{
  "url": "https://openlegislation.uk/eu-regulation-2016-635/annex",
  "json_url": "https://openlegislation.uk/eu-regulation-2016-635/annex.json",
  "legislation": "eur/2016/635",
  "legislation_title": "Commission Implementing Regulation (EU) 2016/635 of 22 April 2016 amending the Annex to Regulation (EC) No 2870/2000 as regards certain reference methods for the analysis of spirit drinks",
  "legislation_url": "https://openlegislation.uk/eu-regulation-2016-635",
  "path": "annex",
  "kind": "annex",
  "number": null,
  "heading": null,
  "text": "The Annex to Regulation (EC) No 2870/2000 is amended as follows:\n(1) The table of contents is amended as follows:\n(a) in points III.3 and VIII, the term ‘(p.m.)’ is deleted;\n(b) the following point is added:\n‘X.\nDetermination of wood compounds: furfural, 5-hydroxymethylfurfural, 5-methylfurfural, vanillin, syringaldehyde, coniferaldehyde, sinapaldehyde, gallic acid, ellagic acid, vanillic acid, syringic acid and scopoletin.’\n(2) In Chapter III the following part is added:\n‘III.3.\nDETERMINATION OF VOLATILE ACIDITY OF SPIRIT DRINKS\n1.\nScope\nThe method has been validated in an interlaboratory study for rum, brandy, marc and fruit spirits, at levels ranging from 30 mg/l to 641 mg/l.\n2.\nNormative references\nISO 3696: 1987 Water for analytical use — Specifications and test methods.\n3.\nDefinitions\n3.1.\nVolatile acidity is calculated by deducting the fixed acidity from the total acidity.\n3.2.\nTotal acidity is the sum of titratable acidities.\n3.3.\nFixed acidity is the acidity of the residue left after evaporating the spirit to dryness.\n4.\nPrinciple\nThe total acidity and fixed acidity are determined by titration or by potentiometry.\n5.\nReagents and materials\nDuring the analysis, unless otherwise stated, use only reagents of recognised analytical grade and water of at least grade 3 as defined in ISO 3696:1987.\n5.1.\n0,01 M sodium hydroxide solution (NaOH)\n5.2.\nMixed indicator solution:\nWeigh 0,1 g of indigo carmine and 0,1 g of phenol red.\nDissolve in 40 ml water and make up to 100 ml with ethanol.\n6.\nApparatus and equipment\nIndirect laboratory apparatus, grade A glassware and the following:\n6.1. Water pump\n6.2. Rotary evaporator or ultrasonic bath\n6.3. Equipment for potentiometric titration (optional).\n7.\nSampling and samples\nSamples are stored at room temperature prior to analysis.\n8.\nProcedure\n8.1.\nTotal acidity\n8.1.1.\nPreparation of sample\nThe spirit is irradiated with ultrasonic (ultrasonication) or stirred two minutes under a vacuum to rid it of carbon dioxide if required.\n8.1.2.\nTitration\nPipette 25 ml of the spirit into a 500 ml Erlenmeyer flask.\nAdd about 200 ml of cooled boiled distilled water (prepared fresh daily) and 2-6 drops of the mixed indicator solution (5.2).\nTitrate with the 0,01 M sodium hydroxide solution (5.1) until the yellow-green colour changes to violet in the case of colourless spirits, the yellow-brown colour to red-brown in the case of brown-coloured spirits respectively.\nThe titration may also be carried out by potentiometry, to pH 7,5.\nLet n1 ml be the volume of the 0,01 M sodium hydroxide solution added.\n8.1.3.\nCalculation\nThe total acidity (TA) expressed in milliequivalents per l of spirit is equal to 0,4 × n1.\nThe total acidity (TA′) expressed in mg of acetic acid per l of spirit is equal to 24 × n1.\n8.2.\nFixed acidity\n8.2.1.