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Commission Regulation (EEC) No 2568/91 of 11 July 1991 on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis

EU Regulation No 2568/1991 · Adopted 11 July 1991 · Extends to United Kingdom

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Commission Regulation (EEC) No 2568/91

of 11 July 1991

on the characteristics of olive oil and olive-residue oil and on the relevant methods of analysis

THE COMMISSION OF THE EUROPEAN COMMUNITIES,

Having regard to the Treaty establishing the European Economic Community,

Having regard to Council Regulation No 136/66/EEC of 22 September 1966 on the establishment of a common organization of the market in oils and fatsf1, as last amended by Regulation (EEC) No 3577/90f2, and in particular Article 35a thereof,

Whereas the Annex to Regulation No 136/66/EEC contains the descriptions and definitions of olive oil and olive-residue oil marketed within each Member State, in intra-Community trade and in trade with third countries;

Whereas, for the purpose of differentiating between the various types of oil, the physical and chemical characteristics of each of them and the organoleptic characteristics of virgin oil should be defined, in order to guarantee the purity and quality of the products concerned, without prejudice to other existing provisions;

Whereas the presence of the characteristics of the different types of oil should be determined uniformly throughout the Community; whereas, to that end, Community methods of chemical analysis and organoleptic evaluation should be established; whereas the use should be permitted, for a transitional period, of other methods of analysis applied in the Member States provided that where there is a difference in the results, those obtained using the common method will be decisive;

Whereas the definition of the physical and chemical characteristics of olive oil and of the methods of analysis entails the amendment of the additional notes to Chapter 15 of the combined nomenclature;

Whereas the method of evaluating the organoleptic characteristics of virgin oil includes the setting up of panels of selected and trained tasters; whereas the period necessary for establishing such a structure should therefore be fixed; whereas in view of the difficulties that some Member States will encounter in setting up panels of tasters, the use of panels in other Member States should be authorized;

Whereas, in order to ensure that the system of levies applicable to imports of olive residues functions correctly, a single method for the determination of the oil content of these products should be laid down;

Whereas, in order not to harm trade, provision should be made for oil packaged prior to the entry into force of this Regulation to be disposed of during a limited period;

Whereas it is necessary to repeal Commission Regulation (EEC) No 1058/77f3, as last amended by Regulation (EEC) No 1858/88f4;

Whereas the Management Committee for Oils and Fats has not delivered an opinion within the time limit set by its chairman,

HAS ADOPTED THIS REGULATION:

Annotations to the whole text

Footnotes

f1

OJ No 172, 30.9.1966, p. 3025/66.

f2

OJ No L 353, 17.12.1990, p. 23.

f3

OJ No L 128, 24.5.1977, p. 6.

f4

OJ No L 166, 1.7.1988, p. 10.

