until 25 November 2007.
   Article 2
   1.   Member States shall adopt and publish, by 21 September 2005 at the latest, the laws, regulations and administrative provisions necessary to comply with this Directive. They shall forthwith communicate to the Commission the text of those provisions and a correlation table between those provisions and this Directive.
   They shall apply those provisions from 25 November 2005.
   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 text of the main provisions of national law which they adopt in the field covered by this Directive.
   Article 3
   This Directive shall enter into force on the day following that of its publication in the Official Journal of the European Union.
   Article 4
   This Directive is addressed to the Member States.

      Done at Brussels, 21 March 2005.

            For the Commission

         Markos KYPRIANOU

            Member of the Commission

      (1)  OJ L 109, 6.5.2000, p. 29. Directive as last amended by Directive 2003/89/EC (OJ L 308, 25.11.2003, p. 15).

      ANNEX
      List of food ingredients and substances provisionally excluded from Annex IIIa of Directive 2000/13/EC

                  Ingredients

                  Products thereof provisionally excluded

                  Cereals containing gluten

                              —

                              Wheat based glucose syrups including dextrose (1)

                              —

                              Wheat based maltodextrins (1)

                              —

                              Glucose syrups based on barley

                              —

                              Cereals used in distillates for spirits

                  Eggs

                              —

                              Lysozym (produced from egg) used in wine

                              —

                              Albumin (produced from egg) used as fining agent in wine and cider

                  Fish

                              —

                              Fish gelatine used as carrier for vitamins and flavours

                              —

                              Fish gelatine or Isinglass used as fining agent in beer, cider and wine

                  Soybean

                              —

                              Fully refined soybean oil and fat (1)

                              —

                              Natural mixed tocopherols (E306), natural D-alpha tocopherol, natural D-alpha tocopherol acetate, natural D-alpha tocopherol succinate from soybean sources

                              —

                              Vegetable oils derived phytosterols and phytosterol esters from soybean sources

                              —

                              Plant stanol ester produced from vegetable oil sterols from soybean sources

                  Milk

                              —

                              Whey used in distillates for spirits

                              —

                              Lactitol

                              —

                              Milk (casein) products used as fining agents in cider and wines

                  Nuts

                              —

                              Nuts used in distillates for spirits

                              —

                              Nuts (almonds, walnuts) used (as flavour) in spirits

                  Celery

                              —

                              Celery leaf and seed oil

                              —

                              Celery seed oleoresin

                  Mustard

                              —

                              Mustard oil

                              —

                              Mustard seed oil

                              —

                              Mustard seed oleoresin

         (1)  And products thereof, in so far as the process that they have undergone is not likely to increase the level of allergenicity assessed by the EFSA for the relevant product from which they originated.


Avis juridique important

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31996L0087

Commission Directive 96/87/EC of 13 December 1996 adapting to technical progress Council Directive 96/49/EC on the approximation of the laws of the Member States with regard to the transport of dangerous goods by rail (Text with EEA relevance)

Official Journal L 335 , 24/12/1996 P. 0045 - 0045

COMMISSION DIRECTIVE 96/87/EC of 13 December 1996 adapting to technical progress Council Directive 96/49/EC on the approximation of the laws of the Member States with regard to the transport of dangerous goods by rail (Text with EEA relevance)THE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Community,Having regard to Council Directive 96/49/EC of 23 July 1996 on the approximation of the laws of the Member States with regard to the transport of dangerous goods by rail (1), and in particular Article 8 thereof,Whereas the Regulations concerning the international carriage of dangerous goods by rail, usually known as the RID, as amended, should be attached to Directive 96/49/EC as an Annex and be applicable not only to cross-frontier transport, but also to transport within the individual Member States;Whereas the Annex to Directive 96/49/EC contains the RID as applicable from 1 January 1995;Whereas the RID is updated every two years and therefore an amended version will be in force as from 1 January 1997;Whereas in accordance with Article 8, all the necessary modifications for adapting to technical and scientific progress in the field covered by the Directive and aiming at aligning it to the new rules have to be adopted in accordance with the procedure set out in Article 9;Whereas it is necessary to adapt the sector to the new RID rules and therefore to amend the Annex to Directive 96/49/EC;Whereas the measures provided for in the Directive are in accordance with the opinion of the Committee provided by Article 9 of Directive 96/49/EC,HAS ADOPTED THIS DIRECTIVE:Article 1 The Annex to Directive 96/49/EC is modified as follows:'The Annex comprises the provisions of the Regulations concerning the international carriage of dangerous goods by rail (RID), appearing as Annex I to Appendix B to Cotif, as applicable with effect from 1 January 1997, on the understanding that "Contracting Party" and "the States or the railways" will be replaced by "Member State".NB: Versions of the RID in all the official languages of the Community will be published as soon as a text is ready in all languages.`Article 2 1. The Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive before 1 January 1997. They shall forthwith inform the Commission thereof.When the Member States adopt these measures they shall contain a reference to this Directive or shall be accompanied by such reference on the occasion of their official publication. The methods of making such reference shall be laid down 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 governed by this Directive.Article 3 This Directive shall enter into force on the day following that of its publication in the Official Journal of the European Communities.Article 4 This Directive is addressed to the Member States.Done at Brussels, 13 December 1996.For the CommissionNeil KINNOCKMember of the Commission(1) OJ No L 235, 17. 9. 1996, p. 25.


Avis juridique important

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31985L0490

Fourth Commission Directive 85/490/EEC of 11 October 1985 on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products

Official Journal L 295 , 07/11/1985 P. 0030 - 0045 Finnish special edition: Chapter 13 Volume 14 P. 0192  Spanish special edition: Chapter 15 Volume 6 P. 0115  Swedish special edition: Chapter 13 Volume 14 P. 0192  Portuguese special edition Chapter 15 Volume 6 P. 0115