\nPreparation of sample\nEvaporate 25 ml of the spirit to dryness:\nPipette 25 ml of the spirit into a flat-bottomed cylindrical evaporating dish 55 mm in diameter. During the first hour of evaporation the evaporating dish is placed on the lid of a boiling water bath so that the liquid will not boil, as this could lead to losses through splattering.\nComplete the drying by placing the evaporating dish in a drying oven at 105 °C for two hours. Allow the evaporating dish to cool in a desiccator.\n8.2.2.\nTitration\nDissolve the residue left after evaporating with cooled boiled distilled water (prepared fresh daily) and make up to a volume to circa 100 ml and add 2-6 drops of the mixed indicator solution (5.2).\nTitrate with the 0,01 M sodium hydroxide solution (5.1).\nThe titration may also be carried out by potentiometry, to pH 7,5.\nLet n2 ml be the volume of the 0,01 M sodium hydroxide solution added.\n8.2.3.\nCalculation\nThe fixed acidity (FA) expressed in milliequivalents per l of spirit is equal to 0,4 × n2.\nThe fixed acidity (FA) expressed in mg of acetic acid per l of spirit is equal to 24 × n2.\n9.\nCalculation of volatile acidity\n9.1.\nExpression in milliequivalents per l:\nLet:\nTA total acidity in milliequivalents per l\nFA fixed acidity in milliequivalents per l\nVolatile acidity, VA, in milliequivalents per l is equal to:\nTA – FA.\n9.2.\nExpression in mg of acetic acid per l:\nLet:\nTA′ total acidity in mg of acetic acid per l\nFA′ fixed acidity in mg of acetic acid per l\nVolatile acidity, VA, in mg of acetic acid per l is equal to:\nTA′ – FA′.\n9.3.\nExpression in g of acetic acid per hl of pure 100 % vol. alcohol is equal to: TA′ − FA′ A × 10\nwhere A is the alcoholic strength by volume of the spirit drink.\n10.\nMethod performance characteristics (Precision)\n10.1.\nStatistical results of the interlaboratory test\nThe following data were obtained from an international method performance study carried out to internationally agreed procedures (1) (2).\nYear of interlaboratory test\n2000\nNumber of laboratories\n18\nNumber of samples\n6\nSamples\nA\nB\nC\nD\nE\nF\nNumber of laboratories retained after eliminating outliers\n16\n18\n18\n14\n18\n18\nNumber of outliers (laboratories)\n2\n4\nNumber of accepted results\n32\n36\n36\n28\n36\n36\nMean value x – (mg/L)\n272*\n241*\n30\n591*\n641*\n46\n107\n492\nRepeatability standard deviation, sr (mg/l)\n8,0\n3,6\n15,0\n3,7\n6,7\n8,5\nRepeatability relative standard deviation, RSDr (%)\n3,1\n11,8\n2,4\n8,0\n6,2\n1,7\nRepeatability limit, r (mg/l)\n23\n10\n42\n10\n19\n24\nReproducibility standard deviation, sR (mg/l)\n8,5\n8,4\n25,0\n4,55\n13,4\n24,4\nReproducibility relative standard deviation, RSDR (%)\n3,3\n27,8\n4,1\n9,9\n12,5\n5,0\nReproducibility limit, R (mg/l)\n24\n23\n70\n13\n38\n68\nSample types:\nA Plum spirit; split level *\nB Rum I; blind duplicates\nC Rum II; split level *\nD Slivovitz; blind duplicates\nE Brandy; blind duplicates\nF Marc spirit; blind duplicates.\n(1)\n“Protocol for the design, conduct and interpretation of method-performance studies”, Horwitz, W. (1995) Pure and Applied Chemistry, 67, 332-343.\n(2)\nHorwitz, W. (1982) Analytical Chemistry, 54, 67A-76A.’\n(3) The following Chapter VIII is inserted:\n‘VIII.\nTOTAL SUGARS\n1.\nScope\nThe HPLC–RI method is applicable for the determination of total sugars (expressed as invert sugar) in spirit drinks, with the exclusion of liqueurs containing egg and milk products.\nThe method has been validated in an interlaboratory study for pastis, distilled anis, cherry liqueur, crème de (followed by the name of a fruit or the raw material used) and crème de cassis, at levels ranging from 10,86 g/l to 509,7 g/l. However, linearity of the instrument response was proven for the concentration range 2,5 g/l to 20,0 g/l.