Contents

  1. 1Article 1
  2. 2Article 2
  3. 2aArticle 2a
  4. 3Article 3
  5. 3aArticle 3a Repealed
  6. 4Article 4
  7. 5Article 5 Repealed
  8. 6Article 6
  9. 7Article 7
  10. 7aArticle 7a
  11. 8Article 8 Repealed
  12. 9Article 9
  13. 10Article 10 Repealed
  14. Signature
  15. Annex ES: SUMMARY
  16. Annex I: OLIVE OIL CHARACTERISTICS
  17. Quality characteristics
  18. Purity characteristics
  19. Notes:
  20. (a)Division (a)
  21. (b)Division (b)
  22. (c)Division (c)
  23. (d)Division (d)
  24. Appendix
  25. Annex IaSAMPLING OF OLIVE OIL OR OLIVE-POMACE OIL DELIVERED IN IMMEDIATE PACKAGING
  26. CONTENT OF PRIMARY SAMPLE
  27. 1.1Immediate packaging not exceeding 5 litres
  28. 1.2Immediate packaging exceeding 5 litres
  29. ANALYSES AND RESULTS
  30. 2.1Division 2.1
  31. 2.2Where all the results of the analyses comply with the characteristics of the category of oil declared, the whole batch is to be declared to comply.
  32. VERIFICATION OF THE CATEGORY OF BATCH
  33. 3.1In order to verify the batch category, the competent authority may increase the number of primary samples taken at different points of the batch according to the following table:
  34. 3.2Division 3.2
  35. Annex Ib: FLOW-CHART FOR VERIFYING WHETHER AN OLIVE OIL SAMPLE IS CONSISTENT WITH THE CATEGORY DECLARED
  36. General table
  37. Table 1 — Extra Virgin Olive Oil — Quality criteria
  38. Table 2 — Virgin Olive Oil — Quality criteria
  39. Table 3 — Extra Virgin Olive Oil and Virgin Olive Oil — Purity criteria
  40. Table 4 — Lampante Olive Oil — Purity criteria
  41. Table 5 — Refined Olive Oil — Quality criteria
  42. Table 6 — Olive Oil (composed of refined olive oil and virgin olive oils) — Quality criteria
  43. Table 7 — Refined Olive Oil and olive oil composed of refined olive oil and Virgin Olive Oils — Purity criteria
  44. Table 8 — Crude Olive-Pomace Oil — Purity criteria
  45. Table 9 — Refined Olive-Pomace Oil — Quality criteria
  46. Table 10 — Olive Pomace Oil — Quality criteria
  47. Table 11 — Refined Olive-Pomace Oil and Olive-Pomace Oil — Purity criteria
  48. Annex II: DETERMINATION OF FREE FATTY ACIDS, COLD METHOD
  49. 1SCOPE AND FIELD OF APPLICATION
  50. 2PRINCIPLE
  51. 3REAGENTS
  52. 3.1Division 3.1
  53. Note 1:Division Note 1:
  54. Note 2:Division Note 2:
  55. 3.2Division 3.2
  56. Note 3:Division Note 3:
  57. 3.3Division 3.3
  58. 4APPARATUS
  59. PROCEDURE
  60. 5.1Preparation of the test sample
  61. 5.2Test portion
  62. 5.3Determination
  63. Note 4:Division Note 4:
  64. Note 5:Division Note 5:
  65. 6EXPRESSION OF RESULTS
  66. Annex III: DETERMINATION OF PEROXIDE VALUE
  67. 1Scope
  68. 2Definition
  69. 3Principle
  70. 4Apparatus
  71. Division
  72. 4.1Division 4.1
  73. 4.2Division 4.2
  74. 4.3Division 4.3
  75. 4.4Division 4.4
  76. Reagents
  77. 5.1Division 5.1
  78. 5.2Division 5.2
  79. 5.3Division 5.3
  80. 5.4Sodium thiosulphate, 0,01 mol/l (equivalent to 0,01 N) accurately standardised aqueous solution, standardised just before use.
  81. 5.5Division 5.5
  82. 6Sample
  83. 7Procedure
  84. 8Expression of results
  85. Annex IV: DETERMINATION OF WAX CONTENT BY CAPILLARY COLUMN GAS CHROMATOGRAPHY
  86. 1SUBJECT
  87. 2PRINCIPLE
  88. EQUIPMENT
  89. 3.1Division 3.1
  90. 3.2Division 3.2
  91. 3.3Division 3.3
  92. 3.3.1Division 3.3.1
  93. 3.3.2Division 3.3.2
  94. 3.3.3Division 3.3.3
  95. 3.3.4Division 3.3.4
  96. 3.3.5Division 3.3.5
  97. 3.4Division 3.4
  98. 3.5Division 3.5
  99. 3.6Division 3.6
  100. 3.7Division 3.7
  101. 3.8Division 3.8
  102. 3.9Division 3.9
  103. REAGENTS
  104. 4.1Division 4.1
  105. 4.2Division 4.2
  106. 4.3Division 4.3
  107. 4.4Division 4.4
  108. 4.5Division 4.5
  109. 4.5.1Division 4.5.1
  110. 4.6Division 4.6
  111. 4.7Division 4.7
  112. PROCEDURE
  113. 5.1Preparation of the chromatographic column.
  114. NB:
  115. Division
  116. Analysis by gas chromatography
  117. 5.2.1Preparatory work
  118. 5.2.2Choice of operating conditions
  119. Division
  120. 5.3Performance of the analysis
  121. 5.4Identification of peaks
  122. 5.5Evaluation of quantity
