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Commission Regulation (EC) No 2870/2000 of 19 December 2000 laying down Community reference methods for the analysis of spirits drinks

EU Regulation No 2870/2000 · Adopted 19 December 2000 · Extends to United Kingdom

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Commission Regulation (EC) No 2870/2000

of 19 December 2000

laying down Community reference methods for the analysis of spirits drinks

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Community,

Having regard to Council Regulation (EEC) No 1576/89 of 29 May 1989 laying down general rules on the definition, description and presentation of spirit drinksf1, as amended by the Act of Accession of Austria, Finland and Sweden, and in particular Article 4(8) thereof,

Whereas:

(1)

Article 4(8) of Regulation (EEC) No 1576/89 provides for the adoption of methods to be used for analysing spirit drinks. Reference methods should be used to ensure compliance with Regulation (EEC) No 1576/89 and Commission Regulation (EEC) No 1014/90 of 24 April 1990 laying down detailed implementing rules on the definition, description and presentation of spirit drinksf2, as last amended by Regulation (EC) No 2140/98f3, when any official control takes place or in the event of a dispute.

(2)

As far as possible, it would be useful to adopt and describe as Community analytical reference methods generally recognised methods.

(3)

In order to take account of scientific advances and of differences in the equipment of official laboratories, the use of methods based on principles of measurement other than the reference methods described in the Annex hereto should be permitted under the responsibility of the laboratory director, where those methods offer adequate guarantees as regards results and in particular meet the criteria set in the Annex to Council Directive 85/591/EEC of 20 December 1985 concerning the introduction of Community methods of sampling and analysis for the monitoring of foodstuffs intended for human consumptionf4 and if it can be shown that the variation in the accuracy, repeatability and reproducibility of the results obtained is within the limits of those obtained using the reference methods described in this Regulation. If that condition is met, the use of other analytical methods should be allowed. However, it is important to specify that in cases of dispute other methods may not replace reference methods.

(4)

The measures provided for in this Regulation are in accordance with the opinion of the Implementation Committee for Spirit Drinks,

HAS ADOPTED THIS REGULATION:

Annotations to the whole text

Footnotes

f1

OJ L 160, 12.6.1989, p. 1.

f2

OJ L 105, 25.4.1990, p. 9.

f3

OJ L 270, 7.10.1998, p. 9.

f4

OJ L 372, 31.12.1985, p. 50.

