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Council Decision of 14 November 1992 laying down methods for the analysis and testing of heat-treated milk for direct human consumption (92/608/EEC)

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  1. Introductory Text

  2. Article 1.The methods for analysing and testing heat-treated milk shall be...

  3. Article 2.The implementation of the reference methods for analysis and testing,...

  4. Article 3.The methods referred to in Article 1 are set out...

  5. Article 4.This Decision is addressed to the Member States.

  6. Signature

    1. ANNEX I

      1. I. GENERAL PROVISIONS

        1. 1. INTRODUCTION

        2. 2. REAGENTS

          1. 2.1. Water

            1. 2.1.1. Wherever mention is made to water for solution, dilution or...

            2. 2.1.2. Wherever reference is made to ‘solution’ or ‘dilution’ without further...

          2. 2.2. Chemicals

        3. 3. EQUIPMENT

          1. 3.1. Lists of equipment

          2. 3.2. Analytical balance

        4. 4. EXPRESSION OF RESULTS

          1. 4.1. Results

          2. 4.2. Calculation of percentage

        5. 5. PRECISION CRITERIA: REPEATABILITY AND REPRODUCIBILITY

          1. 5.1. The precision criteria given in each method is defined as...

            1. 5.1.1. Repeatability (r) is the value below which the absolute difference...

            2. 5.1.2. Reproducibility (R) is the value below which the absolute difference...

            3. 5.1.3. Unless otherwise specified for each individual method the values for...

            4. 5.1.4. The necessary collaborative trials and studies should be planned and...

        6. 6. TEST REPORT

      2. II. SAMPLING OF HEAT-TREATED MILK

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. GENERAL

        3. 3. SAMPLING EQUIPMENT

          1. 3.1. General

        4. 4. SAMPLING TECHNIQUE

          1. 4.1. General

          2. 4.2. Manual sampling

            1. 4.2.1. Sampling a divided bulk

            2. 4.2.2. Sampling from large vessels — Storage, rail and road tanks...

              1. 4.2.2.1. Mix the milk by an appropriate procedure, before sampling.

              2. 4.2.2.2. Mixing of the contents of large vessels or of storage,...

          3. 4.3. Sampling of heat-treated milk for direct consumption in retail-packings

        5. 5. IDENTIFICATIONS OF THE SAMPLE

        6. 6. PRESERVATION, TRANSPORT AND STORAGE OF SAMPLES

    2. ANEX II

      1. I. DETERMINATION OF TOTAL SOLIDS CONTENT

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. PRINCIPLE

        4. 4. APPARATUS AND GLASSWARE

        5. 5. PREPARATION OF THE TEST SAMPLE

        6. 6. PROCEDURE

          1. 6.1. Preparation of the dish

          2. 6.2. Test portion

          3. 6.3. Determination

            1. 6.3.1. Pre-dry the dish for 30 minutes by heating it on...

            2. 6.3.2. Heat the dish, with its lid alongside, in the oven...

            3. 6.3.3. Allow to cool in the desiccator (4.2.) to room temperature...

            4. 6.3.4. Heat the dish again, with its lid alongside, in the...

            5. 6.3.5. Repeat the operations described in 6.3.4. until the difference in...

        7. 7. EXPRESSION OF RESULTS

          1. 7.1. Calculation and formula

          2. 7.2. Precision

            1. 7.2.1. Repeatability (r): 0,10 g of total solids per 100 g...

            2. 7.2.2. Reproducibility (R): 0,20 g of total solids per 100 g...

      2. II. DETERMINATION OF FAT CONTENT

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. PRINCIPLE

        4. 4. REAGENTS

          1. 4.1. Ammonia solution, containing approximately 25 % (m/m) of NH3. A...

          2. 4.2. Ethanol, at least 94% (v/v). Ethanol denatured by methanol may...

          3. 4.3. Congo red or Cresol red solution

          4. 4.4. Diethylether, free from peroxides not containing more than 2 mg/kg...

          5. 4.5. Light petroleum, having any boiling range between 30 and 60...

          6. 4.6 Mixed solvent, prepared shortly before use by mixing equal volumes...

        5. 5. APPARATUS AND GLASSWARE

          2. 5.1. Analytical balance

          3. 5.2. Centrifuge, in which the fat-extraction flasks or tubes (5.6.) can...