  123. 6EXPRESSION OF RESULTS
  124. Division
  125. FigureChromatogram of the waxes of an olive oil
  126. Appendix
  127. Annex V: DETERMINATION OF THE COMPOSITION AND CONTENT OF STEROLS AND TRITERPENES DIALCOHOLS BY CAPILLARY-COLUMN GAS CHROMATOGRAPHY Repealed
  128. 1SCOPE Repealed
  129. 2PRINCIPLE Repealed
  130. 3APPARATUS Repealed
  131. REAGENTS Repealed
  132. 4.1Division 4.1 Repealed
  133. 4.2Potassium hydroxide ethanolic solution, approximately 2 N. Repealed
  134. 4.3Division 4.3 Repealed
  135. 4.4Potassium hydroxide ethanolic solution, approximately 0,2 N. Repealed
  136. 4.5Division 4.5 Repealed
  137. 4.6Division 4.6 Repealed
  138. 4.7Division 4.7 Repealed
  139. 4.8Division 4.8 Repealed
  140. 4.9Division 4.9 Repealed
  141. 4.10Division 4.10 Repealed
  142. 4.11Division 4.11 Repealed
  143. 4.12Division 4.12 Repealed
  144. 4.13Division 4.13 Repealed
  145. 4.14Division 4.14 Repealed
  146. 4.15Division 4.15 Repealed
  147. 4.16Division 4.16 Repealed
  148. 4.17Division 4.17 Repealed
  149. 4.18Sample solutions of sterol trimethylsilyl ethers. Repealed
  150. 4.19Division 4.19 Repealed
  151. 4.20Division 4.20 Repealed
  152. 4.21Division 4.21 Repealed
  153. 4.22Division 4.22 Repealed
  154. 4.23Division 4.23 Repealed
  155. 4.24Division 4.24 Repealed
  156. 4.25Division 4.25 Repealed
  157. PROCEDURE Repealed
  158. 5.1Division 5.1 Repealed
  159. 5.1.1Division 5.1.1 Repealed
  160. Note 1:Division Note 1: Repealed
  161. 5.1.2Division 5.1.2 Repealed
  162. 5.1.3Division 5.1.3 Repealed
  163. Division Repealed
  164. 5.1.4Division 5.1.4 Repealed
  165. 5.1.5Division 5.1.5 Repealed
  166. Separation of the sterol and triterpene dialcohols fraction (erythrodiol + uvaol) Repealed
  167. 5.2.1Division 5.2.1 Repealed
  168. Note 3:Division Note 3: Repealed
  169. 5.2.2Division 5.2.2 Repealed
  170. Note 4:Division Note 4: Repealed
  171. 5.2.3Division 5.2.3 Repealed
  172. 5.2.4Division 5.2.4 Repealed
  173. Division Repealed
  174. 5.2.5Division 5.2.5 Repealed
  175. 5.2.6Division 5.2.6 Repealed
  176. 5.3Division 5.3 Repealed
  177. 5.3.1Division 5.3.1 Repealed
  178. Note 6:Division Note 6: Repealed
  179. 5.3.2Division 5.3.2 Repealed
  180. Note 7:Division Note 7: Repealed
  181. 5.4Division 5.4 Repealed
  182. 5.4.1Division 5.4.1 Repealed
  183. 5.4.1.1Fit the column (point 3.11) in the gas chromatograph, by attaching the inlet end to the split injector and the outlet end to the detector. Repealed
  184. 5.4.1.2If the column is being used for the first time, it is recommended that it be subjected to conditioning: passing a gentle flow of gas through the column itself, then switch on the gas chromatography unit and begin a gradual heating, up to a temperature of at least 20 °C above the operating temperature (Note 8). Hold this temperature for at least two hours, then place the entire unit in operating mode (adjustment of gas flows and splitting, ignition of the flame, connection with the computing system, adjustment of the column, detector and injector temperature, etc.) and then record the signal with a sensitivity at least two times greater than that one intended for the analysis. The course of the base line must be linear, without peaks of any kind, and must not show drift. Repealed
  185. Note 8:Division Note 8: Repealed
  186. 5.4.2Division 5.4.2 Repealed
  187. 5.4.2.1The operating conditions are as follows: Repealed
  188. Analytical procedure Repealed
  189. 5.4.3.1By using the 10 μl microsyringe, take 1 μl of hexane, draw in 0,5 μl of air and then 0,5 to 1 μl of the sample solution. Raise the plunger of the syringe further, so the needle is emptied. Push the needle through the membrane of the injector and after one to two seconds, inject rapidly, and then slowly remove the needle after around five seconds. Repealed
  190. 5.4.3.2Division 5.4.3.2 Repealed
  191. 5.4.4Peak identification Repealed
  192. 5.4.5Division 5.4.5 Repealed
  193. 5.4.5.1Division 5.4.5.1 Repealed
  194. 5.4.5.2Calculate the concentration of each individual sterol, in mg/kg of fatty material, as follows: Repealed