Contents

  1. 1Article 1
  2. 2Article 2
  3. 3Article 3
  4. 4Article 4
  5. 5Article 5
  6. Signature
  7. Annex
  8. DETERMINATION OF ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS
  9. Introduction
  10. 1Scope
  11. 2Normative References
  12. Terms and Definitions
  13. 3.1Division 3.1
  14. Note 1:
  15. Division
  16. 3.2Division 3.2
  17. 3.3Division 3.3
  18. Note 2:
  19. Division
  20. 3.4Division 3.4
  21. Note 3:
  22. Division
  23. 4Principle
  24. APPENDIX I: PREPARATION OF DISTILLATE
  25. 1Scope
  26. 2Principle
  27. Reagents and Materials
  28. 3.1Division 3.1
  29. 3.2Division 3.2
  30. 4Apparatus and equipment
  31. Note:
  32. Division
  33. 5Storage of test samples
  34. 6Procedure
  35. 6.1Division 6.1
  36. 6.2Division 6.2
  37. Note:
  38. Division
  39. 6.3Division 6.3
  40. Note:
  41. Division
  42. APPENDIX II: MEASUREMENT OF DENSITY OF DISTILLATE
  43. DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS — MEASUREMENT BY PYCNOMETRY
  44. A.1Principle
  45. A.2Reagents and materials
  46. A.2.1Division A.2.1
  47. A.3Apparatus and Equipment
  48. Note 1:
  49. Division
  50. A.4Procedure
  51. A.4.1Calibration of pycnometer
  52. A.4.1.1Division A.4.1.1
  53. A.4.1.1.1Division A.4.1.1.1
  54. A.4.1.1.2Division A.4.1.1.2
  55. A.4.1.1.3Division A.4.1.1.3
  56. A.4.1.1.4Calculation
  57. A.4.1.2Division A.4.1.2
  58. A.4.2Determination of alcoholic strength of test sample
  59. Method performance characteristics (precision)
  60. A.5.1Statistical results of the interlaboratory test
  61. DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS — MEASUREMENT BY ELECTRONIC DENSIMETRY (BASED ON THE RESONANT FREQUENCY OSCILLATION OF A SAMPLE IN AN OSCILLATION CELL)
  62. B.1Principle
  63. B.2Reagents and materials
  64. B.3Apparatus and equipment
  65. B.4Procedure
  66. Method performance characteristics (precision)
  67. B.5.1Statistical results of the interlaboratory test
  68. DETERMINATION OF REAL ALCOHOLIC STRENGTH BY VOLUME OF SPIRIT DRINKS — MEASUREMENT BY DENSIMETRY USING HYDROSTATIC BALANCE
  69. C.1Principle
  70. C.2Reagents and materials
  71. C.2.1Float cleaning solution (sodium hydroxide, 30 % w/v)
  72. C.3Apparatus and Equipment
  73. Note 1:
  74. Division
  75. C.4Procedure
  76. Method performance characteristics (precision)
  77. C.5.1Statistical results of the interlaboratory test
  78. DETERMINATION OF TOTAL DRY EXTRACT OF SPIRIT DRINKS BY GRAVIMETRY
  79. 1Scope
  80. 2Normative References
  81. 3Definition
  82. 4Principle
  83. 5Apparatus and Equipment
  84. 6Sampling and samples
  85. Procedure
  86. 7.1Division 7.1
  87. 7.2Division 7.2
  88. 8Calculation
  89. Method performance characteristics (precision)
  90. 9.1Statistical results of the interlaboratory test
  91. DETERMINATION OF VOLATILE SUBSTANCES AND METHANOL OF SPIRIT DRINKS
  92. GENERAL REMARKS
  93. 1Definitions
  94. 2Gas chromatographic analysis of volatile compounds
  95. GAS CHROMATOGRAPHIC DETERMINATION OF VOLATILE CONGENERS: ALDEHYDES, HIGHER ALCOHOLS, ETHYL ACETATE AND METHANOL
  96. 1Scope
  97. 2Normative References
  98. 3Definition
  99. 4Principle
  100. 5Reagents and materials
  101. 6Apparatus and equipment
  102. 7Sampling and samples.
  103. 8Procedure (used for the validated method)
  104. 9Calculation
  105. 10Quality assurance and control (used for the validated method)
  106. 11Method performance characteristics (precision)
  107. DETERMINATION OF VOLATILE ACIDITY OF SPIRIT DRINKS
  108. 1Scope
  109. 2Normative references
  110. Definitions
  111. 3.1Division 3.1
  112. 3.2Division 3.2
  113. 3.3Division 3.3
  114. 4Principle
  115. 5Reagents and materials
  116. 5.1Division 5.1
  117. 5.2Division 5.2
  118. 6Apparatus and equipment
  119. 7Sampling and samples
  120. Procedure
  121. Total acidity
  122. 8.1.1Preparation of sample
  123. 8.1.2Titration
  124. 8.1.3Calculation
  125. Fixed acidity
  126. 8.2.1Preparation of sample
  127. 8.2.2Titration
  128. 8.2.3Calculation
  129. Calculation of volatile acidity
  130. 9.1Division 9.1
  131. 9.2Division 9.2
  132. 9.3Division 9.3
  133. Method performance characteristics (Precision)
  134. 10.1Statistical results of the interlaboratory test
