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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)

EU Decision 1992/608 · Adopted 14 November 1992 · Extends to United Kingdom

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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)

THE COUNCIL OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Economic Community,

Having regard to Council Directive 85/397/EEC of 5 August 1985 on health and animal-health problems affecting intra-Community trade in heat-treated milkf1 and in particular Article 11 (6) thereof,

Having regard to the proposal from the Commission,

Whereas, pursuant to Article 11 (6) of Directive 85/397/EEC, the Council is to lay down the detailed arrangements for the checks provided for in Article 11 (2); whereas the purpose of such checks, to be carried out by establishments under the supervision and responsibility of the official department and with periodic inspection by the official department, is to ensure compliance with the requirements of Directive 85/397/EEC and in particular those laid down in Article 3 (A) (3) thereof;

Whereas, the laying-down of procedures for checks includes the determination of the methods to be employed for their implementation;

Whereas methods have to be prescribed for determining the total solids content, the fat content, the solids-non-fat content, the total nitrogen content, the protein content and the density of heat-treated milk intended for direct human consumption;

Whereas, for technical reasons, the initial requirement is to lay down reference methods for analysis and testing to ensure that the standards prescribed in Article 3 (A) (3) of Directive 85/397/EEC are met; whereas it is particularly important to make a study of the conditions under which routine methods for analysis and testing are Used; whereas, pending the outcome of this study, it is for the competent authorities to see that appropriate routine methods are used with a view to ensuring that the said standards are met;

Whereas the determination of the aforementioned methods includes in particular the determination of analytical procedures and the fixing of criteria of reliability in order to ensure uniform interpretation of the results,

HAS ADOPTED THIS DECISION:

Annotations to the whole text

Footnotes

f1

OJ No L 226, 24. 8. 1985, p. 13, as last amended by Directive 89/662/EEC (OJ No L 395, 30. 12. 1989, p. 13).