  195. EXPRESSION OF THE RESULTS Repealed
  196. 6.1Report individual sterol concentrations as mg/kg of fatty material and their sum as ‘total sterols’. Repealed
  197. 6.2Calculate the percentage of each individual sterol from the ratio of the relevant peak area to the total peak area for sterols: Repealed
  198. 6.3Division 6.3 Repealed
  199. 6.4Calculate the percentage of erythrodiol and uvaol: Repealed
  200. Appendix Repealed
  201. Annex VI: DETERMINATION OF ERYTHRODIOL AND UVAOL Repealed
  202. INTRODUCTION Repealed
  203. 1SCOPE Repealed
  204. 2PRINCIPLE OF THE METHOD Repealed
  205. APPARATUS Repealed
  206. 3.1Division 3.1 Repealed
  207. REAGENTS Repealed
  208. 4.1Division 4.1 Repealed
  209. 4.2Division 4.2 Repealed
  210. PROCEDURE Repealed
  211. 5.1Preparation of the unsaponifiables. Repealed
  212. Separation of erythrodiol and the sterols. Repealed
  213. 5.2.1Division 5.2.1 Repealed
  214. 5.2.2Division 5.2.2 Repealed
  215. 5.2.3Division 5.2.3 Repealed
  216. 5.2.4Division 5.2.4 Repealed
  217. 5.2.5Division 5.2.5 Repealed
  218. 5.2.6Division 5.2.6 Repealed
  219. 5.3Preparation of the trimethylsily esters Repealed
  220. 5.4Gas chromatographic analysis Repealed
  221. 6EXPRESSION OF THE RESULTS Repealed
  222. Annex VII: DETERMINATION OF THE PERCENTAGE OF 2-GLYCERYL MONOPALMITATE
  223. 1PURPOSE AND SCOPE
  224. 2PRINCIPLE
  225. APPARATUS AND MATERIALS
  226. 3.1Division 3.1
  227. 3.2Division 3.2
  228. 3.3Division 3.3
  229. 3.4Division 3.4
  230. 3.5Division 3.5
  231. 3.6Division 3.6
  232. 3.7Division 3.7
  233. 3.8Division 3.8
  234. 3.9Division 3.9
  235. 3.10Division 3.10
  236. 3.11Division 3.11
  237. 3.12Division 3.12
  238. 3.13Division 3.13
  239. 3.14Division 3.14
  240. 3.15Division 3.15
  241. 3.16Division 3.16
  242. 3.17Division 3.17
  243. 3.18Division 3.18
  244. 3.19Division 3.19
  245. REAGENTS
  246. 4.1Division 4.1
  247. 4.2Division 4.2
  248. 4.3Division 4.3
  249. 4.4Division 4.4
  250. 4.5Division 4.5
  251. 4.6Division 4.6
  252. 4.7Division 4.7
  253. 4.8Division 4.8
  254. 4.9Division 4.9
  255. 4.10Division 4.10
  256. 4.11Division 4.11
  257. 4.12Division 4.12
  258. 4.13Division 4.13
  259. 4.14Division 4.14
  260. 4.15Division 4.15
  261. 4.16Division 4.16
  262. METHOD
  263. Sample preparation
  264. 5.1.1Division 5.1.1
  265. 5.1.1.1Division 5.1.1.1
  266. 5.1.2Division 5.1.2
  267. 5.1.3Preparation of the chromatography column
  268. 5.1.4Column chromatography
  269. Hydrolysis by pancreatic lipase
  270. 5.2.1Division 5.2.1
  271. 5.2.2Division 5.2.2
  272. 5.2.3Division 5.2.3
  273. Preparation of the silanised derivatives and gas chromatography
  274. 5.3.1Division 5.3.1
  275. 5.3.2Division 5.3.2
  276. 5.3.3Division 5.3.3
  277. 5.4Gas chromatography
  278. 5.4.1Identification of the peaks
  279. 5.4.2Quantitative evaluation
  280. 6EXPRESSION OF RESULTS
  281. 7ANALYSIS REPORT
  282. Figure 2
  283. ( A )Division ( A )
  284. ( B )Division ( B )
  285. NOTES
  286. Note 1PREPARATION OF THE LIPASE
  287. Note 2MONITORING LIPASE ACTIVITY
  288. Annex VIIIDETERMINATION OF TRILINOLEIN CONTENT Repealed
  289. 1SCOPE Repealed
  290. 2FIELD OF APPLICATION Repealed
  291. 3PRINCIPLE Repealed
  292. APPARATUS Repealed
  293. 4.1Division 4.1 Repealed
  294. 4.2Division 4.2 Repealed
  295. 4.3Division 4.3 Repealed
  296. 4.4Division 4.4 Repealed
  297. 4.5Division 4.5 Repealed
  298. 5REAGENTS Repealed
  299. 5.1Division 5.1 Repealed
  300. 5.2Division 5.2 Repealed
  301. 5.3Division 5.3 Repealed
  302. 5.4Division 5.4 Repealed
  303. 5.5Division 5.5 Repealed
  304. 5.6Division 5.6 Repealed
  305. 6PREPARATION OF SAMPLES Repealed
  306. PROCEDURE Repealed
  307. 7.1Division 7.1 Repealed
  308. 8CALCULATION AND EXPRESSION OF RESULTS Repealed
  309. Note 1. Repealed
  310. Division Repealed
  311. Note 2. Examples: Repealed
  312. Division Repealed
  313. Note 3. Repealed
  314. Division Repealed
  315. Note 4. Repealed
  316. Division Repealed
  317. Note 5: Repealed
  318. Division Repealed
  319. Division Repealed
  320. Division Repealed
  321. Annex IX: SPECTROPHOTOMETRIC INVESTIGATION IN THE ULTRAVIOLET