          4. 5.3. Distillation or evaporation apparatus, to permit the solvents and ethanol...

          5. 5.4. Oven, electrically heated, with ventilation port(s) fully open, capable of...

          6. 5.5. Water bath, capable of being maintained at a temperature of...

          7. 5.6. Mojonnier-type fat extraction flasks

          8. 5.7. Rack, to hold the fat-extraction flasks (or tubes) (see 5.6.)....

          9. 5.8. Wash bottle, suitable for use with the mixed solvent (4.6.)....

          10. 5.9. Fat-collecting vessels, for example boiling flasks (flat-bottom), or Erlenmeyer flasks...

          11. 5.10. Boiling aids, fat-free, of non-porous porcelain or silicon carbide or...

          12. 5.11. Measuring cylinders, of capacities 5 and 25 ml.

          13. 5.12. Pipettes, graduated, of capacity 10 ml.

          14. 5.13. Tongs, made of metal, suitable for holding flasks, beakers or...

        6. 6. PROCEDURE

          2. 6.1. Preparations of the test sample

          3. 6.2. Test portion

          4. 6.3. Blank test

          5. 6.4. Preparation of fat-collecting vessel

          6. 6.5. Determination

            1. 6.5.1. Add 2 ml of the ammonia solution (4.1.) or an...

            2. 6.5.2. Add 10 ml of the ethanol (4.2.) and mix gently...

            3. 6.5.3. Add 25 ml of diethyl ether (4.4.), close the flask...

            4. 6.5.4. Add 25 ml of light petroleum (4.5.), close the flask...

            5. 6.5.5. Centrifuge the closed flask for one to five minutes at...

            6. 6.5.6. Carefully remove the cork or stopper and rinse it and...

            7. 6.5.7. Holding the extraction flask by the small bulb, carefully decant...

            8. 6.5.8. Rinse the outside of the neck of the extraction flask...

            9. 6.5.9. Add 5 ml of the ethanol (4.2.) to the contents...

            10. 6.5.10. Carry out a second extraction by repeating the operations, described...

            11. 6.5.11. Carry out a third extraction by further repeating the operations...

            12. 6.5.12. Remove the solvents (including ethanol) as completely as possible from...

            13. 6.5.13. Heat the fat-collecting vessel (with the flask placed on its...

            14. 6.5.14. Repeat the operations described in 6.5.13. until the mass of...

            15. 6.5.15. Add 25 ml of light petroleum to the fat-collecting vessel...

            16. 6.5.16. If the extracted matter is not wholly soluble in the...

        7. 7. EXPRESSION OF RESULTS

          1. 7.1. Calculation and formula

          2. 7.2. Precision

            1. 7.2.1. Repeatability (r):

            2. 7.2.2. Reproducibility (R):

      3. III. DETERMINATION OF TOTAL NON-FAT SOLIDS

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION AND CALCULATION

      4. IV. DETERMINATION OF TOTAL NITROGEN CONTENT

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. PRINCIPLE

        4. 4. REAGENTS

          1. 4.1. Potassium sulphate (K2SO4).

          2. 4.2. Copper sulphate solution. Dissolve 5,0 g of copper (II) sulphate...

          3. 4.3. Sulphuric acid, at least 98,0% (m/m) H2SO4.

          4. 4.4. Sodium hydroxide solution, 47% (m/m) 704 g NaOH/1 (20 oC)....

          5. 4.5. Boric acid solution. Dissolve 40 g of boric acid (H3BO3)...

          6. 4.6. Indicator solution. Dissolve 0,01 g methyl red, 0,02 g bromothymol...

          7. 4.7. Volumetric solution

          8. 4.8. Nitrogen-free sucrose.

          9. 4.9. Ammonium salt, pure, such as ammonium oxalate (NH4)2C2O4,H2O or ammonium...

          10. 4.10. Tryptophan (C11H12N2O2), phenacetin (C10H7CH2CONH2) or lysine mono- or di-hydrochloride (C6H14N2O2...

        5. 5. APPARATUS AND GLASSWARE

        6. 6. PROCEDURE

          1. 6.1. To the Kjeldahl flask (5.1.) add boiling aid (5.2.) (eg....