*****FOURTH  COMMISSION DIRECTIVE  of 11 October 1985  on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products  (85/490/EEC)  THE COMMISSION OF THE EUROPEAN  COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community,  Having regard to Council Directive 76/768/EEC of 27 July 1976 on the approximation of the laws of the Member States relating to cosmetic products (1), as last amended by Directive 85/391/EEC (2), and in particular Article 8 (1) thereof,  Whereas Directive 76/768/EEC provides for the official testing of cosmetic products with the aim of ensuring that the conditions laid down by Community provisions concerning the composition of cosmetic products are satisfied;  Whereas all the necessary methods of analysis should be laid down as quickly as possible; whereas three steps towards the attainment of this objective having already been taken through the definition of certain methods in Commission Directive 80/1335/EEC (3), 82/434/EEC (4) and 83/514/EEC (5), the fourth step is to consist in the definition of methods for the identification and determination of glycerol 1-(4-aminobenzoate), the determination of chlorobutanol, the identification and determination of quinine, the identification and determination of inorganic sulphites and hydrogen sulphites, the identification and determination of chlorates of the alkali metals and the identification and determination of sodium iodate;  Whereas the measures provided for in this Directive are in accordance with the opinion of the Committee on the Adaptation of Directive 76/768/EEC to Technical Progress,  HAS ADOPTED THIS DIRECTIVE:  Article 1  Member States shall take all necessary steps to ensure that during official testing of cosmetic products:  - identification and determination of glycerol 1-(4aminobenzoate),  - determination of chlorobutanol,  - identification and determination of quinine,  - identification and determination of inorganic sulphites and hydrogen sulphites,  - identification and determination of chlorates of the alkali metals, and  - identification and determination of sodium iodate  are performed in accordance with the methods described in the Annex.  Article 2  Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive not later than 31 December 1986.  They shall forthwith inform the Commission thereof.  Article 3  This Directive is addressed to the Member States.  Done at Brussels, 11 October 1985.  For the Commission  Stanley CLINTON-DAVIS  Member of the Commission  (1) OJ No L 262, 27. 9. 1976, p. 169.  (2) OJ No L 224, 22. 8. 1985, p. 40.  (3) OJ No L 383, 31. 12. 1980, p. 27.  (4) OJ No L 185, 30. 6. 1982, p. 1.  (5) OJ No L 291, 24. 10. 1983, p. 9.  ANNEX  IDENTIFICATION AND DETERMINATION OF GLYCEROL 1-(4-AMINOBENZOATE)  A. IDENTIFICATION  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method will detect alpha-monoglyceryl 4-aminobenzoate (glycerol 1-(4-aminobenzoate). It will also detect ethyl 4-aminobenzoate (benzocaine INN) which may be present as an impurity.   // 2.  // PRINCIPLE   //   // This identification is done by thin layer chromatography on silica gel with a fluorescent indicator and detection of the free primary amine group by formation of a diazo dye on the plate.   // 3.   // REAGENTS   //   // All reagents should be of analytical purity.   // 3.1.   // Solvent mixture: cyclohexane/propan-2-ol/stabilized dichloromethane 48/64/9 (v/v/v).   // 3.2.   // Development solvent: petroleum ether (40-60)/benzene/acetone/ammonium hydroxide solution (minimum 25 % NH3): 35/35/35/1 (v/v/v/v).   // 3.3.  // Developing solution: (a) sodium nitrite: 1 g in 100 ml of 1 M hydrochloric acid (prepared immediately before use); (b) 2-naphthol: 0,2 g in 100 ml of 1 M potassium hydroxide.  // 3.4.   // Standard solutions:   //   // alpha-monoglyceryl 4-aminobenzoate: 0,05 g in 100 ml of mixed solvent 3.1;   //  // ethyl 4-aminobenzoate: 0,05 g in 100 ml of mixed solvent 3.1.   // 3.5.   // Silica gel 60 F254 plates, 0,25 mm thick, 200 mm × 200 mm.   // 4.   // APPARATUS   // 4.1.   // Normal apparatus for thin layer chromatography.   // 4.2.  // Ultrasonic vibrator.   // 4.3.   // Millipore filter FH 0,5 mm or equivalent.   // 5.   // PROCEDURE   // 5.1.   // Sample preparation   //   // Weigh 1,5 g of the product to be analyzed in a 10 ml stoppered graduated flask. Make up to the mark with the solvent 3.1. Stopper and leave for one hour at room temperature in an ultrasonic vibrator (4.2). Filter through a Millipore filter (4.3) and use the filtrate for chromatography.   // 5.2.   // Thin layer chromatography   //   // Deposit 10 m l of sample solution (5.1) and of each standard solution (3.4) on the plate (3.5).   //   // Develop the chromatogram to a height of 150 mm in a tank previously saturated with solvent 3.2. Allow the plate to dry at ambient temperature.   // 5.3.  // Development   // 5.3.1.   // Observe the plate under 254 nm UV light.   // 5.3.2.   // Spray the completely dried plate with the solution 3.3 (a).   //   // Allow to dry at room temperature for 1 minute and immediately spray with the solution 3.3 (b).   //   // Dry the plate in an oven at 60 °C. The spots appear an orange colour. Alpha-monoglyceryl 4-aminobenzoate: RF 0,07; ethyl 4-aminobenzoate: RF 0,55.  B. DETERMINATION  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method determines alpha monoglyceryl 4-aminobenzoate. It will also determine ethyl 4-aminobenzoate. It cannot determine more than 5 % (m/m) of alpha monoglyceryl 4-aminobenzoate and 1 % (m/m) of ethyl 4-aminobenzoate.   // 2.   // DEFINITION   //  // The alpha monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents measured by this method are expressed as percentage by mass (% m/m) of the product.   // 3.  // PRINCIPLE   //   // The product to be analyzed is suspended in methanol and after appropriate treatment of the sample it is determined by high-performance liquid chromatography (HPLC).  // 4.   // REAGENTS   //   // All reagents should be of analytical purity and should be suitable for HPLC where appropriate.   // 4.1.   // Methanol.   // 4.2.   // Potassium dihydrogenorthophosphate (KH2PO4).   // 4.3.   // Zinc di(acetate) (Zn(CH3COO)2 ; 2H2O).   // 4.4.   // Acetic acid (d 20  4 = 1,05).   // 4.5.   // Tetrapotassium hexacyanoferrate, (K4 (Fe(CN)6) ; 3H2O).   // 4.6.   // Ethyl 4-hydroxybenzoate.  // 4.7.   // Alpha monoglyceryl 4-aminobenzoate.   // 4.8.  // Ethyl 4-aminobenzoate.   // 4.9.   // Phosphate buffer solution (0,02 M): dissolve 2,72 g of potassium dihydrogenorthophosphate (4.2) in one litre of water.  // 4.10.   // Eluant: phosphate buffer solution (4.9)/methanol (4.1) 61/39(v/v)   //   // The composition of the mobile phase may be changed in order to achieve a resolution factor R  1,5. 1.2.3.4 //   //   // R = 2   // d'R2 - d'R1 W1 + W2   //  // where   //   //  1.2.3 //   // R1 and R2   // = retention times, in minutes, of the peaks,   //   // W1 and W2   // = peak widths at half height, in milimetres,   //   // d'   // = the chart speed, in millimetres per minute.  1.2 // 4.11.  // Stock solution of alpha-monoglyceryl 4-aminobenzoate: weigh accurately about 40 mg of alpha-monoglyceryl 4-aminobenzoate and introduce it into a 100 ml graduated flask. Dissolve in 40 ml of methanol (4.1). Make up to the mark with buffer solution (4.9) and mix.   // 4.12.   // Stock solution of ethyl 4-aminobenzoate: weigh accurately about 40 mg of ethyl 4-aminobenzoate and introduce it into a 100 ml graduated flask. Dissolve in 40 ml of methanol (4.1). Make up to the mark with the buffer solution (4.9) and mix.   // 4.13.   // Internal standard solution: weigh accurately about 50 mg of ethyl 4-hydroxybenzoate (4.6), transfer to a 100 ml standard flask, dissolve in 40 ml of methanol (4.1), make up to the mark with the buffer solution (4.9) and mix.   // 4.14.   // Standard solutions: prepare four standard solutions by dissolving in 100 ml eluant (4.10) according to the following table: 1.2,3.4,5.6,7 //    //   //   //   // Standard solution  // Alpha-monoglyceryl 4-aminobenzoate  // Ethyl 4-aminobenzoate  // Ethyl 4-hydroxybenzoate  //  //  // 1.2.3.4.5.6.7 //  // (mg/ml) (*)   // ml (4.11)  // (mg/ml) (*)   // ml (4.12)   // (mg/ml) (*)   // ml (4.13)  //    //   //   //   //   //   //   // I   // 8   // 2   // 8  // 2   // 50   // 10   // II   // 16   // 4   // 12   // 3  // 50   // 10   // III   // 24   // 6   // 16   // 4   // 50  // 10   // IV   // 40   // 10   // 20   // 5   // 50   // 10  //    //   //   //   //   //   //  1.2 //   // (*) These values are given as an indication and correspond to the exact masses of 4.11, 4.12 and 4.13.   //   // NB: These solutions may be prepared in a different way.   //    //  // 4.15   // Carrez I solution: dissolve 26,5 g of tetrapotassium hexacyanoferrate (4.5) in water and make up to 250 ml.   // 4.16.   // Carrez II solution: dissolve 54,9 g of zinc di(acetate) (4.3) and 7,5 ml of acetic acid (4.4) in water and make up to 250 ml.   // 4.17.   // Merck Lichrosorb RP-18, or equivalent, with an average particle size of 5 mm.   // 5.  // APPARATUS   // 5.1.   // The usual laboratory equipment.  // 5.2.   // High-performance chromatography equipment with a variable wavelength UV detector and thermostatted chamber set at 45 °C.   // 5.3.   // Stainless-steel column: length: 250 mm; internal diameter: 4,6 mm; packing: Lichrosorb RP - 18 (4.17).   // 5.4.   // Ultrasonic bath.   // 6.   // PROCEDURE  // 6.1.   // Sample preparation   // 6.1.1.   // Weigh accurately about 1 g of sample into a 100 ml beaker and add 10 ml of methanol (4.1).   // 6.1.2.   // Place the beaker in the ultrasonic bath (5.4) for 20 minutes to produce a suspension. Transfer the suspension thus obtained quantitatively into a 100 ml standard flask with not more than 75 ml of eluant (4.10).  //   // Add in succession 1 ml of Carrez I solution (4.15) and 1 ml of Carrez II solution (4.16) and mix after each addition. Make up to the mark with eluant (4.10), re-mix and filter through a pleated filter paper.   // 6.1.3.   // With a pipette, transfer 3,0 ml of the filtrate obtained in 6.1.2 and 5,0 ml of the internal standard solution (4.13) into a 50 ml standard flask. Make up to the mark with eluant (4.10) and mix. Use the solution thus obtained for carrying out the chromatography analysis described in 6.2.   // 6.2.  // Chromatography   // 6.2.1.   // Adjust the flow rate of the mobile phase (4.10) to 1,2 ml/min and set the column temperature to 45 °C.   // 6.2.2.   // Set the detector (5.2) to 274 nm.   // 6.2.3.   // With a microsyringe, inject at least two times 20 ml of solution (6.1.3) into the chromatograph and measure the areas of the peaks.   // 6.3.  // Calibration curve   // 6.3.1.   // Inject 20 ml of each of the standard solutions (4.14) and measure the peak area.  // 6.3.2.   // For each concentration calculate the ratio between the peak areas of alpha-monoglyceryl 4-aminobenzoate and the peak areas of the internal standard. Plot this ratio on the abscissa and on the ordinate the ratio of the corresponding masses.   // 6.3.3.   // Proceed in the same manner for ethyl 4-hydroxybenzoate.   // 7.   // CALCULATION   // 7.1.   // From the calibration curve obtained in 6.3 read off the mass ratios (RP1, RP2) corresponding to the ratios between the areas of the peaks calculated in 6.2.3 where   //   // RP1 = mass of alpha-monoglyceryl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate, RP2 = mass of ethyl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate.  // 7.2.   // From the mass ratios obtained in this way calculate the alpha-monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents, as mass percentages (% m/m) with the formulae:   //   // Rp % (m/m) alpha-monoglyceryl 4-aminobenzoate = RP1 × q  6 p   //   // Rp % (m/m) ethyl 4-aminobenzoate = RP2 × q  6 p   //   // q = quantity of ethyl 4-hydroxybenzoate (internal standard) weighed, in milligrams, in 4.12, p = quantity of sample, in grams, weighed in 6.1.1.  // 8.   // REPEATABILITY (1)   // 8.1.   // For a 5 % (m/m) content of alpha-monoglyceryl 4-aminobenzoate, the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,25 %.   // 8.2.   // For a 1 % (m/m) content of ethyl 4-aminobenzoate the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,10 %.   // 9.   // NOTES  // 9.1.   // Before carrying out an analysis, check whether the sample contains substances likely to overlap with the peak of the internal standard (ethyl 4-aminobenzoate) on the chromatogram.   // 9.2.   // In order to check the absence of any interference, repeat the determination by changing the proportion of methanol in the mobile phase by 10 % relative.  DETERMINATION OF CHLOROBUTANOL  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method is suitable for the determination of chlorobutanol (INN) up to a maximum concentration of 0,5 % (m/m) in any cosmetic product, except aerosols.   // 2.   // DEFINITION   //   // The content of chlorobutanol measured by this method is expressed as percentage by mass (% m/m) of product.   // 3.  // PRINCIPLE   //   // After appropriate treatment of the product to be analyzed the determination is done by gas chromatography using 2,2,2-trichloroethanol as the internal standard.   // 4.   // REAGENTS   //   // All the reagents should be of analytical purity.   // 4.1.   // Chlorobutanol (1,1,1-trichloro-2-methylpropan-2-ol).   // 4.2.  // 2,2,2-Trichloroethanol.   // 4.3.   // Absolute ethanol.  // 4.4.   // Standard solution of chlorobutanol: 0,025 g in 100 ml ethanol (4.3) (m/v).   // 4.5.   // Standard solution of 2,2,2-trichloroethanol: 4 mg in 100 ml ethanol (4.3) (m/v).  // 5.   // APPARATUS   // 5.1.   // Normal laboratory equipment.   // 5.2.   // Gas chromatograph with electron detector, Ni 63.   // 6.   // PROCEDURE   // 6.1.  // Preparation of sample   //   // Weigh accurately between 0,1 and 0,3 g (p g) of the sample. Place in 100 ml volumetric flask. Dissolve it in ethanol (4.3), add 1 ml of the internal standard solution (4.5) and make up to the mark with ethanol  (1) ISO 5725.   // 6.2.   // Gas chromatography conditions   // 6.2.1.  // The operating conditions must yield a resolution factor R 1,5.  1.2.3.4 //   //   // R = 2   // d'R2 - d'R1 W1 + W2   //  // Where   //   //  1.2.3 //   // R1 and R2   // = retention times, in minutes, of the peaks,   //   // W1 and W2   // = peak widths at half height, in millimetres,   //   // d'   // = the chart speed, in millimetres per minute.  1.2 // 6.2.2.  // As examples, the following operating conditions provide the required resolution:  1.2.3 //    //   //   // Column  // I  // II  //  //  //  // Material   // Glass   // Stainless steel   // Length   // 1,80 m   // 3 m   // Diameter   // 3 mm   // 3 mm   // Stationary phase   // 10 % Carbowax 20 M TPA on Gaschrom Q 80-100 mesh   // 5 % OV 17 on Chromosorb WAW DMCS 80-100 mesh   // Conditioning   // 2 to 3 days at 190 °C   //  // Temperature:   //   //   // - injector   // 200 °C   // 150 °C   // - column   // 150 °C   // 100 °C   // - detector  // 200 °C   // 150 °C   // Carrier gas   // Nitrogen  // Argon/methane (95/5 v/v)   // Flowrate   // 35 ml/min  // 35 ml/min   //    //   //  1.2 // 6.3.   // Standard curve  //   // Using five 100 ml volumetric flasks, add 1 ml of the standard solution (4.5) and 0,2, 0,3, 0,4, 0,5, and 0,6 ml of solution 4.4 respectively, and make up to the mark with ethanol (4.3) and mix. Inject 1 ml of each of these solutions into the chromatograph in accordance with the operating conditions described in 6.2.2 and construct a calibration curve by plotting as the abscissa the ratio of the mass of chlorobutanol to that of 2,2,2-trichloroethanol and as the ordinate the ratio of the corresponding peak areas.   // 6.4.   // Inject 1 ml of solution obtained in 6.1 and proceed according to the conditions described in 6.2.2   // 7.   // CALCULATION  // 7.1.   // Calculate from the standard curve (6.3) the quantity 'a' expressed as mg of chlorobutanol, in the solution 6.1.   // 7.2.   // The content of chlorobutanol in the sample is calculated according to the formula:  1.2.3.4.5.6 //   //  // % chlorobutanol (m/m) =   // a × 102 p × 106   // =   // a p × 104  1.2 // 8.   // REPEATABILITY (1)   //   // For a chlorobutanol content of 0,5 % (m/m) the difference between the results of two determinations in parallel carried out on the same sample should not exceed 0,01 %.   //   // Note If the result is equal to or exceeds the maximum permitted concentration it is necessary to check the absence of interferences. (4.3).  (1) ISO 5725.  IDENTIFICATION AND DETERMINATION OF QUININE  A. IDENTIFICATION  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method is intended to detect the presence of quinine in shampoo and hair lotions.   // 2.   // PRINCIPLE   //  // Identification is done by thin layer chromatography on silica gel. Detection of quinine is by the blue fluorescence of quinine in acidic conditions at 360 nm.   //   // For further confirmation, the fluorescence can be eliminated by bromine vapours, and ammonia vapours will cause a yellowish fluorescence to appear.   // 3.   // REAGENTS   //   // All reagents should be of analytical purity.   // 3.1.   // Silica gel plates, without fluorescence indicators, 0,25 mm thick, 200 mm × 200 mm.   // 3.2.   // Developing solvent: toluene / diethyl ether / dichloromethane / diethylamine / 20/20/20/8 (v/v/v/v).   // 3.3.   // Methanol.   // 3.4.   // Sulphuric acid (96 %; d 20  4 = 1,84).   // 3.5.   // Diethyl ether.  // 3.6.   // Developing agent: carefully add 5 ml of sulphuric acid (3.4) to 95 ml of diethyl ether (3.5) in a cooled container.   // 3.7.   // Bromine.   // 3.8.   // Ammonium hydroxide solution (28 %; d 20  4 = 0,90).   // 3.9.  // Quinine, anhydrous.   // 3.10.   // Standard solution: weigh accurately about 100,0 mg of anhydrous quinine (3.9) into a standard flask and dissolve in 100 ml of methanol (3.3).  // 4.   // APPARATUS   // 4.1.   // Normal equipment for thin layer chromatography.   // 4.2.   // Ultrasonic bath.   // 4.3.   // Millipore filter, FH 0,5 m or equivalent with suitable filtration equipment.   // 5.   // PROCEDURE   // 5.1.  // Preparation of the sample   //   // Weigh accurately a quantity of the sample which may contain approximately 100 mg of quinine into a 100 ml standard flask, dissolve and make up to the mark with methanol (3.3).   //   // Stopper the flask and leave for one hour at room temperature in an ultrasonic vibrator (4.2). Filter (4.3) and use the filtrate for the chromatography.   // 5.2.   // Thin layer chromatography   //  // Deposit 1,0 ml of standard solution (3.10) and 1,0 ml of sample solution (5.1) on the silica gel plate (3.1). Develop the chromatogram over a distance of 150 mm using solvent 3.2. in a tank previously saturated with solvent (3.2).   // 5.3.  // Development   // 5.3.1.   // Dry the plate at room temperature.   // 5.3.21.   // Spray with reagent 3.6.  // 5.3.3.   // Leave the plate to dry for one hour at room temperature.   // 5.3.4.   // Observe under the light from a UV lamp adjusted to a wavelength of 360 nm. Quinine appears as a fluorescent intense blue spot.   //   // By way of example the table below gives the values of the RF of the main alkaloids related to quinine when developed with solvent 3.2.  1.2.3 //  //   //   //   // Alkaloid  // RF   //    //   //   //  // Quinine   // 0,20   //   // Quinidine   // 0,29   //  // Cinchonine   // 0,33   //   // Cinchonidine   // 0,27   //  // Hydroquinidine   // 0,17   //    //   // 1.2 // 5.3.5.   // For further confirmation that quinine is present, the plate is exposed for approximately one hour to bromine vapour (3.7). The fluorescence disappears. When the same plate is exposed to ammonia vapour (3.8), the spots reappear with a brown colour, and when the plate is again examined under UV light at 360 nm a yellowish fluorescence can be observed.   //   // Detection limit: 0,1 mg of quinine.  B. DETERMINATION  1.2 // 1.   // SCOPE AND FIELD OF APPLICATION   //   // This method describes the determination of quinine. It may be used to determine the maximum permitted concentration of 0,5 % (m/m) in shampoos and 0,2 % in hair lotions.   // 2.   // DEFINITION  //   // The quinine content determined by this method is expressed as a percentage by mass (% m/m) of the product.  // 3.   // PRINCIPLE   //   // After appropriate treatment of the product to be analyzed the determination is done by high-performance liquid chromatography (HPLC).   // 4.  // REAGENTS   //   // All reagents should be of analytical purity and suitable for HPLC.   // 4.1.   // Acetonitrile.  // 4.2.   // Potassium dihydrogenorthophosphate (KH2PO4).  // 4.3.   // Orthophosphoric acid (85 %; d 20  4 = 1,7).  // 4.4.   // Tetramethylaminium bromide.   // 4.5.  // Quinine, anhydrous.   // 4.6.   // Methanol.   // 4.7.  // Orthophosphoric acid solution (0,1 M): weigh 11,53 g of orthophosphoric acid (4.3) and dissolve in 1 000 nl of water in a graduated flask.   // 4.8.   // Potassium dihyrogenorthophosphate solution (0,1 M): weigh 13,6 g of potassium dihydrogenorthophosphate (4.2) and dissolve in 1 000 ml of water in a graduated flask.   // 4.9.  // Tetramethylammonium bromide solution: dissolve 15,40 g of tetramethylammonium bromide (4.4) in 1 000 ml of water in a graduated flask.   // 4.10   // Eluant: orthophosphoric acid (4.7) / potassium dihydrogenorthophosphate (4.8) / tetramethylammonium bromide (4.9)/water/acetonitrile (4.1) 10/50/100/340/90 (v/v/v/v/v).   //   // The composition of this mobile phase may be changed in order to achieve a resolution factor R  1,5.  1.2.3.4 //   //   // R = 2   // d'R2 - d'R1 W1 + W2   //   // where   //   //  1.2.3 //   // R1 and R2   // = retention times, in minutes, of the peaks,   //   // W1 and W2  // = peak widths at half height, in millimetres,   //   // d'  // = the chart speed, in millimetres per minute.  1.2 // 4.11.   // Silica treated with octadecylsilane, 10 mm.   // 4.12.  // Standard solutions: weigh accurately approximately 5,0, 10,0, 15,0 and 20,0 mg respectively of quinine anhydrous (4.5) into a set of 100 ml standard flasks. Make up to the mark with methanol (4.6) and shake the contents of the flasks until the quinine dissolves. Filter each sample through a 0,5 mm filter.  // 5.   // APPARATUS   // 5.1.   // Usual laboratory equipment.   // 5.2.   // Ultrasonic bath.   // 5.3.  // High-performance liquid chromatography equipment with a variable wavelength detector.   // 5.4.   // Column: length: 250 mm; internal diameter: 4,6 mm; filling: silica (4.11).  // 5.5.   // Millipore filter FH 0,5 mm, or equivalent, with suitable filtration apparatus.  // 6.   // PROCEDURE   // 6.1.   // Sample preparation   //  // Weigh accurately into a 100 ml standard flask a quantity of the product sufficient to contain 10,0 mg of anhydrous quinine, add 20 ml of methanol (4.6) and place the flask in an ultrasonic bath (5.2) for 20 minutes. Make up to the mark with methanol (4.6). Mix the solution and then filter an aliquot (5.5).   // 6.2.   // Chromatography   //   // Flowrate: 1,0 ml/min.   //   // Detector wavelength (5.3) : 332 nm.   //  // Injection volume: 10 ul of filtered solution (6.1).   //  // Measurement: peak area.   // 6.3.   // Calibration curve  //   // Inject at least three times 10,0 ml of each reference solution (4.12), measure the area of the peaks, and calculate the average area at each concentration.   //   // Produce the calibration curve and verify that it is rectilinear.   // 7.  // CALCULATION   // 7.1.   // From the calibration curve (6.3) determine the quantity in mg of anhydrous quinine present in the volume injected (6.2).   // 7.2.   // The concentration of anhydrous quinine in the sample, as a percentage by mass (% m/m), is obtained by the following formula:   //   // % (m/m) of anhydrous quinine = B  A   //   // where   //   // B is the quantity, in micrograms, of anhydrous quinine determined in the 10 microlitres of the filtered solution (6.1).   //   // A is the mass of the sample in grams (6.1).   // 8.  // REPEATABILITY (1)   //   // For an anhydrous quinine content of 0,5 % (m/m), the difference between the results of two determinations performed in parallel on the same sample must not exceed 0,02 %.   //   // For an anhydrous quinine content of 0,2 % (m/m), the difference between the results of two determinations performed in parallel on the same sample must not exceed 0,01 %.  IDENTIFICATION AND DETERMINATION OF INORGANIC SULPHITES AND HYDROGEN SULPHITES  SCOPE AND FIELD OF APPLICATION  The method describes the identification and determination of inorganic sulphites and hydrogen sulphites in cosmetic products. It is only applicable to products that have an aqueous or alcoholic phase and for concentrations up to 0,2 % sulphur dioxide.  A. IDENTIFICATION  1.2 // 1.   // PRINCIPLE   //   // The sample is heated in hydrochloric acid, and sulphur dioxide liberated is identified either by its odour or its effect on an indicator paper.  // 2.   // REAGENTS   //   // All reagents should be of analytical purity.   // 2.1.   // Hydrochloric acid (4 M).  // 2.2.   // Potassium iodate starch paper or other suitable alternative.   // 3.   // APPARATUS   // 3.1.   // Normal laboratory equipment.   // 3.2.   // Flask (25 ml) fitted with a short reflux condenser.   // 4.   // PROCEDURE   // 4.1.  // Place about 2,5 g of sample in the flask (3.2) with 10 ml of hydrochloric acid (2.1).   // 4.2.   // Mix and heat to boiling.   // 4.3.   // Test for the emission of sulphur  (1) ISO 5725.  B. DETERMINATION  1.2 // 1.   // DEFINITION   //   // The sulphite or hydrogen sulphite content of the sample as determined by the method is expressed as percentage by mass of sulphur dioxide.   // 2.  // PRINCIPLE   //   // After acidification of the sample, sulphur dioxide liberated is distilled into a solution of hydrogen peroxide. Sulphuric acid formed is titrated against a standardized sodium hydroxide solution.   // 3.   // REAGENTS  //   // All reagants should be of analytical purity.   // 3.1.   // Hydrogen peroxide 0,2 % (m/v). Prepare daily.   // 3.2.  // Orthophosphoric acid (d 25  4 = 1,75).   // 3.3.  // Methanol.   // 3.4.   // Sodium hydroxide (0,01 M) standardized solution.   // 3.5.   // Nitrogen.   // 3.6.  // Indicator: mixture 1: 1 (v/v) of methyl red (0,03 % m/v in ethanol) and methylene blue (0,05 % m/v in ethanol). Filter the solution.   // 4.   // APPARATUS   // 4.1.   // Normal laboratory equipment.   // 4.2.   // Distillation apparatus (see figure).   // 5.   // PROCEDURE   // 5.1.   // Weigh accurately about 2,5 g of sample into the distillation flask A (see figure).   // 5.2.   // Add 60 ml of water and 50 ml of methanol (3.3) and mix.   // 5.3.   // Place 10 ml of hydrogen peroxide (3.1), 60 ml of water and a few drops of indicator (3.6) in the distillation receiver D (see figure). Add a few drops of sodium hydroxide (3.4) until the indicator turns green.   // 5.4.   // Repeat 5.3 for the wash bottle E (see figure).   // 5.5.   // Assemble the apparatus and adjust the nitrogen (3.5) flow to about 60 bubbles per minute.   // 5.6.  // Run 15 ml of orthophosphoric acid (3.2) from the funnel into the distillation flask A.   // 5.7.   // Heat rapidly to boiling and then simmer gently for a total time of 30 minutes.  // 5.8.   // Detach the distillation receiver D. Rinse the tube and then titrate with sodium hydroxide solution (3.4) until the indicator turns green (3.6).   // 6.   // CALCULATION   //   // Calculate the content of sulphite or hydrogen sulphite by mass in the sample by the expresssion:  1.2.3.4 //  //   // % m/m of sulphur dioxide =   // 3,2 MV m   //  // where   //   //  1.2.3 //   // M   // = molar concentration of sodium hydroxide solution (3.4),   //   // V   // = volume of sodium hydroxide (3.4) required for titration (5.8), in millilitres,   //   // m   // = mass of sample (5.1) in grams. 1.2 // 7.   // REPEATABILITY (1)   //   // For a content of 0,2 % m/m of sulphur dioxide the difference between two parallel determinations done on the same sample should not be greater than 0,006 %. dioxide either by smell or indicator paper (2.2).  (1) ISO 5725.  Sulphurdioxide distillation apparatus according to Tanner  All dimensions in mm IDENTIFICATION AND DETERMINATION OF CHLORATES OF THE ALKALI METALS  SCOPE AND FIELD OF APPLICATION  The method describes the identification and determination of chlorates in toothpastes and other cosmetic products.  A. IDENTIFICATION  1.2 // 1.   // PRINCIPLE   //   // Chlorates are separated from other halates by thin layer chromatography and identified by the oxidation of iodide to form iodine.   // 2.  // REAGENTS   //   // All reagents should be of analytical purity.   // 2.1.   // Reference solutions: aqueous solutions of potassium chlorate, bromate and iodate (0,2 % m/v) prepared freshly.   // 2.2.   // Development solvent: ammonia solution (28 % m/v) acetone/butanol (60/130/30 v/v/v).   // 2.3.  // Potassium iodide, aqueous solution (5 % m/v).   // 2.4.  // Starch solution (1 to 5 % m/v).   // 2.5.   // Hydrochloric acid (1 M).   // 2.6.   // Ready-for-use cellulose thin-layer plates (0,25 mm).   // 3.   // APPARATUS   //   // Normal equipment for thin layer chromatography.   // 4.   // PROCEDURE   // 4.1.   // Extract about 1 g of the sample with water, filter, and dilute to about 25 ml.   // 4.2.   // Deposit 2 ml on the plate (2.6) of the solution (4.1) together with 2 ml aliquots of each of the three reference solutions (2.1).  // 4.3.   // Place the plate in a tank and develop by ascending chromatography about three-quarters of the length of the plate (2.6) with solvent 2.2.   // 4.4.   // Remove from the tank and allow the solvent to evaporate. (NB: This may take up to two hours.)   // 4.5.   // Spray the plate with potassium iodide (2.3) and allow to dry for about five minutes.   // 4.6.   // Spray the plate with starch solution (2.4) and allow to dry for about five minutes.   // 4.7.   // Spray the plate with hydrochloric acid (2.5).   // 5.   // EVALUATION   //   // If the chlorate is present a blue spot (possibly a brown spot) will appear after half an hour with RF value approximately 0,7 to 0,8.  1.2.3 //    //   //   //   // Halates  // RF   //  //   //   //   // Iodate   // 0 to 0,2   //   // Bromate  // 0,5 to 0,6   //   // Chlorate   // 0,7 to 0,8   //    //  //  1.2 //   // It should be noted that bromates and iodates give immediate reaction. Care should be taken not to confuse spots from bromates and chlorates.  B. DETERMINATION  1.2 // 1.   // DEFINITION   //   // The chlorate content of the sample determined by this method is expressed as percentage by mass of chlorate.   // 2.   // PRINCIPLE   //   // Chlorate is reduced by zinc powder under acid conditions. The formed chloride is measured by potentiometric titration using a silver nitrate solution. A similar determination before reduction permits the possible presence of halides.   // 3.   // REAGENTS   //   // All reagents should be of analytical purity.  // 3.1.   // Acetic acid, 80 % (m/m).   // 3.2.   // Zinc powder.   // 3.3.   // Silver nitrate standard solution (0,1 M).   // 4.   // APPARATUS   // 4.1.   // Normal laboratory equipment.   // 4.2.   // Potentiometer equipped with a silver indicator electrode.   // 5.   // PROCEDURE   // 5.1.  // Sample preparation   //   // Weigh accurately a quantity 'm' of approximately 2 g in centrifuge tube. Add about 15 ml acetic acid (3.1) and mix carefully. Wait 30 minutes and centrifuge for 15 minutes at 2 000 rev/min. Transfer the supernatant solution to a 50 ml volumetric flask. Repeat centrifuging twice by adding 15 ml acetic acid (3.1) to the residue. Collect the solution containing chlorate in the same volumetric flask. Fill to the mark with acetic acid (3.1).  // 5.2.   // Reduction of chlorate   //   // Take 20 ml of solution 5.1 and add 0,6 g of zinc powder (3.2). Bring to the boil in a flask fitted with a condenser tube. After 30 minutes boiling, cool and filter. Rinse the flask with water. Filter and combine the filtrate with the rises.   // 5.3.  // Determination of chloride   //   // Titrate 20 ml solution 5.2 with silver nitrate (3.3) by using the potentiometer (4.2). Titrate in the same way 20 ml of solution 5.1 with silver nitrate (3.3).   //   // NB: If the product contains bromine or iodine derivatives which can release bromides or iodides after reduction, the titration curve will have several inflexion points. In this case the volume of the titrated solution (3.3) corresponding to chloride is the difference between the last and the penultimate inflexion points.   // 6.   // CALCULATION  //   // The content of chlorate of the sample (% m/m) is calculated by the formula:  1.2.3.4 //   //   // Chlorate (Clo3 -) % m/m =   // 20,9 (V - V' ) M m   //   // where   //   // 1.2.3 //   // V   // = volume in millilitres, of silver nitrate solution (3.3) used to titrate solution 5.2,   //   // V'  // = volume, in millilitres, of silver nitrate solution (3.3) used to titrate 20 millilitres of solution 5.1,   //   // M  // = molality of silver nitrate standard solution (3.3),   //  // m   // = mass of sample, in grams.  1.2 // 7.  // REPEATABILITY (1)   //   // For a chlorate content of 3 to 5 % m/m the difference between the results of two determinations carried out in parallel on the same sample  (1) ISO 5725.  IDENTIFICATION AND DETERMINATION OF SODIUM IODATE  SCOPE AND FIELD OF APPLICATION  The method describes the procedure for identifying and determining rinse of cosmetic products containing sodium iodate.  A. IDENTIFICATION  1.2 // 1.   // PRINCIPLE   //   // Sodium iodate is separated from other halates by thin layer chromatography and identified by the oxidation of iodide to form iodine.   // 2.  // REAGENTS   //   // All reagents should be of analytical purity.   // 2.1.   // Reference solutions. Aqueous solutions of potassium chlorate, bromate and iodate (0,01 % m/v) prepared freshly.   // 2.2.   // Development solvent.   //   // Ammonia solution (28 % m/v) / acetone / butanol (60/130/30 v/v/v).  // 2.3.   // Potassium iodide aqueous solution (5 % m/v).  // 2.4.   // Starch solution (1 to 5 % m/v).   // 2.5.  // Hydrochloric acid (1 M).   // 3.   // APPARATUS   // 3.1.  // Ready-for-use cellulose thin-layer chromatography (0,25 mm) plates.   // 3.2.   // Normal equipment for thin layer chromatography.   // 4.   // PROCEDURE   // 4.1.   // Extract about 1 g of the sample with water, filter, and dilute to about 10 ml.   // 4.2.   // Deposit 2 ml of this solution onto the base line of the plate (3.1) together with 2 ml aliquots of each of the three reference solutions (2.1).   // 4.3.  // Place the plate in a tank and develop by ascending chromatography about three-quarters of the length of the plate with solvent (2.2).   // 4.4.   // Remove the plate from the tank and allow the solvent to evaporate at ambient temparature (NB: this may take up to two hours).   // 4.5.   // Spray the plate with potassium iodide (2.3) and allow to dry for about five minutes.   // 4.6.   // Spray with starch (2.4) and allow to dry for about five minutes.   // 4.7.   // Finally spray with hydrochloric (2.5).   // 5.   // EVALUATION   //   // If iodate is present a blue spot (the colour may be brown or become brown on standing) will appear immediately with an RF value approximately 0 to 0,2.   //   // It should be noted that bromates give immediate reactions at RF values approximately at 0,5 to 0,6 and chlorates, after about 30 minutes, at RF values of 0,7 to 0,8 respectively.  B. DETERMINATION  1.2 // 1.   // DEFINITION   //   // The sodium iodate content as determined by this method is expressed as a percentage by mass of sodium iodate.   // 2.   // PRINCIPLE   //   // Sodium iodate is dissolved in water and determined by means of high-performance liquid chromatography, using in series, a reverse-phase C18 column and an anion-exchange column.  // 3.   // REAGENTS   //   // All reagents should be of analytical purity and especially suitable for high-performance liquid chromatography (HPLC).   // 3.1.   // Hydrochloric acid (4 M).   // 3.2.   // Sodium sulphite aq, 5 % m/v.   // 3.3.  // Sodium iodate stock solution.   //   // Prepare a stock solution containing 50 mg sodium iodate per 100 ml water.  // 3.4.   // Potassium dihydrogenorthophosphate.   // 3.5.  // Disodium hydrogenorthophosphate ; 2H20.   // 3.6.   // HPLC mobile phase: dissolve 3,88 g potassium dihydrogenorthophosphate (3.4) and 1,19 g disodium hydrogenorthophosphate ; 2H2O (3.5) in 1 litre water.   //  // The pH of the resulting solution is 6.2.   // 3.7.  // Universal indicator paper, pH 1-11.   // 4.   // APPARATUS  // 4.1.   // Ordinary laboratory apparatus.   // 4.2.  // Circular filter paper, diameter 110 mm, Schleicher and Schuell No 575, or equivalent.   // 4.3.   // High-performance liquid chromatograph with a variable wavelength detector.  // 4.4.   // Columns: length: 120 mm; internal diameter: 4,6 mm; number: two connected in series; first column - Necleosil R 5 C18 or equivalent; second column - Vydac TM-301-SB or equivalent.   // 5.   // PROCEDURE   // 5.1.   // Sample preparation   // 5.1.1.   // Fluid samples (shampoos)   //  // Weigh accurately a test portion of approximately 1,0 g sample in a 10 ml glass stoppered calibrated tube or measuring flask.   //   // Fill up to the mark with water and mix.   //  // If necessary, filter the solution.   //   // Determine the iodate in the solution by means of HPLC as described in section 5.2.   // 5.1.2.   // Solid samples (soap)   //   // Finely divide part of the sample and weigh accurately a test portion of approximately 1,0 g into a 100 ml glass stoppered measuring cylinder. Fill up to 50 ml with water and shake vigorously for one minute. Centrifuge and filter through a filter paper (4.1) or allow the mixture to stand for at least one night.   //  // Shake the jellylike solution vigorously and filter it through a filter paper (4.1).   //   // Determine the iodate in the filtrate by means of HPLC as described in section 5.2.  // 5.2.   // Chromatography   //   // Flowrate: 1 ml/min.  //   // Detector wavelength (4.2): 210 nm.   //   // Injection volume: 10 ml.   //   // Measurement: peak area.   // 5.3.  // Calibration   //   // Pipette respectively 1,0, 2,0, 5,0, 10,0 and 20,0 ml of the sodium iodate stock solution (3.3) into 50 ml volumetric flasks. Fill to the mark and mix.   //  // The solutions thus obtained, contain 0,01, 0,02, 0,05, 0,10 and 0,20 mg sodium iodate per ml respectively.   //   // Inject a 10 ml portion of each standard iodate solution into the liquid chromatograph (4.2) and obtain a chromatogram. Determine the peak area for iodate and plot a curve relating the peak area to the sodium iodate concentration.  // 6.   // CALCULATION   //   // Calculate the sodium iodate content, in percentage by mass (% m/m), using the formula: 1.2.3.4 //   //   // % (m/m) of sodium iodate =   // Vc 10 m  //   // where   //   //  1.2.3 //   // m   // is the mass, in grams, of the test portion (5.1),   //   // V   // is the total volume of the sample solution, in millilitres, obtained as described in 5.1,   //   // c   // is the concentration, in milligrams per millilitre of sodium iodate, obtained from the calibration curve (5.3).  1.2 // 7.   // REPEATABILITY (1)  //   // For a sodium iodate content of 0,1 % (m/m) the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,002 %.   // 8.   // CONFIRMATION   // 8.1.   // Principle   //   // In an acidified solution of a cosmetic product, iodate (IO3-) is reduced to iodide (I-) by sulphite and the resulting solution is investigated by means of HPLC. If a peak having a retention time corresponding to the retention time of iodate disappears after treatment with sulphite, the original peak can most probably be attributed to iodate.   // 8.2.   // Procedure  //   // Pipette a 5 ml portion of the sample solution obtained as described in section 5.1 into a conical flask.   //  // Adjust the pH of the solution to a value of 3 or lower with hydrochloric acid (3.1); universal indicator paper (3.7).   //  // Add three drops of sodium sulphite solution (3.2) and mix.  //   // Inject a 10 ml portion of the solution into the liquid chromatograph (4.2).   //   // Compare this chromatogram with the chromatogram obtained as described in paragraph 5 for the same sample. should not exceed 0,07 % m/m.  (1) ISO 5725.3 .  PRINCIPLE   //  AFTER APPROPRIATE TREATMENT OF THE PRODUCT TO BE ANALYZED THE DETERMINATION IS DONE BY GAS CHROMATOGRAPHY USING 2,2,2-TRICHLOROETHANOL AS THE INTERNAL STANDARD .  4 .  REAGENTS   //  ALL THE REAGENTS SHOULD BE OF ANALYTICAL PURITY .  4.1 .  CHLOROBUTANOL ( 1,1,1-TRICHLORO-2-METHYLPROPAN-2-OL ).  4.2 .  2,2,2-TRICHLOROETHANOL .  4.3 .  ABSOLUTE ETHANOL .  4.4 .  STANDARD SOLUTION OF CHLOROBUTANOL : 0,025 G IN 100 ML ETHANOL ( 4.3 ) ( M/V ).  4.5 .  STANDARD SOLUTION OF 2,2,2-TRICHLOROETHANOL : 4 MG IN 100 ML ETHANOL ( 4.3 ) ( M/V ).  5 .  APPARATUS  5.1 .  NORMAL LABORATORY EQUIPMENT .  5.2 .  GAS CHROMATOGRAPH WITH ELECTRON DETECTOR, NI 63 .  6 .  PROCEDURE  6.1 .  PREPARATION OF SAMPLE   //  WEIGH ACCURATELY BETWEEN 0,1 AND 0,3 G ( P G ) OF THE SAMPLE . PLACE IN 100 ML VOLUMETRIC FLASK . DISSOLVE IT IN ETHANOL ( 4.3 ), ADD 1 ML OF THE INTERNAL STANDARD SOLUTION ( 4.5 ) AND MAKE UP TO  ( 1 ) ISO 5725 .  6.2 .  GAS CHROMATOGRAPHY CONDITIONS  6.2.1 .  THE OPERATING CONDITIONS MUST YIELD A RESOLUTION FACTOR R 1,5 .  1.2.3.4 //  //  R = 2  D'R2 - D'R1 W1 + W2   //  WHERE   //  //  1.2.3 //  R1 AND R2  = RETENTION TIMES, IN MINUTES, OF THE PEAKS,   //  W1 AND W2  = PEAK WIDTHS AT HALF HEIGHT, IN MILLIMETRES,   //  D'  = THE CHART SPEED, IN MILLIMETRES PER MINUTE .  1.26.2.2 .  AS EXAMPLES, THE FOLLOWING OPERATING CONDITIONS PROVIDE THE REQUIRED RESOLUTION :  1.2.3 //   //  //  COLUMN  I  II  MATERIAL  GLASS  STAINLESS STEEL  LENGTH  1,80 M  3 M  DIAMETER  3 MM  3 MM  STATIONARY PHASE  10 % CARBOWAX 20 M TPA ON GASCHROM Q 80-100 MESH  5 % OV 17 ON CHROMOSORB WAW DMCS 80-100 MESH  CONDITIONING  2 TO 3 DAYS AT 190 *C   //  TEMPERATURE :   //  //  - INJECTOR  200 *C  150 *C  - COLUMN  150 *C  100 *C  - DETECTOR  200 *C  150 *C  CARRIER GAS  NITROGEN  ARGON/METHANE ( 95/5 V/V )  FLOWRATE  35 ML/MIN  35 ML/MIN   //   //  //  1.26.3 .  STANDARD CURVE   //  USING FIVE 100 ML VOLUMETRIC FLASKS, ADD 1 ML OF THE STANDARD SOLUTION ( 4.5 ) AND 0,2, 0,3, 0,4, 0,5, AND 0,6 ML OF SOLUTION 4.4 RESPECTIVELY, AND MAKE UP TO THE MARK WITH ETHANOL ( 4.3 ) AND MIX . INJECT 1 *L OF EACH OF THESE SOLUTIONS INTO THE CHROMATOGRAPH IN ACCORDANCE WITH THE OPERATING CONDITIONS DESCRIBED IN 6.2.2 AND CONSTRUCT A CALIBRATION CURVE BY PLOTTING AS THE ABSCISSA THE RATIO OF THE MASS OF CHLOROBUTANOL TO THAT OF 2,2,2-TRICHLOROETHANOL AND AS THE ORDINATE THE RATIO OF THE CORRESPONDING PEAK AREAS .  6.4 .  INJECT 1 *L OF SOLUTION OBTAINED IN 6.1 AND PROCEED ACCORDING TO THE CONDITIONS DESCRIBED IN 6.2.2  7 .  CALCULATION  7.1 .  CALCULATE FROM THE STANDARD CURVE ( 6.3 ) THE QUANTITY "A' EXPRESSED AS *G OF CHLOROBUTANOL, IN THE SOLUTION 6.1 .  7.2 .  THE CONTENT OF CHLOROBUTANOL IN THE SAMPLE IS CALCULATED ACCORDING TO THE FORMULA :  1.2.3.4.5.6 //  //  % CHLOROBUTANOL ( M/M   A X 102 P X 106  =  A P X 104  1.28 .  REPEATABILITY ( 1 )   //  FOR A CHLOROBUTANOL CONTENT OF 0,5 % ( M/M ) THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS IN PARALLEL CARRIED OUT ON THE SAME SAMPLE SHOULD NOT EXCEED 0,01 %.   //  NOTE IF THE RESULT IS EQUAL TO OR EXCEEDS THE MAXIMUM PERMITTED CONCENTRATION IT IS NECESSARY TO CHECK THE ABSENCE OF INTERFERENCES . THE MARK WITH ETHANOL ( 4.3 ).  ( 1 ) ISO 5725 .  IDENTIFICATION AND DETERMINATION OF QUININE  A . IDENTIFICATION  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THIS METHOD IS INTENDED TO DETECT THE PRESENCE OF QUININE IN SHAMPOO AND HAIR LOTIONS .  2 .  PRINCIPLE   //  IDENTIFICATION IS DONE BY THIN LAYER CHROMATOGRAPHY ON SILICA GEL . DETECTION OF QUININE IS BY THE BLUE FLUORESCENCE OF QUININE IN ACIDIC CONDITIONS AT 360 NM .   //  FOR FURTHER CONFIRMATION, THE FLUORESCENCE CAN BE ELIMINATED BY BROMINE VAPOURS, AND AMMONIA VAPOURS WILL CAUSE A YELLOWISH FLUORESCENCE TO APPEAR .  3 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY .  3.1 .  SILICA GEL PLATES, WITHOUT FLUORESCENCE INDICATORS, 0,25 MM THICK, 200 MM X 200 MM .  