  322. FOREWORD
  323. 1SCOPE
  324. 2PRINCIPLE OF THE METHOD
  325. EQUIPMENT
  326. 3.1Division 3.1
  327. 3.1.1Division 3.1.1
  328. 3.1.2Division 3.1.2
  329. 3.2Division 3.2
  330. 3.3Division 3.3
  331. 3.4Division 3.4
  332. 4REAGENTS
  333. PROCEDURE
  334. 5.1Division 5.1
  335. 5.2Division 5.2
  336. Division
  337. 5.3Division 5.3
  338. 5.4Division 5.4
  339. Division
  340. EXPRESSION OF THE RESULTS
  341. 6.1Division 6.1
  342. 6.2Variation of the specific extinction (ΔΚ)
  343. Annex X: DETERMINATION OF FATTY ACID METHYL ESTERS BY GAS CHROMATOGRAPHY
  344. 1SCOPE
  345. 2PRINCIPLE
  346. PREPARATION OF THE FATTY ACID METHYL ESTERS FROM OLIVE OIL AND OLIVE-POMACE OIL
  347. 1SCOPE
  348. 2FIELD OF APPLICATION
  349. METHODOLOGY
  350. Trans-esterification with methanolic solution of potassium hydroxide at room temperature
  351. 3.1.1Principle
  352. Reagents
  353. 3.1.2.1Division 3.1.2.1
  354. 3.1.2.2Division 3.1.2.2
  355. 3.1.2.3Division 3.1.2.3
  356. 3.1.2.4Division 3.1.2.4
  357. 3.1.2.5Division 3.1.2.5
  358. 3.1.2.6Division 3.1.2.6
  359. 3.1.2.7Division 3.1.2.7
  360. 3.1.2.8Division 3.1.2.8
  361. Apparatus
  362. 3.1.3.1Division 3.1.3.1
  363. 3.1.3.2Division 3.1.3.2
  364. 3.1.4Purification of oil samples
  365. 3.1.5Procedure
  366. ANALYSIS OF FATTY ACID METHYL ESTERS BY GAS CHROMATOGRAPHY
  367. 1SCOPE
  368. REAGENTS
  369. 2.1Carrier gas
  370. Note 1:Division Note 1:
  371. Auxiliary gases
  372. 2.2.1Division 2.2.1
  373. 2.2.2Division 2.2.2
  374. 2.2.3Division 2.2.3
  375. 2.3Reference standard
  376. 3APPARATUS
  377. 3.1Gas chromatograph
  378. 3.1.1Injection system
  379. 3.1.2Oven
  380. Capillary column
  381. 3.1.3.1Division 3.1.3.1
  382. 3.1.3.2Division 3.1.3.2
  383. Note 2:Division Note 2:
  384. 3.1.3.3Assembly and conditioning of the column
  385. Note 3:Division Note 3:
  386. Flame ionisation detector and converter-amplifier
  387. 3.2Syringe
  388. 3.3Data acquisition system
  389. 4PROCEDURE
  390. Test conditions
  391. 4.1.1Selection of optimum operating conditions for capillary columns
  392. 4.1.2Determination of the resolution (see Appendix A)
  393. EXPRESSION OF RESULTS
  394. 5.1Qualitative analysis
  395. Quantitative analysis
  396. 5.2.1Determination of the composition
  397. Method of calculation
  398. 5.2.2.1General case
  399. Note 4:Division Note 4:
  400. 5.2.2.2Use of correction factors
  401. Note 5:Division Note 5:
  402. Note 6:Division Note 6:
  403. 5.2.2.3Use of an internal standard
  404. 6TEST REPORT
  405. PRECISION
  406. 7.1Results of interlaboratory test
  407. 7.2Repeatability
  408. 7.3Reproducibility
  409. AAppendix A
  410. BAppendix B
  411. Annex XI: DETERMINATION OF VOLATILE HALOGENATED SOLVENTS CONTENT OF OLIVE OIL
  412. 1METHOD
  413. EQUIPMENT
  414. 2.1Division 2.1
  415. 2.2Division 2.2
  416. 2.3Division 2.3
  417. 2.4Division 2.4
  418. 2.5Division 2.5
  419. 2.6Division 2.6
  420. 2.7Division 2.7
  421. 3REAGENTS
  422. PROCEDURE
  423. 4.1Division 4.1
  424. 4.2Division 4.2
  425. 4.3Division 4.3
  426. 4.4Division 4.4
  427. Annex XII: THE INTERNATIONAL OLIVE COUNCIL’S METHOD FOR THE ORGANOLEPTIC ASSESSMENT OF VIRGIN OLIVE OIL
  428. 1PURPOSE AND SCOPE
  429. 2GENERAL BASIC VOCABULARY FOR SENSORY ANALYSIS
  430. SPECIFIC VOCABULARY
  431. 3.1Negative attributes
  432. 3.1.1Other negative attributes
  433. 3.2Positive attributes
  434. 3.3Optional terminology for labelling purposes
  435. 4GLASS FOR OIL TASTING
  436. 5TEST ROOM
  437. 6ACCESSORIES
  438. PANEL LEADER AND TASTERS
  439. 7.1Panel leader
  440. 7.1.1Deputy panel leader
  441. 7.2Tasters
  442. TEST CONDITIONS
  443. 8.1Presentation of the sample
  444. 8.2Test and sample temperature
  445. 8.3Test times
  446. 8.4Tasters: general rules of conduct
  447. 9PROCEDURE FOR THE ORGANOLEPTIC ASSESSMENT AND CLASSIFICATION OF VIRGIN OLIVE OIL
  448. Tasting technique