          2. 6.2. Heat each Kjeldahl flask on the digestion apparatus (5.5.), very...

          3. 6.3. When the Kjeldahl flasks are cool, add 300 ml of...

          4. 6.4. Immediately connect each Kjeldahl flask to a distillation apparatus (5.6.)....

          5. 6.5 Titrate each distillate with standard volumetric solution (4.7.) until the...

          6. 6.6. Carry out a blank test according to 6.1. to 6.5....

          7. 6.7. Regularly check the accuracy of the procedure by using two...

          8. 6.7.1. Check that no loss of nitrogen occurs as a result...

          9. 6.7.2. Check that the digestion procedure is sufficient to release all...

        7. 7. SAFETY PRECAUTIONS

        8. 8. EXPRESSION OF RESULTS

          1. 8.1. Calculation and formula:

          2. 8.2. Precision

            1. 8.2.1. Repeatability (r): 0,007 g per 100 g.

            2. 8.2.2. Reproducibility (R): 0,015 g per 100 g.

        9. 9. MODIFIED PROCEDURES

          1. 9.1. Use a block digestion apparatus fitted with cylindrical flasks, instead...

          2. 9.2. Use of steam distillation instead of direct heating of the...

          3. 9.3. A test portion of 1 g of milk (semi-macro Kjeldahl)...

      5. V. DETERMINATION OF PROTEIN CONTENT

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. CALCULATION

      6. VI. DETERMINATION OF SPECIFIC MASS

        1. 1. SCOPE AND FIELD OF APPLICATION

        2. 2. DEFINITION

        3. 3. PRINCIPLE

        4. 4. APPARATUS AND GLASSWARE

          1. 4.1. Hydrometer

          2. 4.2. Cylinders (glass or stainless steel).

          3. 4.3. Water bath regulated at 20 ± 0,1 oC.

          4. 4.4. Water bath regulated at 40 ± 2 oC.

          5. 4.5. Thermometer, graduated to 0,5 oC.

        5. 5. PROCEDURE

          1. 5.1. Mix the sample by inversion to disperse the fat and...

          2. 5.2. Mix the sample thoroughly by careful inversion to avoid inclusion...

          3. 5.3. When the hydrometer reaches equilibrium read the graduation at the...

          4. 5.4. Immediately after taking the hydrometer reading introduce the thermometer (4.5.)...

        6. 6. TEMPERATURE CORRECTION

          1. 6.1. If the temperature of the milk sample is not exactly...

        7. 7. EXPRESSION OF RESULTS

        8. 8. PRECISION

          1. 8.1. Repeatability (r): 0,0003 g/ml.

          2. 8.2. Reproducibility (R): 0,0015 g/ml.

      7. Appendix

        (to Annex II)

        1. ALTERNATIVE PROCEDURE USING FAT-EXTRACTION TUBES WITH SIPHON OR WASH-BOTTLE FITTINGS...

          1. A.1. PROCEDURE

            1. A.1.1. Preparation of the test sample

            2. A.1.2. Test portion

            3. A.1.3. Blank test

            4. A.1.4. Preparation of fat-collecting vessel

            5. A.1.5. Determination

              1. A.1.5.1. Add 2 ml of the ammonia solution (4.1.), or an...

              2. A.1.5.2. Add 10 ml of the ethanol (4.2.) and mix gently...

              3. A.1.5.3. Add 25 ml of diethyl ether (4.4.), close the tube...

              4. A.1.5.4. Add 25 ml of light petroleum (4.5.), close the tube...

              5. A.1.5.5. Centrifuge the closed tube for one to five minutes at...

              6. A.1.5.6. Carefully remove the cork or stopper and rinse it and...

              7. A.1.5.7. Insert a siphon fitting or a wash-bottle fitting into the...

              8. A.1.5.8. Loosen the fitting from the neck of the tube, slightly...

              9. A.1.5.9. Again loosen the fitting from the neck, slightly raise the...

              10. A.1.5.10. Carry out the second extraction by repeating the operations described...

              11. A.1.5.11. Carry out a third extraction by again repeating the operations...

              12. A.1.5.12. Proceed as described in 6.5.12. to 6.5.16.

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