\nThis method is not intended for determining low levels of sugars.\n2.\nNormative references\nISO 3696:1987 Waters for analytical use — Specifications and test methods.\n3.\nPrinciple\nHigh-performance liquid chromatography assays of sugar solutions, in order to determine their glucose, fructose, sucrose, maltose and lactose concentrations.\nThis method uses an alkylamine stationary phase and differential refractometry detection and is given as an example. The use of anion exchange resins as stationary phase would also be possible.\n4.\nReagents and materials\n4.1.\nGlucose (CAS 50-99-7), at least 99 % pure.\n4.2.\nFructose (CAS 57-48-7), at least 99 % pure.\n4.3.\nSucrose (CAS 57-50-1), at least 99 % pure.\n4.4.\nLactose (CAS 5965-66-2), at least 99 % pure.\n4.5.\nMaltose monohydrate (CAS 6363-53-7), at least 99 % pure.\n4.6.\nPure acetonitrile (CAS 75-05-8) for HPLC analysis.\n4.7.\nDistilled or demineralised water, preferably microfiltered.\n4.8.\nSolvents (example)\nThe elution solvent is composed of:\n75 parts by volume of acetonitrile (4.6),\n25 parts by volume of distilled water (4.7).\nPass helium through at a slow rate for 5-10 minutes prior to use to degas.\nIf the water being used has not been microfiltered, the solvent should be filtered with a filter for organic solvents with a pore size less than or equal to 0,45 μm.\n4.9.\nEthanol absolute (CAS 64-17-5).\n4.10.\nEthanol solution (5 %, v/v).\n4.11.\nPreparation of stock standard solution (20 g/l)\nWeigh 2 g each of the sugars to be analysed (4.1 to 4.5), transfer them without loss to a 100 ml volumetric flask. (NB 2,11 g of maltose monohydrate is equivalent to 2 g of maltose).\nAdjust to 100 ml with a 5 % vol. alcohol solution (4.10), shake and store at around + 4 °C. Prepare a new stock solution once a week.\n4.12.\nPreparation of working standard solutions (2,5, 5,0, 7,5, 10,0 and 20,0 g/L)\nDilute the stock solution, 20 g/l (4.11) appropriately with a 5 % vol. alcohol solution (4.10) to give five working standards of 2,5, 5,0, 7,5, 10,0 and 20,0 g/l. Filter with a filter of a pore size less than or equal to 0,45 μm (5.3).\n5.\nApparatus and Equipment\n5.1.\nHPLC system capable of achieving baseline resolution of all of the sugars.\n5.1.1.\nHigh-performance liquid chromatograph with a six-way injection valve fitted with a 10 μl loop or any other device, whether automatic or manual, for the reliable injection of microvolumes.\n5.1.2.\nPumping system enabling one to achieve and maintain a constant or programmed rate of flow with great precision.\n5.1.3.\nDifferential refractometer.\n5.1.4.\nComputational integrator or recorder, the performance of which is compatible with the rest of the set-up.\n5.1.5.\nPre-column:\nIt is recommended that a suitable pre-column is attached to the analytical column.\n5.1.6.\nColumn (example):\nMaterial:\nstainless steel or glass.\nInternal diameter:\n2-5 mm.\nLength:\n100-250 mm (depending on the packing particle size), for example, 250 mm if the particles are 5 μm in diameter.\nStationary phase:\nalkylamine functional groups bonded to silica, maximum particle size 5 μm.\n5.1.7.\nChromatography conditions (example):\nElution solvent (4.8), flow rate: 1 ml/minute.\nDetection: Differential refractometry.\nTo make certain that the detector is perfectly stable, it should be switched on a few hours before use. The reference cell must be filled with the elution solvent.\n5.2.\nAnalytical balance accurate to 0,1 mg.