  449. 9.1.1The tasters shall pick up the glass, keeping it covered with the watch-glass, and shall bend it gently; they shall then rotate the glass fully in this position so as to wet the inside as much as possible. Once this stage is completed, they shall remove the watch-glass and smell the sample, taking slow deep breaths to evaluate the oil. Smelling should not exceed 30 seconds. If no conclusion has been reached during this time, they shall take a short rest before trying again.
  450. Division
  451. 9.1.2When organoleptically assessing a virgin olive oil, it is recommended that FOUR SAMPLES at the most be evaluated in each session with a maximum of three sessions per day, to avoid the contrast effect that could be produced by immediately tasting other samples.
  452. 9.2Use of the profile sheet by tasters
  453. 9.3Use of the data by the panel leaders
  454. 9.4Classification of the oil
  455. Note 1:Division Note 1:
  456. 9.5Criteria for the acceptance and rejection of duplicates
  457. Appendix
  458. Annex XIII: NEUTRALIZATION AND DECOLORIZATION OF OLIVE OIL IN THE LABORATORY Repealed
  459. NEUTRALIZATION AND DECOLORIZATION OF OLIVE OIL IN THE LABORATORY Repealed
  460. Neutralization of the oil Repealed
  461. 1.1.1Apparatus Repealed
  462. 1.1.2Reagents Repealed
  463. Procedure Repealed
  464. (a)Oils with a free fatty acid content, expressed as oleic acid, of less than 30 % Repealed
  465. (b)Oils with a free fatty acid content expressed as oleic acid exceeding 30 %. Repealed
  466. Decolorization of neutralized oil Repealed
  467. 1.2.1Apparatus Repealed
  468. 1.2.2Procedure Repealed
  469. Annex XIV: ADDITIONAL NOTES 2, 3 AND 4 TO CHAPTER 15 OF THE COMBINED NOMENCLATURE Repealed
  470. Repealed
  471. ADivision A Repealed
  472. BDivision B Repealed
  473. IDivision I Repealed
  474. IIDivision II Repealed
  475. CDivision C Repealed
  476. DDivision D Repealed
  477. EDivision E Repealed
  478. 3Division 3 Repealed
  479. 4Division 4 Repealed
  480. Annex XV
  481. OIL CONTENT OF OLIVE RESIDUE
  482. 1.1Apparatus
  483. 1.2Reagent
  484. PROCEDURE
  485. 2.1Preparation of the test sample
  486. 2.2Test portion
  487. 2.3Preparation of the extraction thimble
  488. 2.4Peliminary drying
  489. 2.5Preparation of the round-bottomed flask
  490. 2.6Initial extraction
  491. 2.7Second extraction
  492. 2.8Removal of solvent and weighing of extract
  493. EXPRESSION OF RESULTS
  494. 3.1Method of calculation and formula
  495. 3.2Repeatability
  496. Annex XVI: DETERMINATION OF IODINE VALUE
  497. 1SCOPE
  498. 2DEFINITION
  499. 2.1Division 2.1
  500. 3PRINCIPLE
  501. 4REAGENTS
  502. 4.1Division 4.1
  503. 4.2Division 4.2
  504. 4.3Division 4.3
  505. 4.4Division 4.4
  506. 4.5Division 4.5
  507. 4.6Division 4.6
  508. 5APPARATUS
  509. 5.1Division 5.1
  510. 5.2Division 5.2
  511. 6PREPARATION OF THE TEST SAMPLE
  512. PROCEDURE
  513. 7.1Division 7.1
  514. 7.2Division 7.2
  515. Note:
  516. Division
  517. 7.3Division 7.3
  518. 8EXPRESSION OF RESULTS
  519. Annex XVIIMETHOD FOR THE DETERMINATION OF STIGMASTADIENES IN VEGETABLE OILS
  520. 1PURPOSE
  521. 2SCOPE
  522. 3PRINCIPLE
  523. APPARATUS
  524. 4.1Division 4.1
  525. 4.2Division 4.2
  526. 4.3Division 4.3
  527. 4.4Division 4.4
  528. 4.5Division 4.5
  529. 4.6Division 4.6
  530. 4.7Division 4.7
  531. Note 1:
  532. Division
  533. 4.8Division 4.8
  534. 4.9Division 4.9
  535. 4.10Division 4.10
  536. 5REAGENTS
  537. 5.1Division 5.1
  538. 5.2Division 5.2
  539. 5.3Division 5.3
  540. 5.4Division 5.4
  541. Note 3:
  542. Division
  543. 5.5Division 5.5
  544. Note 4:
  545. Division
  546. 5.6Division 5.6
  547. 5.7Division 5.7
  548. Note 5:
  549. Division
  550. 5.8Division 5.8
  551. 5.9Division 5.9
  552. 5.10Division 5.10
  553. PROCEDURE
  554. Preparation of unsaponifiable matter
  555. 6.1.1Division 6.1.1
  556. Note 6:
  557. Division
  558. 6.1.2Division 6.1.2
  559. 6.1.3Division 6.1.3
  560. Separation of steroidal hydrocarbon fraction
  561. 6.2.1Division 6.2.1
  562. Note 7:
  563. Division
  564. 6.2.2Division 6.2.2
  565. Note 8:
  566. Division
  567. Gas chromatography
  568. 6.3.1Division 6.3.1
  569. 6.3.2Division 6.3.2
  570. Note 9:
  571. Division
  572. 6.3.3Division 6.3.3
  573. Figure 1
  574. Division