Contents

  1. 1Article 1
  2. 2Article 2
  3. 3Article 3
  4. 4Article 4
  5. Signature
  6. Annex I
  7. GENERAL PROVISIONS
  8. 1INTRODUCTION
  9. REAGENTS
  10. Water
  11. 2.1.1Division 2.1.1
  12. 2.1.2Division 2.1.2
  13. 2.2Chemicals
  14. EQUIPMENT
  15. 3.1Lists of equipment
  16. 3.2Analytical balance
  17. EXPRESSION OF RESULTS
  18. 4.1Results
  19. 4.2Calculation of percentage
  20. PRECISION CRITERIA: REPEATABILITY AND REPRODUCIBILITY
  21. 5.1Division 5.1
  22. 5.1.1Division 5.1.1
  23. 5.1.2Division 5.1.2
  24. 5.1.3Division 5.1.3
  25. 5.1.4Division 5.1.4
  26. 6TEST REPORT
  27. SAMPLING OF HEAT-TREATED MILK
  28. 1SCOPE AND FIELD OF APPLICATION
  29. 2GENERAL
  30. SAMPLING EQUIPMENT
  31. 3.1General
  32. SAMPLING TECHNIQUE
  33. 4.1General
  34. Manual sampling
  35. 4.2.1Sampling a divided bulk
  36. Sampling from large vessels — Storage, rail and road tanks
  37. 4.2.2.1Mix the milk by an appropriate procedure, before sampling.
  38. 4.2.2.2Mixing of the contents of large vessels or of storage, rail or road tanks can be carried out:
  39. 4.3Sampling of heat-treated milk for direct consumption in retail-packings
  40. 5IDENTIFICATIONS OF THE SAMPLE
  41. 6PRESERVATION, TRANSPORT AND STORAGE OF SAMPLES
  42. Annex ANEX II
  43. DETERMINATION OF TOTAL SOLIDS CONTENT
  44. 1SCOPE AND FIELD OF APPLICATION
  45. 2DEFINITION
  46. 3PRINCIPLE
  47. 4APPARATUS AND GLASSWARE
  48. 5PREPARATION OF THE TEST SAMPLE
  49. PROCEDURE
  50. 6.1Preparation of the dish
  51. 6.2Test portion
  52. Determination
  53. 6.3.1Division 6.3.1
  54. 6.3.2Division 6.3.2
  55. 6.3.3Division 6.3.3
  56. 6.3.4Division 6.3.4
  57. 6.3.5Division 6.3.5
  58. EXPRESSION OF RESULTS
  59. 7.1Calculation and formula
  60. Precision
  61. 7.2.1Division 7.2.1
  62. 7.2.2Division 7.2.2
  63. DETERMINATION OF FAT CONTENT
  64. 1SCOPE AND FIELD OF APPLICATION
  65. 2DEFINITION
  66. 3PRINCIPLE
  67. 4REAGENTS
  68. 4.1Division 4.1
  69. 4.2Division 4.2
  70. 4.3Congo red or Cresol red solution
  71. Division
  72. 4.4Division 4.4
  73. 4.5Division 4.5
  74. 4.6Division 4.6
  75. 5APPARATUS AND GLASSWARE
  76. Division
  77. 5.1Division 5.1
  78. Centrifuge, in which the fat-extraction flasks or tubes (5.6.) can be spun at a rotational frequency of 500 to 600 rev min-1 to produce a gravitational field of 80 to 90 g at the outer end of the flasks or tubes.
  79. Division
  80. 5.3Division 5.3
  81. 5.4Division 5.4
  82. 5.5Division 5.5
  83. 5.6Mojonnier-type fat extraction flasks
  84. Division
  85. 5.7Division 5.7
  86. 5.8Division 5.8
  87. 5.9Division 5.9
  88. 5.10Division 5.10
  89. 5.11Division 5.11
  90. 5.12Division 5.12
  91. 5.13Division 5.13
  92. PROCEDURE
  93. Division
  94. 6.1Preparations of the test sample
  95. 6.2Test portion
  96. 6.3Blank test
  97. 6.4Preparation of fat-collecting vessel
  98. Determination
  99. 6.5.1Division 6.5.1
  100. 6.5.2Division 6.5.2
  101. 6.5.3Division 6.5.3
  102. 6.5.4Division 6.5.4
  103. 6.5.5Division 6.5.5
  104. 6.5.6Carefully remove the cork or stopper and rinse it and the inside of the neck of the flask with a little of the mixed solvent (4.6.) so that the rinsings run into the flask.
  105. 6.5.7Division 6.5.7
  106. 6.5.8Rinse the outside of the neck of the extraction flask with a little of the mixed solvent (4.6.), collecting the rinsings in the fat-collecting vessel and taking care that the mixed solvent does not spread over the outside of the extraction flask.
  107. 6.5.9Division 6.5.9
  108. 6.5.10Division 6.5.10
  109. 6.5.11Carry out a third extraction by further repeating the operations described in 6.5.3. to 6.5.8. inclusive, but using only 15 ml of diethyl ether (4.4.) and 15 ml of light petroleum (4.5.); use the ether to rinse the inside of the neck of the extraction flask. If necessary, raise the interface to the middle of the neck of the flask to enable the final decantation of solvent to be as complete as possible.
  110. 6.5.12Division 6.5.12
  111. 6.5.13Heat the fat-collecting vessel (with the flask placed on its side to allow solvent vapour to escape) for one hour in the oven (5.4.). Remove the fat-collecting vessel from the oven, allow to cool (not in a desiccator, but protected from dust) to the temperature of the weighing room (for glass vessels allow at least one hour, for metal dishes allow at least 30 minutes) and weigh to the nearest 0,1 mg.
  112. 6.5.14Division 6.5.14
  113. 6.5.15Add 25 ml of light petroleum to the fat-collecting vessel in order to verify whether or not the extracted matter is wholly soluble. Warm gently and swirl the solvent until all the fat is dissolved.
  114. 6.5.16If the extracted matter is not wholly soluble in the light petroleum, or in case of doubt, extract the fat completely from the vessel by repeatedly washing with warm light petroleum.
  115. EXPRESSION OF RESULTS
  116. 7.1Calculation and formula
  117. Precision
  118. 7.2.1Repeatability (r):
  119. 7.2.2Reproducibility (R):