  135. (1)Division (1)
  136. (2)Division (2)
  137. ANETHOLE. GAS CHROMATOGRAPHIC DETERMINATION OF TRANS-ANETHOLE IN SPIRIT DRINKS
  138. 1Scope
  139. 2Normative references
  140. 3Principle
  141. 4Reagents and materials
  142. 4.1Division 4.1
  143. 4.2Division 4.2
  144. 4.3Division 4.3
  145. 4.4Division 4.4
  146. 4.5Preparation of standard solutions
  147. 4.5.1Standard solution A
  148. 4.5.2Internal standard solution B
  149. 4.5.3Solutions used to check the linearity response of the flame ionisation detector (FID)
  150. 4.5.4Standard solution C
  151. Apparatus and equipment
  152. 5.1Division 5.1
  153. 5.2Division 5.2
  154. 5.3Capillary column, for example:
  155. 5.4Division 5.4
  156. 6Chromatography conditions
  157. 7Samples
  158. Procedure
  159. 8.1Sample screening for estragole
  160. 8.2Preparation of unknown samples
  161. 8.3Blank
  162. 8.4Linearity test
  163. 8.5Determination
  164. 9Calculation of response factor
  165. 9.1Response factor (RF i ) calculation
  166. 9.2Analysis of the linearity response test solutions
  167. 9.3Analysis of the sample
  168. 10Calculation of results
  169. 11Quality assurance and control
  170. 12Treatment of spirits sample containing large amount of sugar and of liqueur sample prior to GC analysis
  171. 12.1Principle
  172. 12.2Reagents and materials
  173. 12.2.1Division 12.2.1
  174. 12.2.2Division 12.2.2
  175. 12.3Apparatus and equipment
  176. Procedure
  177. 12.4.1Sample screening for estragole
  178. 12.4.2Extraction
  179. 12.4.3Preparation of the extracted sample to be analysed
  180. 12.5Determination
  181. 12.6Calculation of results
  182. 12.7Quality control and assurance
  183. 13Method performance characteristics (precision)
  184. GLYCYRRHIZIC ACID. DETERMINATION OF GLYCYRRHIZIC ACID USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY
  185. 1Scope
  186. 2Normative references
  187. 3Principle
  188. 4Reagents and materials
  189. 4.1Division 4.1
  190. 4.2Division 4.2
  191. 4.3Division 4.3
  192. 4.4Division 4.4
  193. 4.5Division 4.5
  194. Preparation of the HPLC elution solutions
  195. 4.6.1Elution solvent A (example)
  196. Note:
  197. Division
  198. 4.6.2Elution solvent B
  199. 4.7Preparation of standard solutions
  200. 4.7.1Reference solution C
  201. 4.7.2Standard solutions used to check the linearity of the response of the instrumentation
  202. Apparatus and equipment
  203. Separation system
  204. 5.1.1Division 5.1.1
  205. 5.1.2Division 5.1.2
  206. 5.1.3Division 5.1.3
  207. 5.1.4Division 5.1.4
  208. 5.2Division 5.2
  209. 5.3Division 5.3
  210. Laboratory equipment
  211. 5.4.1Division 5.4.1
  212. 5.4.2Division 5.4.2
  213. 5.4.3Division 5.4.3
  214. Chromatography conditions
  215. 6.1Elution characteristics: (example)
  216. 6.2Detection:
  217. Procedure
  218. 7.1Preparation of the spirit sample
  219. 7.2Determination
  220. 8Method performance characteristics (precision)
  221. CHALCONES. HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR VERIFYING THE PRESENCE OF CHALCONES IN PASTIS
  222. 1Scope
  223. 2Normative references
  224. 3Principle
  225. 4Reagents and materials
  226. 4.1Division 4.1
  227. 4.2Division 4.2
  228. 4.3Division 4.3
  229. 4.4Division 4.4
  230. 4.5Division 4.5
  231. Preparation of solutions
  232. 4.6.1Ethanol 50 % volume
  233. 4.6.2Solvent A: acetonitrile
  234. 4.6.3Solvent B: 0,1 M sodium acetate buffer solution, pH 4,66.
  235. Preparation of the reference extract from Glycyrrhiza glabra (4.3)
  236. 5.1Division 5.1
  237. 5.2Division 5.2
  238. 5.3Division 5.3
  239. 5.4Division 5.4
  240. 5.5Division 5.5
  241. 5.6Division 5.6
  242. Apparatus and equipment
  243. Separation system.
  244. 6.1.1Division 6.1.1
  245. 6.1.2Division 6.1.2
  246. 6.1.3Division 6.1.3
  247. 6.1.4Division 6.1.4
  248. 6.1.5Division 6.1.5
  249. 6.2Division 6.2
  250. 6.3Column
  251. 6.4Division 6.4
  252. Chromatography conditions (example).
  253. 6.5.1Elution characteristics of solvents A (4.6.2) and B (4.6.3):
  254. 6.5.2Division 6.5.2
  255. 6.5.3UV detector settings:
  256. Procedure
  257. 7.1Preparation of the spirit sample
  258. 7.2Preparation of the residual liquorice extract (5.6)
  259. Determination