  575. Annex XVIIIDETERMINATION OF THE DIFFERENCE BETWEEN ACTUAL AND THEORETICAL CONTENT OF TRIACYLGLYCEROLS WITH ECN 42
  576. 1SCOPE
  577. 2FIELD OF APPLICATION
  578. 3PRINCIPLE
  579. 4METHOD
  580. Apparatus
  581. 4.1.1Division 4.1.1
  582. 4.1.2Division 4.1.2
  583. 4.1.3Division 4.1.3
  584. 4.1.4Division 4.1.4
  585. 4.1.5Division 4.1.5
  586. 4.1.6Division 4.1.6
  587. 4.1.7Division 4.1.7
  588. 4.1.8Division 4.1.8
  589. 4.1.9Division 4.1.9
  590. 4.1.10Division 4.1.10
  591. 4.1.11Division 4.1.11
  592. 4.1.12Division 4.1.12
  593. 4.1.13Division 4.1.13
  594. 4.1.14Division 4.1.14
  595. 4.1.15Division 4.1.15
  596. 4.2Reagents
  597. 4.2.1Division 4.2.1
  598. 4.2.2Division 4.2.2
  599. 4.2.3Division 4.2.3
  600. 4.2.4Division 4.2.4
  601. 4.2.5Division 4.2.5
  602. 4.2.6Division 4.2.6
  603. 4.2.7Division 4.2.7
  604. 4.2.8Division 4.2.8
  605. 4.2.9Division 4.2.9
  606. 4.2.10Division 4.2.10
  607. 4.2.11Division 4.2.11
  608. 4.2.12Division 4.2.12
  609. 4.3Sample preparation
  610. 4.3.1Chromatographic column preparation
  611. 4.3.2Column chromatography
  612. 4.3.3SPE purification
  613. HPLC analysis
  614. 4.4.1Preparation of the samples for chromatographic analysis
  615. 4.4.2Procedure
  616. 4.4.3Calculation and expression of results
  617. Calculation of triacylglycerols composition (moles %) from fatty acid composition data (area %)
  618. 4.5.1Determination of fatty acid composition
  619. 4.5.2Fatty acids for calculation
  620. 4.5.3Conversion of area % into moles for all fatty acids (1)
  621. 4.5.4Normalisation of fatty acid moles to 100 % (2)
  622. 4.5.5Calculation of the fatty acid composition in 2- and 1, 3- positions of TAGs
  623. 4.5.5.1Saturated fatty acids in 2-position [P(2) and S(2)] (4):
  624. 4.5.5.2Unsaturated fatty acids in 2-position [Po(2), O(2), L(2) and Ln(2)] (5):
  625. 4.5.5.3Fatty acids in 1,3-positions [P(1,3), S(1,3), Po(1,3), O(1,3), L(1,3) and Ln(1,3)] (6):
  626. Calculation of triacylglycerols
  627. 4.5.6.1TAGs with one fatty acid (AAA, here LLL, PoPoPo) (7)
  628. 4.5.6.2TAGs with two fatty acids (AAB, here PoPoL, PoLL) (8)
  629. 4.5.6.3TAGs with three different fatty acids (ABC, here OLLn, PLLn, PoOLn, PPoLn) (9)
  630. 4.5.6.4Triacylglycerols with ECN42
  631. 5EVALUATION OF THE RESULTS
  632. EXAMPLE (THE NUMBERS REFER TO THE SECTIONS IN THE TEXT OF THE METHOD)
  633. — 4.5.1Calculation of moles % fatty acids from GLC data (normalised area %)
  634. — 4.5.3Conversion of area % into moles for all fatty acids (see formula (1))
  635. — 4.5.4Normalisation of fatty acid moles to 100 % (see formula (2))
  636. Calculation of the fatty acid composition in 2- and 1,3-positions of the TAGs
  637. — 4.5.5.1Saturated fatty acids in 2-position [P(2) and S(2)] (see formula (4))
  638. — 4.5.5.2Unsaturated fatty acids in 2-position [Po(1,3), O(1,3), L(1,3) and Ln(1,3)] (see formula (5))
  639. — 4.5.5.3Fatty acids in 1,3-positions [P(1,3), S(1,3), Po(1,3), O(1,3), L(1,3) and Ln(1,3)] (see formula (6))
  640. — 4.5.6Calculation of triacylglycerols
  641. — 4.5.6.1TAGs with one fatty acid (LLL, PoPoPo) (see formula (7))
  642. — 4.5.6.2TAGs with two fatty acids (PoLL, SLnLn, PoPoL) (see formula (8))
  643. — 4.5.6.3TAGs with three different fatty acids (PoPLn, OLLn, PLLn, PoOLn) See formula (9)
  644. Division
  645. Division
  646. Division
  647. Division
  648. Annex XIX
  649. DETERMINATION OF THE STEROL COMPOSITION AND CONTENT AND ALCOHOLIC COMPOUNDS BY CAPILLARY GAS CHROMATOGRAPHY
  650. 1SCOPE
  651. 2PRINCIPLE
  652. Part 1: PREPARATION OF THE UNSAPONIFIABLE MATTER
  653. 1SCOPE
  654. 2PRINCIPLE
  655. 3APPARATUS
  656. 4REAGENTS
  657. 5PROCEDURE
  658. Note 1:Division Note 1:
  659. Note 2:Division Note 2:
  660. Part 2: SEPARATION OF THE ALCOHOLIC COMPOUNDS FRACTIONS
  661. 1SCOPE
  662. 2PRINCIPLE
  663. 3APPARATUS
  664. 4REAGENTS
  665. 5REFERENCE METHOD: SEPARATION OF THE ALCOHOLIC COMPOUNDS BY BASIC THIN-LAYER CHROMATOGRAPHY (TLC) PLATE
  666. Note 3:Division Note 3:
  667. Note 4:Division Note 4:
  668. 6SEPARATION OF THE ALCOHOLIC FRACTION BY HPLC