3.2 .  DEVELOPING SOLVENT : TOLUENE / DIETHYL ETHER / DICHLOROMETHANE / DIETHYLAMINE / 20/20/20/8 ( V/V/V/V ).  3.3 .  METHANOL .  3.4 .  SULPHURIC ACID ( 96 %; D 20  4 = 1,84 ).  3.5 .  DIETHYL ETHER .  3.6 .  DEVELOPING AGENT : CAREFULLY ADD 5 ML OF SULPHURIC ACID ( 3.4 ) TO 95 ML OF DIETHYL ETHER ( 3.5 ) IN A COOLED CONTAINER .  3.7 .  BROMINE .  3.8 .  AMMONIUM HYDROXIDE SOLUTION ( 28 %; D 20  4 = 0,90 ).  3.9 .  QUININE, ANHYDROUS .  3.10 .  STANDARD SOLUTION : WEIGH ACCURATELY ABOUT 100,0 MG OF ANHYDROUS QUININE ( 3.9 ) INTO A STANDARD FLASK AND DISSOLVE IN 100 ML OF METHANOL ( 3.3 ).  4 .  APPARATUS  4.1 .  NORMAL EQUIPMENT FOR THIN LAYER CHROMATOGRAPHY .  4.2 .  ULTRASONIC BATH .  4.3 .  MILLIPORE FILTER, FH 0,5 M OR EQUIVALENT WITH SUITABLE FILTRATION EQUIPMENT .  5 .  PROCEDURE  5.1 .  PREPARATION OF THE SAMPLE   //  WEIGH ACCURATELY A QUANTITY OF THE SAMPLE WHICH MAY CONTAIN APPROXIMATELY 100 MG OF QUININE INTO A 100 ML STANDARD FLASK, DISSOLVE AND MAKE UP TO THE MARK WITH METHANOL ( 3.3 ).   //  STOPPER THE FLASK AND LEAVE FOR ONE HOUR AT ROOM TEMPERATURE IN AN ULTRASONIC VIBRATOR ( 4.2 ). FILTER ( 4.3 ) AND USE THE FILTRATE FOR THE CHROMATOGRAPHY .  5.2 .  THIN LAYER CHROMATOGRAPHY   //  DEPOSIT 1,0 *L OF STANDARD SOLUTION ( 3.10 ) AND 1,0 *L OF SAMPLE SOLUTION ( 5.1 ) ON THE SILICA GEL PLATE ( 3.1 ). DEVELOP THE CHROMATOGRAM OVER A DISTANCE OF 150 MM USING SOLVENT 3.2 . IN A TANK PREVIOUSLY SATURATED WITH SOLVENT ( 3.2 ).  5.3 .  DEVELOPMENT  5.3.1 .  DRY THE PLATE AT ROOM TEMPERATURE .  5.3.21 .  SPRAY WITH REAGENT 3.6 .  5.3.3 .  LEAVE THE PLATE TO DRY FOR ONE HOUR AT ROOM TEMPERATURE .  5.3.4 .  OBSERVE UNDER THE LIGHT FROM A UV LAMP ADJUSTED TO A WAVELENGTH OF 360 NM . QUININE APPEARS AS A FLUORESCENT INTENSE BLUE SPOT .   //  BY WAY OF EXAMPLE THE TABLE BELOW GIVES THE VALUES OF THE RF OF THE MAIN ALKALOIDS RELATED TO QUININE WHEN DEVELOPED WITH SOLVENT 3.2 .  1.2.3 //   //  //  //  ALKALOID  RF   //   //  //  //  QUININE  0,20   //  QUINIDINE  0,29   //  CINCHONINE  0,33   //  CINCHONIDINE  0,27   //  HYDROQUINIDINE  0,17   //   //  //  1.25.3.5 .  FOR FURTHER CONFIRMATION THAT QUININE IS PRESENT, THE PLATE IS EXPOSED FOR APPROXIMATELY ONE HOUR TO BROMINE VAPOUR ( 3.7 ). THE FLUORESCENCE DISAPPEARS . WHEN THE SAME PLATE IS EXPOSED TO AMMONIA VAPOUR ( 3.8 ), THE SPOTS REAPPEAR WITH A BROWN COLOUR, AND WHEN THE PLATE IS AGAIN EXAMINED UNDER UV LIGHT AT 360 NM A YELLOWISH FLUORESCENCE CAN BE OBSERVED .   //  DETECTION LIMIT : 0,1 *G OF QUININE .  B . DETERMINATION  1.21 .  SCOPE AND FIELD OF APPLICATION   //  THIS METHOD DESCRIBES THE DETERMINATION OF QUININE . IT MAY BE USED TO DETERMINE THE MAXIMUM PERMITTED CONCENTRATION OF 0,5 % ( M/M ) IN SHAMPOOS AND 0,2 % IN HAIR LOTIONS .  2 .  DEFINITION   //  THE QUININE CONTENT DETERMINED BY THIS METHOD IS EXPRESSED AS A PERCENTAGE BY MASS (% M/M ) OF THE PRODUCT .  3 .  PRINCIPLE   //  AFTER APPROPRIATE TREATMENT OF THE PRODUCT TO BE ANALYZED THE DETERMINATION IS DONE BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ( HPLC ).  4 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY AND SUITABLE FOR HPLC .  4.1 .  ACETONITRILE .  4.2 .  POTASSIUM DIHYDROGENORTHOPHOSPHATE ( KH2PO4 ).  4.3 .  ORTHOPHOSPHORIC ACID ( 85 %; D 20  4 = 1,7 ).  4.4 .  TETRAMETHYLAMINIUM BROMIDE .  4.5 .  QUININE, ANHYDROUS .  4.6 .  METHANOL .  4.7 .  ORTHOPHOSPHORIC ACID SOLUTION ( 0,1 M ): WEIGH 11,53 G OF ORTHOPHOSPHORIC ACID ( 4.3 ) AND DISSOLVE IN 1 000 NL OF WATER IN A GRADUATED FLASK .  4.8 .  POTASSIUM DIHYROGENORTHOPHOSPHATE SOLUTION ( 0,1 M ): WEIGH 13,6 G OF POTASSIUM DIHYDROGENORTHOPHOSPHATE ( 4.2 ) AND DISSOLVE IN 1 000 ML OF WATER IN A GRADUATED FLASK .  4.9 .  TETRAMETHYLAMMONIUM BROMIDE SOLUTION : DISSOLVE 15,40 G OF TETRAMETHYLAMMONIUM BROMIDE ( 4.4 ) IN 1 000 ML OF WATER IN A GRADUATED FLASK .  4.10  ELUANT : ORTHOPHOSPHORIC ACID ( 4.7 ) / POTASSIUM DIHYDROGENORTHOPHOSPHATE ( 4.8 ) / TETRAMETHYLAMMONIUM BROMIDE ( 4.9)/WATER/ACETONITRILE ( 4.1 ) 10/50/100/340/90 ( V/V/V/V/V ).  //  THE COMPOSITION OF THIS MOBILE PHASE MAY BE CHANGED IN ORDER TO ACHIEVE A RESOLUTION FACTOR R  1,5 .  1.2.3.4 //  //  R = 2  D'R2 - D'R1 W1 + W2   //  WHERE   //  //  1.2.3 //  R1 AND R2  = RETENTION TIMES, IN MINUTES, OF THE PEAKS,   //  W1 AND W2  = PEAK WIDTHS AT HALF HEIGHT, IN MILLIMETRES,   //  D'  = THE CHART SPEED, IN MILLIMETRES PER MINUTE .  1.24.11 .  SILICA TREATED WITH OCTADECYLSILANE, 10 *M .  4.12 .  STANDARD SOLUTIONS : WEIGH ACCURATELY APPROXIMATELY 5,0, 10,0, 15,0 AND 20,0 MG RESPECTIVELY OF QUININE ANHYDROUS ( 4.5 ) INTO A SET OF 100 ML STANDARD FLASKS . MAKE UP TO THE MARK WITH METHANOL ( 4.6 ) AND SHAKE THE CONTENTS OF THE FLASKS UNTIL THE QUININE DISSOLVES . FILTER EACH SAMPLE THROUGH A 0,5 *M FILTER .  5 .  APPARATUS  5.1 .  USUAL LABORATORY EQUIPMENT .  5.2 .  ULTRASONIC BATH .  5.3 .  HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY EQUIPMENT WITH A VARIABLE WAVELENGTH DETECTOR .  5.4 .  COLUMN : LENGTH : 250 MM; INTERNAL DIAMETER : 4,6 MM; FILLING : SILICA ( 4.11 ).  5.5 .  MILLIPORE FILTER FH 0,5 *M, OR EQUIVALENT, WITH SUITABLE FILTRATION APPARATUS .  6 .  PROCEDURE  6.1 .  SAMPLE PREPARATION   //  WEIGH ACCURATELY INTO A 100 ML STANDARD FLASK A QUANTITY OF THE PRODUCT SUFFICIENT TO CONTAIN 10,0 MG OF ANHYDROUS QUININE, ADD 20 ML OF METHANOL ( 4.6 ) AND PLACE THE FLASK IN AN ULTRASONIC BATH ( 5.2 ) FOR 20 MINUTES . MAKE UP TO THE MARK WITH METHANOL ( 4.6 ). MIX THE SOLUTION AND THEN FILTER AN ALIQUOT ( 5.5 ).  6.2 .  CHROMATOGRAPHY   //  FLOWRATE : 1,0 ML/MIN .   //  DETECTOR WAVELENGTH ( 5.3 ) : 332 NM .   //  INJECTION VOLUME : 10 UL OF FILTERED SOLUTION ( 6.1 ).   //  MEASUREMENT : PEAK AREA .  6.3 .  CALIBRATION CURVE   //  INJECT AT LEAST THREE TIMES 10,0 *L OF EACH REFERENCE SOLUTION ( 4.12 ), MEASURE THE AREA OF THE PEAKS, AND CALCULATE THE AVERAGE AREA AT EACH CONCENTRATION .   //  PRODUCE THE CALIBRATION CURVE AND VERIFY THAT IT IS RECTILINEAR .  7 .CALCULATION  7.1 .  FROM THE CALIBRATION CURVE ( 6.3 ) DETERMINE THE QUANTITY IN *G OF ANHYDROUS QUININE PRESENT IN THE VOLUME INJECTED ( 6.2 ).  7.2 .  THE CONCENTRATION OF ANHYDROUS QUININE IN THE SAMPLE, AS A PERCENTAGE BY MASS (% M/M ), IS OBTAINED BY THE FOLLOWING FORMULA :   //  % ( M/M ) OF ANHYDROUS QUININE = B  A   //  WHERE   //  B IS THE QUANTITY, IN MICROGRAMS, OF ANHYDROUS QUININE DETERMINED IN THE 10 MICROLITRES OF THE FILTERED SOLUTION ( 6.1 ).   //  A IS THE MASS OF THE SAMPLE IN GRAMS ( 6.1 ).  8 .  REPEATABILITY ( 1 )   //  FOR AN ANHYDROUS QUININE CONTENT OF 0,5 % ( M/M ), THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS PERFORMED IN PARALLEL ON THE SAME SAMPLE MUST NOT EXCEED 0,02 %.   //  FOR AN ANHYDROUS QUININE CONTENT OF 0,2 % ( M/M ), THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS PERFORMED IN PARALLEL ON THE SAME SAMPLE MUST NOT EXCEED 0,01 %.  IDENTIFICATION AND DETERMINATION OF INORGANIC SULPHITES AND HYDROGEN SULPHITES  SCOPE AND FIELD OF APPLICATION  THE METHOD DESCRIBES THE IDENTIFICATION AND DETERMINATION OF INORGANIC SULPHITES AND HYDROGEN SULPHITES IN COSMETIC PRODUCTS . IT IS ONLY APPLICABLE TO PRODUCTS THAT HAVE AN AQUEOUS OR ALCOHOLIC PHASE AND FOR CONCENTRATIONS UP TO 0,2 % SULPHUR DIOXIDE .  A . IDENTIFICATION  1.21 .  PRINCIPLE   //  THE SAMPLE IS HEATED IN HYDROCHLORIC ACID, AND SULPHUR DIOXIDE LIBERATED IS IDENTIFIED EITHER BY ITS ODOUR OR ITS EFFECT ON AN INDICATOR PAPER .  2 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY .  2.1 .  HYDROCHLORIC ACID ( 4 M ).  2.2 .  POTASSIUM IODATE STARCH PAPER OR OTHER SUITABLE ALTERNATIVE .  3 .  APPARATUS  3.1 .  NORMAL LABORATORY EQUIPMENT .  3.2 .  FLASK ( 25 ML ) FITTED WITH A SHORT REFLUX CONDENSER .  4 .  PROCEDURE  4.1 .  PLACE ABOUT 2,5 G OF SAMPLE IN THE FLASK ( 3.2 ) WITH 10 ML OF HYDROCHLORIC ACID ( 2.1 ).  4.2 .  MIX AND HEAT TO BOILING .  4.3 .  TEST FOR THE EMISSION OF SULPHUR DIOXIDE EITHER BY SMELL OR  ( 1 ) ISO 5725 .  B . DETERMINATION  1.21 .  DEFINITION   //  THE SULPHITE OR HYDROGEN SULPHITE CONTENT OF THE SAMPLE AS DETERMINED BY THE METHOD IS EXPRESSED AS PERCENTAGE BY MASS OF SULPHUR DIOXIDE .  2 .  PRINCIPLE   //  AFTER ACIDIFICATION OF THE SAMPLE, SULPHUR DIOXIDE LIBERATED IS DISTILLED INTO A SOLUTION OF HYDROGEN PEROXIDE . SULPHURIC ACID FORMED IS TITRATED AGAINST A STANDARDIZED SODIUM HYDROXIDE SOLUTION .  3 .  REAGENTS   //  ALL REAGANTS SHOULD BE OF ANALYTICAL PURITY .  3.1 .  HYDROGEN PEROXIDE 0,2 % ( M/V ). PREPARE DAILY .  3.2 .  ORTHOPHOSPHORIC ACID ( D 25  4 = 1,75 ).  3.3 .  METHANOL .  3.4 .  SODIUM HYDROXIDE ( 0,01 M ) STANDARDIZED SOLUTION .  3.5 .  NITROGEN .  3.6 .  INDICATOR : MIXTURE 1 : 1 ( V/V ) OF METHYL RED ( 0,03 % M/V IN ETHANOL ) AND METHYLENE BLUE ( 0,05 % M/V IN ETHANOL ). FILTER THE SOLUTION .  4 .  APPARATUS  4.1 .  NORMAL LABORATORY EQUIPMENT .  4.2 .  DISTILLATION APPARATUS ( SEE FIGURE ).  5 .  PROCEDURE  5.1 .  WEIGH ACCURATELY ABOUT 2,5 G OF SAMPLE INTO THE DISTILLATION FLASK A ( SEE FIGURE ).  5.2 .  ADD 60 ML OF WATER AND 50 ML OF METHANOL ( 3.3 ) AND MIX .  5.3 .  PLACE 10 ML OF HYDROGEN PEROXIDE ( 3.1 ), 60 ML OF WATER AND A FEW DROPS OF INDICATOR ( 3.6 ) IN THE DISTILLATION RECEIVER D ( SEE FIGURE ). ADD A FEW DROPS OF SODIUM HYDROXIDE ( 3.4 ) UNTIL THE INDICATOR TURNS GREEN .  5.4 .  REPEAT 5.3 FOR THE WASH BOTTLE E ( SEE FIGURE ).  5.5 .  ASSEMBLE THE APPARATUS AND ADJUST THE NITROGEN ( 3.5 ) FLOW TO ABOUT 60 BUBBLES PER MINUTE .  5.6 .  RUN 15 ML OF ORTHOPHOSPHORIC ACID ( 3.2 ) FROM THE FUNNEL INTO THE DISTILLATION FLASK A .  5.7 .  HEAT RAPIDLY TO BOILING AND THEN SIMMER GENTLY FOR A TOTAL TIME OF 30 MINUTES .  5.8 .  DETACH THE DISTILLATION RECEIVER D . RINSE THE TUBE AND THEN TITRATE WITH SODIUM HYDROXIDE SOLUTION ( 3.4 ) UNTIL THE INDICATOR TURNS GREEN ( 3.6 ).  6 .  CALCULATION   //  CALCULATE THE CONTENT OF SULPHITE OR HYDROGEN SULPHITE BY MASS IN THE SAMPLE BY THE EXPRESSSION :  1.2.3.4 //  //  % M/M OF SULPHUR DIOXIDE =  3,2 MV M   //  WHERE   //  //  1.2.3 //  M  = MOLAR CONCENTRATION OF SODIUM HYDROXIDE SOLUTION ( 3.4 ),  //  V  = VOLUME OF SODIUM HYDROXIDE ( 3.4 ) REQUIRED FOR TITRATION ( 5.8 ), IN MILLILITRES,   //  M  = MASS OF SAMPLE ( 5.1 ) IN GRAMS .  1.27 .  REPEATABILITY ( 1 )   //  FOR A CONTENT OF 0,2 % M/M OF SULPHUR DIOXIDE THE DIFFERENCE BETWEEN TWO PARALLEL DETERMINATIONS DONE ON THE SAME SAMPLE SHOULD NOT BE GREATER THAN 0,006 %. INDICATOR PAPER ( 2.2 ).  ( 1 ) ISO 5725 .  SULPHURDIOXIDE DISTILLATION APPARATUS ACCORDING TO TANNER  ALL DIMENSIONS IN MM  IDENTIFICATION AND DETERMINATION OF CHLORATES OF THE ALKALI METALS  SCOPE AND FIELD OF APPLICATION  THE METHOD DESCRIBES THE IDENTIFICATION AND DETERMINATION OF CHLORATES IN TOOTHPASTES AND OTHER COSMETIC PRODUCTS .  A . IDENTIFICATION  1.21 .  PRINCIPLE   //  CHLORATES ARE SEPARATED FROM OTHER HALATES BY THIN LAYER CHROMATOGRAPHY AND IDENTIFIED BY THE OXIDATION OF IODIDE TO FORM IODINE .  2 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY .  2.1 .  REFERENCE SOLUTIONS : AQUEOUS SOLUTIONS OF POTASSIUM CHLORATE, BROMATE AND IODATE ( 0,2 % M/V ) PREPARED FRESHLY .  2.2 .  