  260. 7.3.1Division 7.3.1
  261. 7.3.2Division 7.3.2
  262. 7.3.3Division 7.3.3
  263. 8Characteristic chromatogram for a pastis
  264. 9Method performance characteristics (precision)
  265. TOTAL SUGARS
  266. 1Scope
  267. 2Normative references
  268. 3Principle
  269. Reagents and materials
  270. 4.1Division 4.1
  271. 4.2Division 4.2
  272. 4.3Division 4.3
  273. 4.4Division 4.4
  274. 4.5Division 4.5
  275. 4.6Division 4.6
  276. 4.7Division 4.7
  277. 4.8Solvents (example)
  278. 4.9Division 4.9
  279. 4.10Division 4.10
  280. 4.11Preparation of stock standard solution (20 g/l)
  281. 4.12Preparation of working standard solutions (2,5, 5,0, 7,5, 10,0 and 20,0 g/L)
  282. Apparatus and Equipment
  283. HPLC system capable of achieving baseline resolution of all of the sugars.
  284. 5.1.1Division 5.1.1
  285. 5.1.2Division 5.1.2
  286. 5.1.3Division 5.1.3
  287. 5.1.4Division 5.1.4
  288. 5.1.5Division 5.1.5
  289. 5.1.6Division 5.1.6
  290. 5.1.7Division 5.1.7
  291. 5.2Division 5.2
  292. 5.3Division 5.3
  293. 6Sample storage
  294. Procedure
  295. PART A: Sample preparation
  296. 7.1.1Division 7.1.1
  297. 7.1.2Division 7.1.2
  298. PART B: HPLC
  299. 7.2.1Determination
  300. 7.2.2Division 7.2.2
  301. 8Calculation
  302. Method performance characteristics (precision)
  303. 9.1Statistical results of the interlaboratory test
  304. (1)Division (1)
  305. (2)Division (2)
  306. EGG YOLK. DETERMINATION OF EGG YOLK CONCENTRATION IN SPIRIT DRINKS — PHOTOMETRIC METHOD
  307. 1Scope
  308. 2Normative references
  309. 3Principle
  310. Reagents and materials
  311. 4.1Division 4.1
  312. 4.2Division 4.2
  313. 4.3Division 4.3
  314. 4.4Division 4.4
  315. 4.5Division 4.5
  316. 4.6Division 4.6
  317. 4.7Division 4.7
  318. 4.8Reagent for phosphate determination:
  319. Apparatus and equipment
  320. 5.1Division 5.1
  321. 5.2Division 5.2
  322. 5.3Division 5.3
  323. 5.4Division 5.4
  324. 5.5Division 5.5
  325. 5.6Division 5.6
  326. 5.7Division 5.7
  327. 5.8Division 5.8
  328. 5.9Division 5.9
  329. 5.10Division 5.10
  330. 5.11Division 5.11
  331. 5.12Division 5.12
  332. 5.13Division 5.13
  333. 6Samples
  334. Procedure
  335. Sample preparation
  336. 7.1.1Division 7.1.1
  337. 7.1.2Division 7.1.2
  338. 7.1.3Division 7.1.3
  339. 7.1.4Division 7.1.4
  340. 7.1.5Division 7.1.5
  341. 7.1.6Division 7.1.6
  342. 7.1.7Division 7.1.7
  343. 7.1.8Division 7.1.8
  344. Photometric phosphate assay
  345. Comparative solution
  346. 7.2.1.1Division 7.2.1.1
  347. 7.2.1.2Division 7.2.1.2
  348. 7.2.1.3Division 7.2.1.3
  349. 7.2.1.4Division 7.2.1.4
  350. Sample solution
  351. 7.2.2.1Division 7.2.2.1
  352. 7.2.2.2Division 7.2.2.2
  353. 7.2.2.3Division 7.2.2.3
  354. Calibration curve
  355. 7.2.3.1Division 7.2.3.1
  356. 7.2.3.2Division 7.2.3.2
  357. 7.2.3.3Construction of the calibration curve:
  358. 8Expression of results
  359. 9Method performance characteristics (precision)
  360. DETERMINATION OF THE FOLLOWING WOOD COMPOUNDS IN SPIRIT DRINKS BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY (HPLC): FURFURAL, 5-HYDROXYMETHYLFURFURAL, 5-METHYLFURFURAL, VANILLIN, SYRINGALDEHYDE, CONIFERALDEHYDE, SINAPALDEHYDE, GALLIC ACID, ELLAGIC ACID, VANILLIC ACID, SYRINGIC ACID AND SCOPOLETIN
  361. 1Scope
  362. 2Normative reference
  363. 3Principle
  364. 4Reagents
  365. 4.1Division 4.1
  366. 4.2Division 4.2
  367. 4.3Division 4.3
  368. 4.4Division 4.4
  369. 4.5Division 4.5
  370. 4.6Division 4.6
  371. 5Apparatus
  372. 5.1Division 5.1
  373. 5.2Division 5.2
  374. 5.3Division 5.3
  375. 5.4Division 5.4
  376. Procedure
  377. 6.1Preparation of the solution to be injected
  378. 6.2Division 6.2
  379. Determination
  380. 6.3.1Division 6.3.1
  381. 6.3.2Division 6.3.2
  382. 6.3.3Division 6.3.3
  383. 7Expression of results
  384. 8Performance characteristics of the method (precision)
  385. 8.1Furfural
  386. 8.25-Hydroxymethylfurfural
  387. 8.35-Methylfurfural
  388. 8.4Vanillin
  389. 8.5Syringaldehyde
  390. 8.6Coniferaldehyde
  391. 8.7Sinapaldehyde
  392. 8.8Gallic acid
  393. 8.9Ellagic acid
  394. 8.10Vanillic acid
  395. 8.11Syringic acid
  396. 8.12Scopoletin
  397. (1)Division (1)
  398. (2)Division (2)