  669. Note 5:Division Note 5:
  670. Part 3: GAS CHROMATOGRAPHIC ANALYSIS OF THE ALCOHOLIC COMPOUNDS FRACTIONS
  671. 1SCOPE
  672. 2PRINCIPLE
  673. 3APPARATUS
  674. 4REAGENTS
  675. 5PREPARATION OF THE TRIMETHYLSILYL ETHERS
  676. Note 6:Division Note 6:
  677. Note 7:Division Note 7:
  678. GAS CHROMATOGRAPHIC ANALYSIS
  679. 6.1Preliminary operations, capillary column conditioning
  680. Note 8:Division Note 8:
  681. 6.2Operating conditions
  682. 6.2.1Aliphatic alcohols
  683. 6.2.2Sterol and triterpenic dialcohols
  684. 6.3Analytical procedure
  685. 6.4Peak identification
  686. 6.5Quantitative evaluation
  687. 7EXPRESSION OF THE RESULTS
  688. Appendix
  689. Annex XXMethod for the determination of the content of waxes, fatty acid methyl esters and fatty acid ethyl esters by capillary gas chromatography
  690. 1PURPOSE
  691. 2PRINCIPLE
  692. APPARATUS
  693. 3.1Division 3.1
  694. 3.2Division 3.2
  695. 3.3Division 3.3
  696. 3.3.1Division 3.3.1
  697. 3.3.2Division 3.3.2
  698. 3.3.3Division 3.3.3
  699. 3.3.4Division 3.3.4
  700. Note 1:Division Note 1:
  701. 3.3.5Division 3.3.5
  702. Note 2:Division Note 2:
  703. 3.4Division 3.4
  704. 3.5Division 3.5
  705. 3.6Division 3.6
  706. 3.7Division 3.7
  707. 3.8Division 3.8
  708. 3.9Division 3.9
  709. REAGENTS
  710. 4.1Division 4.1
  711. 4.2Division 4.2
  712. 4.3Ethyl ether, chromatography grade
  713. 4.4Division 4.4
  714. 4.5Division 4.5
  715. Note 3:Division Note 3:
  716. 4.6Division 4.6
  717. 4.7Division 4.7
  718. 4.8Division 4.8
  719. WARNING
  720. 4.9Auxiliary gases :
  721. WARNING
  722. PROCEDURE
  723. 5.1Preparation of the chromatography column
  724. Note 4:Division Note 4:
  725. Note 5:100 μl of Sudan I dye at 1 % in the elution mixture can be added to the sample solution to check visually that the waxes are eluted properly.
  726. Gas chromatography analysis
  727. 5.2.1Preliminary procedure
  728. 5.2.2Choice of operating conditions for waxes and methyl and ethyl esters (Note 6).
  729. Note 6:Division Note 6:
  730. 5.3Performance of the analysis
  731. 5.4Peak identification
  732. 5.5Quantitative analysis of the waxes
  733. 5.5.1Quantitative analysis of the methyl and ethyl esters
  734. 6EXPRESSION OF RESULTS
  735. Note 7:Division Note 7:
  736. AAppendix A
  737. Annex XXa: METHOD FOR THE DETECTION OF EXTRANEOUS OILS IN OLIVE OILS Repealed
  738. 1SCOPE Repealed
  739. 2PRINCIPLE Repealed
  740. MATERIAL AND REAGENTS Repealed
  741. Oil purification Repealed
  742. 3.1.1Division 3.1.1 Repealed
  743. 3.1.2Division 3.1.2 Repealed
  744. 3.1.3Division 3.1.3 Repealed
  745. 3.1.4Division 3.1.4 Repealed
  746. 3.1.5Division 3.1.5 Repealed
  747. 3.1.6Division 3.1.6 Repealed
  748. 3.1.7Division 3.1.7 Repealed
  749. HPLC analysis of triacylglycerols Repealed
  750. 3.2.1Division 3.2.1 Repealed
  751. 3.2.2Division 3.2.2 Repealed
  752. 3.2.3Division 3.2.3 Repealed
  753. 3.3Preparation of fatty acid methyl esters Repealed
  754. 3.3.1Division 3.3.1 Repealed
  755. 3.3.2Division 3.3.2 Repealed
  756. 3.3.3Division 3.3.3 Repealed
  757. 3.3.4Division 3.3.4 Repealed
  758. 3.4GC analysis of FAMEs Repealed
  759. 3.4.1Division 3.4.1 Repealed
  760. 3.4.2Division 3.4.2 Repealed
  761. 3.4.3Division 3.4.3 Repealed
  762. 3.4.4Division 3.4.4 Repealed
  763. 3.4.5Division 3.4.5 Repealed
  764. APPARATUS Repealed
  765. 4.1Division 4.1 Repealed
  766. 4.2Division 4.2 Repealed
  767. 4.3HPLC equipment composed of: Repealed
  768. 4.4Capillary gas chromatography equipment described in Annex X A, provided with: Repealed
  769. 4.5Division 4.5 Repealed
  770. ANALYTICAL PROCEDURE Repealed
  771. 5.1Oil purification Repealed
  772. Division Repealed
  773. 5.2HPLC analysis of triacylglycerols Repealed
  774. Division Repealed
  775. 5.3Preparation of fatty acid methyl esters Repealed
  776. 5.4GC analysis of fatty acid methyl esters Repealed
  777. INTEGRATION OF CHROMATOGRAPHIC PEAKS Repealed
  778. 6.1HPLC chromatogram Repealed
  779. 6.2GC chromatogram Repealed
  780. 7DETECTION OF EXTRANEOUS OILS IN OLIVE OILS Repealed
  781. Annex XXIAnnex XXI