DEVELOPMENT SOLVENT : AMMONIA SOLUTION ( 28 % M/V ) ACETONE/BUTANOL ( 60/130/30 V/V/V ).  2.3 .  POTASSIUM IODIDE, AQUEOUS SOLUTION ( 5 % M/V ).  2.4 .  STARCH SOLUTION ( 1 TO 5 % M/V ).  2.5 .  HYDROCHLORIC ACID ( 1 M ).  2.6 .  READY-FOR-USE CELLULOSE THIN-LAYER PLATES ( 0,25 MM ).  3 .  APPARATUS   //  NORMAL EQUIPMENT FOR THIN LAYER CHROMATOGRAPHY .  4 .  PROCEDURE  4.1 .  EXTRACT ABOUT 1 G OF THE SAMPLE WITH WATER, FILTER, AND DILUTE TO ABOUT 25 ML .  4.2 .  DEPOSIT 2 *L ON THE PLATE ( 2.6 ) OF THE SOLUTION ( 4.1 ) TOGETHER WITH 2 *L ALIQUOTS OF EACH OF THE THREE REFERENCE SOLUTIONS ( 2.1 ).  4.3 .  PLACE THE PLATE IN A TANK AND DEVELOP BY ASCENDING CHROMATOGRAPHY ABOUT THREE-QUARTERS OF THE LENGTH OF THE PLATE ( 2.6 ) WITH SOLVENT 2.2 .  4.4 .  REMOVE FROM THE TANK AND ALLOW THE SOLVENT TO EVAPORATE . ( NB : THIS MAY TAKE UP TO TWO HOURS .)  4.5 .  SPRAY THE PLATE WITH POTASSIUM IODIDE ( 2.3 ) AND ALLOW TO DRY FOR ABOUT FIVE MINUTES .  4.6 .  SPRAY THE PLATE WITH STARCH SOLUTION ( 2.4 ) AND ALLOW TO DRY FOR ABOUT FIVE MINUTES .  4.7 .  SPRAY THE PLATE WITH HYDROCHLORIC ACID ( 2.5 ).  5 .  EVALUATION   //  IF THE CHLORATE IS PRESENT A BLUE SPOT ( POSSIBLY A BROWN SPOT ) WILL APPEAR AFTER HALF AN HOUR WITH RF VALUE APPROXIMATELY 0,7 TO 0,8 .  1.2.3 //   //  //  //  HALATES  RF   //   //  //  //  IODATE  0 TO 0,2   //  BROMATE  0,5 TO 0,6   //  CHLORATE  0,7 TO 0,8   //   //  //  1.2 //  IT SHOULD BE NOTED THAT BROMATES AND IODATES GIVE IMMEDIATE REACTION . CARE SHOULD BE TAKEN NOT TO CONFUSE SPOTS FROM BROMATES AND CHLORATES .  B . DETERMINATION  1.21 .  DEFINITION   //  THE CHLORATE CONTENT OF THE SAMPLE DETERMINED BY THIS METHOD IS EXPRESSED AS PERCENTAGE BY MASS OF CHLORATE .  2 .  PRINCIPLE   //  CHLORATE IS REDUCED BY ZINC POWDER UNDER ACID CONDITIONS . THE FORMED CHLORIDE IS MEASURED BY POTENTIOMETRIC TITRATION USING A SILVER NITRATE SOLUTION . A SIMILAR DETERMINATION BEFORE REDUCTION PERMITS THE POSSIBLE PRESENCE OF HALIDES .  3 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY .  3.1 .  ACETIC ACID, 80 % ( M/M ).  3.2 .  ZINC POWDER .  3.3 .  SILVER NITRATE STANDARD SOLUTION ( 0,1 M ).  4 .  APPARATUS  4.1 .  NORMAL LABORATORY EQUIPMENT .  4.2 .  POTENTIOMETER EQUIPPED WITH A SILVER INDICATOR ELECTRODE .  5 .  PROCEDURE  5.1 .  SAMPLE PREPARATION   //  WEIGH ACCURATELY A QUANTITY "M' OF APPROXIMATELY 2 G IN CENTRIFUGE TUBE . ADD ABOUT 15 ML ACETIC ACID ( 3.1 ) AND MIX CAREFULLY . WAIT 30 MINUTES AND CENTRIFUGE FOR 15 MINUTES AT 2 000 REV/MIN . TRANSFER THE SUPERNATANT SOLUTION TO A 50 ML VOLUMETRIC FLASK . REPEAT CENTRIFUGING TWICE BY ADDING 15 ML ACETIC ACID ( 3.1 ) TO THE RESIDUE . COLLECT THE SOLUTION CONTAINING CHLORATE IN THE SAME VOLUMETRIC FLASK . FILL TO THE MARK WITH ACETIC ACID ( 3.1 ).  5.2 .  REDUCTION OF CHLORATE   //  TAKE 20 ML OF SOLUTION 5.1 AND ADD 0,6 G OF ZINC POWDER ( 3.2 ). BRING TO THE BOIL IN A FLASK FITTED WITH A CONDENSER TUBE . AFTER 30 MINUTES BOILING, COOL AND FILTER . RINSE THE FLASK WITH WATER . FILTER AND COMBINE THE FILTRATE WITH THE RISES .  5.3 .  DETERMINATION OF CHLORIDE   //  TITRATE 20 ML SOLUTION 5.2 WITH SILVER NITRATE ( 3.3 ) BY USING THE POTENTIOMETER ( 4.2 ). TITRATE IN THE SAME WAY 20 ML OF SOLUTION 5.1 WITH SILVER NITRATE ( 3.3 ).   //  NB : IF THE PRODUCT CONTAINS BROMINE OR IODINE DERIVATIVES WHICH CAN RELEASE BROMIDES OR IODIDES AFTER REDUCTION, THE TITRATION CURVE WILL HAVE SEVERAL INFLEXION POINTS . IN THIS CASE THE VOLUME OF THE TITRATED SOLUTION ( 3.3 ) CORRESPONDING TO CHLORIDE IS THE DIFFERENCE BETWEEN THE LAST AND THE PENULTIMATE INFLEXION POINTS .  6 .  CALCULATION   //  THE CONTENT OF CHLORATE OF THE SAMPLE (% M/M ) IS CALCULATED BY THE FORMULA :  1.2.3.4 //  //  CHLORATE ( CLO3 -) % M/M =  20,9 ( V - V' ) M M   //  WHERE   //  //  1.2.3 //  V  = VOLUME IN MILLILITRES, OF SILVER NITRATE SOLUTION ( 3.3 ) USED TO TITRATE SOLUTION 5.2,   //  V'  = VOLUME, IN MILLILITRES, OF SILVER NITRATE SOLUTION ( 3.3 ) USED TO TITRATE 20 MILLILITRES OF SOLUTION 5.1,   //  M  = MOLALITY OF SILVER NITRATE STANDARD SOLUTION ( 3.3 ),   //  M  = MASS OF SAMPLE, IN GRAMS .  1.27 .  REPEATABILITY ( 1 )   //  FOR A CHLORATE CONTENT OF 3 TO 5 % M/M THE DIFFERENCE BETWEEN THE RESULTS OF TWO DETERMINATIONS CARRIED OUT IN PARALLEL ON  ( 1 ) ISO 5725 .  IDENTIFICATION AND DETERMINATION OF SODIUM IODATE  SCOPE AND FIELD OF APPLICATION  THE METHOD DESCRIBES THE PROCEDURE FOR IDENTIFYING AND DETERMINING RINSE OF COSMETIC PRODUCTS CONTAINING SODIUM IODATE .  A . IDENTIFICATION  1.21 .  PRINCIPLE   //  SODIUM IODATE IS SEPARATED FROM OTHER HALATES BY THIN LAYER CHROMATOGRAPHY AND IDENTIFIED BY THE OXIDATION OF IODIDE TO FORM IODINE .  2 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY .  2.1 .  REFERENCE SOLUTIONS . AQUEOUS SOLUTIONS OF POTASSIUM CHLORATE, BROMATE AND IODATE ( 0,01 % M/V ) PREPARED FRESHLY .  2.2 .  DEVELOPMENT SOLVENT .   //  AMMONIA SOLUTION ( 28 % M/V ) / ACETONE / BUTANOL ( 60/130/30 V/V/V ).  2.3 .  POTASSIUM IODIDE AQUEOUS SOLUTION ( 5 % M/V ).  2.4 .  STARCH SOLUTION ( 1 TO 5 % M/V ).  2.5 .  HYDROCHLORIC ACID ( 1 M ).  3 .  APPARATUS  3.1 .  READY-FOR-USE CELLULOSE THIN-LAYER CHROMATOGRAPHY ( 0,25 MM ) PLATES .  3.2 .  NORMAL EQUIPMENT FOR THIN LAYER CHROMATOGRAPHY .  4 .  PROCEDURE  4.1 .  EXTRACT ABOUT 1 G OF THE SAMPLE WITH WATER, FILTER, AND DILUTE TO ABOUT 10 ML .  4.2 .  DEPOSIT 2 *L OF THIS SOLUTION ONTO THE BASE LINE OF THE PLATE ( 3.1 ) TOGETHER WITH 2 *L ALIQUOTS OF EACH OF THE THREE REFERENCE SOLUTIONS ( 2.1 ).  4.3 .  PLACE THE PLATE IN A TANK AND DEVELOP BY ASCENDING CHROMATOGRAPHY ABOUT THREE-QUARTERS OF THE LENGTH OF THE PLATE WITH SOLVENT ( 2.2 ).4.4 .  REMOVE THE PLATE FROM THE TANK AND ALLOW THE SOLVENT TO EVAPORATE AT AMBIENT TEMPARATURE ( NB : THIS MAY TAKE UP TO TWO HOURS ).  4.5 .  SPRAY THE PLATE WITH POTASSIUM IODIDE ( 2.3 ) AND ALLOW TO DRY FOR ABOUT FIVE MINUTES .  4.6 .  SPRAY WITH STARCH ( 2.4 ) AND ALLOW TO DRY FOR ABOUT FIVE MINUTES .  4.7 .  FINALLY SPRAY WITH HYDROCHLORIC ( 2.5 ).  5 .  EVALUATION   //  IF IODATE IS PRESENT A BLUE SPOT ( THE COLOUR MAY BE BROWN OR BECOME BROWN ON STANDING ) WILL APPEAR IMMEDIATELY WITH AN RF VALUE APPROXIMATELY 0 TO 0,2 .   //  IT SHOULD BE NOTED THAT BROMATES GIVE IMMEDIATE REACTIONS AT RF VALUES APPROXIMATELY AT 0,5 TO 0,6 AND CHLORATES, AFTER ABOUT 30 MINUTES, AT RF VALUES OF 0,7 TO 0,8 RESPECTIVELY .  B . DETERMINATION  1.21 .  DEFINITION   //  THE SODIUM IODATE CONTENT AS DETERMINED BY THIS METHOD IS EXPRESSED AS A PERCENTAGE BY MASS OF SODIUM IODATE .  2 .  PRINCIPLE   //  SODIUM IODATE IS DISSOLVED IN WATER AND DETERMINED BY MEANS OF HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY, USING IN SERIES, A REVERSE-PHASE C18 COLUMN AND AN ANION-EXCHANGE COLUMN .  3 .  REAGENTS   //  ALL REAGENTS SHOULD BE OF ANALYTICAL PURITY AND ESPECIALLY SUITABLE FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY ( HPLC ).  3.1 .  HYDROCHLORIC ACID ( 4 M ).  3.2 .  SODIUM SULPHITE AQ, 5 % M/V .  3.3 .  SODIUM IODATE STOCK SOLUTION .   //  PREPARE A STOCK SOLUTION CONTAINING 50 MG SODIUM IODATE PER 100 ML WATER .  3.4 .  POTASSIUM DIHYDROGENORTHOPHOSPHATE .  3.5 .  DISODIUM HYDROGENORTHOPHOSPHATE  2H20 .  3.6 .  HPLC MOBILE PHASE : DISSOLVE 3,88 G POTASSIUM DIHYDROGENORTHOPHOSPHATE ( 3.4 ) AND 1,19 G DISODIUM HYDROGENORTHOPHOSPHATE  2H2O ( 3.5 ) IN 1 LITRE WATER .   //  THE PH OF THE RESULTING SOLUTION IS 6.2 .  3.7 .  UNIVERSAL INDICATOR PAPER, PH 1-11 .  4 .  APPARATUS  4.1 .  ORDINARY LABORATORY APPARATUS .  4.2 .  CIRCULAR FILTER PAPER, DIAMETER 110 MM, SCHLEICHER AND SCHUELL NO 575, OR EQUIVALENT .  4.3 .  HIGH-PERFORMANCE LIQUID CHROMATOGRAPH WITH A VARIABLE WAVELENGTH DETECTOR .  4.4 .  COLUMNS : LENGTH : 120 MM; INTERNAL DIAMETER : 4,6 MM; NUMBER : TWO CONNECTED IN SERIES; FIRST COLUMN - NECLEOSIL R 5 C18 OR EQUIVALENT; SECOND COLUMN - VYDAC TM-301-SB OR EQUIVALENT .  5 .  PROCEDURE  5.1 .  SAMPLE PREPARATION  5.1.1 .  FLUID SAMPLES ( SHAMPOOS )   //  WEIGH ACCURATELY A TEST PORTION OF APPROXIMATELY 1,0 G SAMPLE IN A 10 ML GLASS STOPPERED CALIBRATED TUBE OR MEASURING FLASK .  //  FILL UP TO THE MARK WITH WATER AND MIX .   //  IF NECESSARY, FILTER THE SOLUTION .   //  DETERMINE THE IODATE IN THE SOLUTION BY MEANS OF HPLC AS DESCRIBED IN SECTION 5.2 .  5.1.2 .  SOLID SAMPLES ( SOAP )   //  FINELY DIVIDE PART OF THE SAMPLE AND WEIGH ACCURATELY A TEST PORTION OF APPROXIMATELY 1,0 G INTO A 100 ML GLASS STOPPERED MEASURING CYLINDER . FILL UP TO 50 ML WITH WATER AND SHAKE VIGOROUSLY FOR ONE MINUTE . CENTRIFUGE AND FILTER THROUGH A FILTER PAPER ( 4.1 ) OR ALLOW THE MIXTURE TO STAND FOR AT LEAST ONE NIGHT .   //  SHAKE THE JELLYLIKE SOLUTION VIGOROUSLY AND FILTER IT THROUGH A FILTER PAPER ( 4.1 ).   //  DETERMINE THE IODATE IN THE FILTRATE BY MEANS OF HPLC AS DESCRIBED IN SECTION 5.2 .  5.2 .  CHROMATOGRAPHY   //  FLOWRATE : 1 ML/MIN .   //  DETECTOR WAVELENGTH ( 4.2 ): 210 NM .   //  INJECTION VOLUME : 10 *L .   //  MEASUREMENT : PEAK AREA .  5.3 .  CALIBRATION   //  PIPETTE RESPECTIVELY 1,0, 2,0, 5,0, 10,0 AND 20,0 ML OF THE SODIUM IODATE STOCK SOLUTION ( 3.3 ) INTO 50 ML VOLUMETRIC FLASKS . FILL TO THE MARK AND MIX .   //  THE SOLUTIONS THUS OBTAINED, CONTAIN 0,01, 0,02, 0,05, 0,10 AND 0,20 MG SODIUM IODATE PER ML RESPECTIVELY .   //  INJECT A 10 *L PORTION OF EACH STANDARD IODATE SOLUTION INTO THE LIQUID CHROMATOGRAPH ( 4.2 ) AND OBTAIN A CHROMATOGRAM . DETERMINE THE PEAK AREA FOR IODATE AND PLOT A CURVE RELATING THE PEAK AREA TO THE SODIUM IODATE CONCENTRATION .  6 .  CALCULATION   //  CALCULATE THE SODIUM IODATE CONTENT, IN PERCENTAGE BY MASS (% M/M ), USING THE FORMULA :  1.2.3.4 //  //  % ( M/M ) OF SODIUM IODATE =  VC 10 M   //  WHERE   //  //  1.2.3 //  M  IS THE MASS, IN GRAMS, OF THE TEST PORTION ( 5.1 ),   //  V  IS THE TOTAL VOLUME OF THE SAMPLE SOLUTION, IN MILLILITRES, OBTAINED AS DESCRIBED IN 5.1,   //  C  IS THE CONCENTRATION, IN MILLIGRAMS PER MILLILITRE OF SODIUM IODATE, OBTAINED FROM THE CALIBRATION CURVE ( 5.3 ).  1.27 .  REPEATABILITY ( 1 )   //  FOR A SODIUM IODATE CONTENT OF 0,1 % ( M/M ) THE DIFFERENCE BETWEEN THE RESULTS OF TWO PARALLEL DETERMINATIONS CARRIED OUT ON THE SAME SAMPLE MUST NOT EXCEED 0,002 %.  8 .  CONFIRMATION  8.1 .  PRINCIPLE   //  IN AN ACIDIFIED SOLUTION OF A COSMETIC PRODUCT, IODATE ( IO3 -) IS REDUCED TO IODIDE ( I -) BY SULPHITE AND THE RESULTING SOLUTION IS INVESTIGATED BY MEANS OF HPLC . IF A PEAK HAVING A RETENTION TIME CORRESPONDING TO THE RETENTION TIME OF IODATE DISAPPEARS AFTER TREATMENT WITH SULPHITE, THE ORIGINAL PEAK CAN MOST PROBABLY BE ATTRIBUTED TO IODATE .  8.2 .  PROCEDURE   //  PIPETTE A 5 ML PORTION OF THE SAMPLE SOLUTION OBTAINED AS DESCRIBED IN SECTION 5.1 INTO A CONICAL FLASK .   //  ADJUST THE PH OF THE SOLUTION TO A VALUE OF 3 OR LOWER WITH HYDROCHLORIC ACID ( 3.1 ); UNIVERSAL INDICATOR PAPER ( 3.7 ).   //  ADD THREE DROPS OF SODIUM SULPHITE SOLUTION ( 3.2 ) AND MIX .  //  INJECT A 10 *L PORTION OF THE SOLUTION INTO THE LIQUID CHROMATOGRAPH ( 4.2 ).   //  COMPARE THIS CHROMATOGRAM WITH THE CHROMATOGRAM OBTAINED AS DESCRIBED IN PARAGRAPH 5 FOR THE SAME SAMPLE . THE SAME SAMPLE SHOULD NOT EXCEED 0,07 % M/M .  ( 1 ) ISO 5725 .