  120. DETERMINATION OF TOTAL NON-FAT SOLIDS
  121. 1SCOPE AND FIELD OF APPLICATION
  122. 2DEFINITION AND CALCULATION
  123. DETERMINATION OF TOTAL NITROGEN CONTENT
  124. 1SCOPE AND FIELD OF APPLICATION
  125. 2DEFINITION
  126. 3PRINCIPLE
  127. REAGENTS
  128. 4.1Division 4.1
  129. 4.2Division 4.2
  130. 4.3Division 4.3
  131. Sodium hydroxide solution, 47% (m/m) 704 g NaOH/1 (20 oC).
  132. Division
  133. 4.5Division 4.5
  134. 4.6Division 4.6
  135. 4.7Volumetric solution
  136. 4.8Division 4.8
  137. 4.9Division 4.9
  138. Tryptophan (C11H12N2O2), phenacetin (C10H7CH2CONH2) or lysine mono- or di-hydrochloride (C6H14N2O2 HCl or C6H14N2O2 · 2HCl).
  139. Division
  140. 5APPARATUS AND GLASSWARE
  141. PROCEDURE
  142. To the Kjeldahl flask (5.1.) add boiling aid (5.2.) (eg. three glass beads), 15 g of potassium sulphate (4.1.), 1,0 ml of copper sulphate solution (4.2.), approximately 5 g of milk sample (weighed to the nearest 0,001 g) and 25 ml of sulphuric acid (4.3.). Use the acid to wash down any copper sulphate solution, potassium sulphate or milk on the neck of the flask, and gently mix the contents of the flask.
  143. Division
  144. 6.2Heat each Kjeldahl flask on the digestion apparatus (5.5.), very gently at first so that all the black froth stays within the bulb. When the initial frothing has ceased and copious white vapour appears, boil vigorously (acid vapour will condense half-way up the neck of the flask) until no black particles remain and until the digest becomes clear pale blue-green in colour. Then boil gently for at least 1,5 hours. Note the following requirements:
  145. When the Kjeldahl flasks are cool, add 300 ml of water (see note) to each so as to wash carefully down the neck of the flask, and mix the contents thoroughly ensuring that the crystals which have separated out are dissolved. Add some boiling aid (5.2.) to ensure uniform boiling. Then to each flask, add 70 ml of sodium hydroxide solution (4.4.) (see note) by gently pouring the solution down the inclined neck of the flask to form a bottom layer in the bulb; do not wet the top of the neck with the sodium hydroxide solution.
  146. Division
  147. 6.4Immediately connect each Kjeldahl flask to a distillation apparatus (5.6.). Ensure that the tip of the condenser outlet-tube is immersed in 50 ml of boric acid solution (4.5.) together with 0,20 ml (5 - 6 drops) of indicator solution (4.6.) all contained in a conical flask (5.8.). Swirl the contents of each Kjeldahl flask to mix thoroughly and boil, but gently at first to prevent excessive frothing. When 100 to 125 ml of distillate have been collected, lower each conical flask until the tip of the condenser outlet-tube is approximately 40 mm above the 200 ml mark. Continue each distillation until irregular boiling (‘bumping’) starts and then immediately stop the heating. Disconnect each Kjeldahl flask and rinse the tip of each condenser outlet-tube with a little water, collecting the rinsings in the conical flask. Note the following requirements:
  148. 6.5Titrate each distillate with standard volumetric solution (4.7.) until the pH is 4,6 ± 0,1, using a pH meter and if desired an automatic burette. Addition of an indicator helps to check whether the titration is proceeding correctly. Take each burette reading to the nearest 0.01 ml with the aid of a magnifying lens (5.10.) avoiding errors of parallax.
  149. Carry out a blank test according to 6.1. to 6.5. inclusive, taking 5 ml of distilled water together with about 0,1 g of sucrose (4.8.) through the procedure instead of the milk sample.
  150. Division
  151. 6.7Division 6.7
  152. 6.7.1Check that no loss of nitrogen occurs as a result of excessive heat or mechanical leaks during distillation, by using a test portion of 0,15 g of ammonium oxalate or sulphate (4.9.) weighed to the nearest 0,001 g together with 0,1 g of sucrose (4.8.).
  153. 6.7.2Division 6.7.2
  154. 7SAFETY PRECAUTIONS
  155. EXPRESSION OF RESULTS
  156. 8.1Calculation and formula:
  157. Precision
  158. 8.2.1Division 8.2.1
  159. 8.2.2Division 8.2.2
  160. MODIFIED PROCEDURES
  161. 9.1Division 9.1
  162. 9.2Division 9.2
  163. 9.3A test portion of 1 g of milk (semi-macro Kjeldahl) can be used instead of 5 g (6.1.) provided:
  164. Division
  165. DETERMINATION OF PROTEIN CONTENT
  166. 1SCOPE AND FIELD OF APPLICATION
  167. 2DEFINITION
  168. 3CALCULATION
  169. DETERMINATION OF SPECIFIC MASS
  170. 1SCOPE AND FIELD OF APPLICATION
  171. 2DEFINITION
  172. 3PRINCIPLE
  173. 4APPARATUS AND GLASSWARE
  174. 4.1Hydrometer
  175. 4.2Cylinders (glass or stainless steel).
  176. 4.3Division 4.3
  177. 4.4Division 4.4
  178. 4.5Division 4.5
  179. PROCEDURE
  180. 5.1Division 5.1
  181. 5.2Division 5.2
  182. 5.3Division 5.3
  183. 5.4Division 5.4
  184. TEMPERATURE CORRECTION
  185. 6.1Division 6.1
  186. 7EXPRESSION OF RESULTS
  187. PRECISION
  188. 8.1Division 8.1
  189. 8.2Division 8.2
  190. (to Annex II)