title: Commission Directive 2009/106/EC of 14 August 2009 amending Council Directive 2001/112/EC relating to fruit juices and certain similar products intended for human consumption

text:
               15.8.2009

               EN

               Official Journal of the European Union

               L 212/42

      COMMISSION DIRECTIVE 2009/106/EC
   of 14 August 2009
   amending Council Directive 2001/112/EC relating to fruit juices and certain similar products intended for human consumption
   THE COMMISSION OF THE EUROPEAN COMMUNITIES,
   Having regard to the Treaty Establishing the European Communities,
   Having regard to Council Directive 2001/112/EC of 20 December 2001 relating to fruit juices and certain similar products intended for human consumption (1), and in particular article 7 thereof,
   Whereas:

               (1)

               In order to enhance free movement of fruit juices and certain similar products within the Community, Directive 2001/112/EC has laid down specific provisions regarding production, composition and labelling of the products concerned. Those rules should be adapted to technical progress and should take account of developments in relevant international standards, in particular the Codex Standard for fruit juices and nectars (Codex Stan 247-2005) which was adopted by the Codex Alimentarius Commission during its 28th session on 4-9 July 2005 and the Code of Practice of the European Fruit juice Association (AIJN).

               (2)

               This Codex Standard establishes in particular quality factors and labelling requirements for fruit juices and similar products. The AIJN Code of Practice also establishes quality factors for fruit juice from concentrate and is internationally used as a reference standard for self-regulation in the fruit juice industry. Directive 2001/112/EC should be brought into line, as far as possible, with these standards.

               (3)

               This Codex Standard lays down that the product made by reconstituting concentrated fruit juice is described as ‘fruit juice from concentrate’. The corresponding labelling requirement at Community level should also use these internationally recognised terms. In order to ensure consistency of labelling in all Member States, linguistic versions should be modified where necessary to comply with the Codex wording.

               (4)

               This Codex Standard and the AIJN code of practice also establish minimum Brix values for a list of fruit juices from concentrate; as these values facilitate the testing for minimum quality requirements, they should be taken into consideration as far as they correspond to the reference values used in the Community.

               (5)

               Directive 2001/112/EC should be amended accordingly.

               (6)

               The measures provided for in this Directive are in accordance with the opinion of the Standing Committee on the Food Chain and Animal Health,

         HAS ADOPTED THIS DIRECTIVE:
   Article 1
   Directive 2001/112/EC is amended as follows:

               1.

               In Article 3, paragraph 6, the words ‘made with concentrate(s)’ and ‘partially made with concentrate(s)’ shall be replaced by the words ‘from concentrate(s)’ and ‘partially from concentrate(s)’ respectively.

               2.

               In Annex I, Part I (Definitions), paragraph 1, point (b), the second subparagraph is replaced by the following:
               ‘The product thus obtained shall display organoleptic and analytical characteristics at least equivalent to those of an average type of juice obtained from fruits of the same kind within the meaning of point (a). The minimum Brix levels for fruit juices from concentrate are indicated in Annex V.’

               3.

               An Annex V, as set out in the Annex to this Directive, is added.

         Article 2
   The Member States shall, by 1 January 2011 at the latest, bring into force the laws, regulations and administrative provisions necessary to comply with this Directive. They shall immediately communicate the text of those provisions to the Commission.
   When the Member States adopt those measures, they shall contain a reference to this Directive or shall be accompanied by such reference on the occasion of their official publication.
   The methods of making such reference shall be laid down by the Member States.
   Article 3
   This Directive shall enter into force on the seventh day following its publication in the Official Journal of the European Union.
   Article 4
   This Directive is addressed to the Member States.

      Done at Brussels, 14 August 2009.

            For the Commission

         Mariann FISCHER BOEL

            Member of the Commission

      (1)  OJ L 10, 12.1.2002, p. 58.

      ANNEX

            ‘ANNEX V

                        Fruit’s Common Name

                        Botanical Name

                        Minimum degree Brix values for reconstituted fruit juice and reconstituted fruit purée

                        Apple (*)

                           Malus domestica Borkh.

                        11,2

                        Apricot (**)

                           Prunus armeniaca L.

                        11,2

                        Banana (**)

                           Musa sp.

                        21,0

                        Blackcurrant (*)

                           Ribes nigrum L.

                        11,6

                        Grape (*)

                           Vitis vinifera L. or hybrids thereof

                           Vitis labrusca L. or hybrids thereof

                        15,9

                        Grapefruit (*)

                           Citrus x paradise Macfad.

                        10,0

                        Guava (**)

                           Psidium guajava L.

                        9,5

                        Lemon (*)

                           Citrus limon (L.) Burm.f.

                        8,0

                        Mango (**)

                           Mangifera indica L.

                        15,0

                        Orange (*)

                           Citrus sinensis (L.) Osbeck

                        11,2

                        Passion Fruit (*)

                           Passiflora edulis Sims

                        13,5

                        Peach (**)

                           Prunus persica (L.) Batsch var. Persica

                        10,0

                        Pear (**)

                           Pyrus communis L.

                        11,9

                        Pineapple (*)

                           Ananas comosus (L.) Merr.

                        12,8

                        Raspberry (*)

                           Rubus idaeus L.

                        7,0

                        Sour Cherry (*)

                           Prunus cerasus L.

                        13,5

                        Strawberry (*)

                           Fragaria x ananassa Duch.

                        7,0

                        Mandarin (*)

                           Citrus reticulata Blanco

                        11,2

                        If a juice from concentrate is manufactured from a fruit not mentioned in the above list, the minimum Brix level of the reconstituted juice shall be the Brix level of the juice as extracted from the fruit used to make the concentrate.
                        For those products marked with an asterisk (*), which are produced as a juice, a minimum relative density is determined as such in relation to water at 20/20 °C.
                        For those products marked with two asterisks (**), which are produced as a purée, only a minimum uncorrected Brix reading (without correction of acid) is determined.
                        In respect of blackcurrant, guava, mango and passion fruit, the minimum Brix degree values only apply to reconstituted fruit juice and reconstituted fruit purée produced in the Community.’