\n5.3.\nFiltration set-up for small volumes using a 0,45 μm micromembrane.\n6.\nSample storage\nOn receipt, samples are to be stored at room temperature prior to analysis.\n7.\nProcedure\n7.1.\nPART A: Sample preparation\n7.1.1.\nShake the sample.\n7.1.2.\nFilter the sample through a filter with a pore size less than or equal to 0,45 μm (5.3).\n7.2.\nPART B: HPLC\n7.2.1.\nDetermination\nInject 10 μl of the standard solutions (4.12) and samples (7.1.2). Perform the analysis under suitable chromatography conditions, for example those described above.\n7.2.2.\nShould any peak of a sample have a greater area (or height) than the corresponding peak in the most concentrated standard, then the sample should be diluted with distilled water and reanalysed.\n8.\nCalculation\nCompare the two chromatograms obtained for the standard solution and spirit. Identify the peaks by their retention times. Measure their areas (or heights) to calculate the concentrations by the external standard method. Take into account any dilutions made to the sample.\nThe final result is the sum of sucrose, maltose, lactose, glucose and fructose, expressed as invert sugar in g/l.\nInvert sugar is calculated as the sum of all monosaccharides and reducing disaccharides present, plus the stoichiometric amount of glucose and fructose calculated from the sucrose present.\nInvert sugar (g/l) glucose (g/l) + fructose (g/l) + maltose (g/l) + lactose (g/l) + (sucrose (g/l) × 1,05).\n1,05 (molecular weight of fructose + molecular weight of glucose)/molecular weight of sucrose.\n9.\nMethod performance characteristics (precision)\n9.1.\nStatistical results of the interlaboratory test\nThe following data were obtained from an international method performance study carried out to internationally agreed procedures (1) (2).\nYear of interlaboratory test\n2000\nNumber of laboratories\n24\nNumber of samples\n8\n(1)\n“Protocol for the design, conduct and interpretation of method-performance studies”, Horwitz, W. (1995) Pure and Applied Chemistry, 67, 332-343.\n(2)\nHorwitz, W. (1982) Analytical Chemistry, 54, 67A-76A.\nTable 1\nFructose, glucose, maltose\nAnalyte\nFructose\nGlucose\nMaltose\nSamples (× 2)\nCrème de Cassis\nStandard (50 g/l)\nAniseed-flavoured spirit drink\nCrème de Cassis\nStandard (50 g/l)\nAniseed-flavoured spirit drink\nStandard (10 g/l)\nMean value (g/l)\n92,78\n50,61\n15,62\n93,16\n50,06\n15,81\n9,32\nNo of labs without outliers\n21\n22\n21\n23\n19\n21\n22\nRepeatability standard deviation, sr, (g/l)\n2,34\n2,12\n0,43\n3,47\n1,01\n0,48\n0,54\nRepeatability relative standard deviation, RSDr (%)\n2,53\n4,2\n2,76\n3,72\n2,03\n3,02\n5,77\nRepeatability limit, r (g/l)\n(r = 2,8 × sr)\n6,56\n5,95\n1,21\n9,71\n2,84\n1,34\n1,51\nReproducibility standard deviation, sR (g/l)\n7,72\n3,13\n0,84\n9,99\n2,7\n0,88\n1,4\nReproducibility relative standard deviation, RSDR (%)\n8,32\n6,18\n5,37\n10,72\n5,4\n5,54\n15,06\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n21,62\n8,76\n2,35\n27,97\n7,57\n2,45\n3,93\nTable 2\nSucrose\nsplit level.\nAnalyte\nSucrose\nSamples\nPastis\nOuzo\nCherry liqueur\nCrème de Menthe\nCrème de Cassis\nStandard (100 g/l)\nMean value (g/l)\n10,83\n29,2\n19,7\n103,33\n349,96\n319,84\n99,83\nNo of labs without outliers\n19\n19\n20\n18\n18\n18\nRepeatability standard deviation, sr (g/l)\n0,09\n0,75\n2,17\n5,99\n4,31\n1,25\nRepeatability relative standard deviation, RSDr (%)\n0,81\n3,07\n2,1\n1,71\n1,35\n1,25\nRepeatability limit, r (g/l)\n(r = 2,8 × sr)\n0,25\n2,1\n6,07\n16,76\n12,06\n3,49\nReproducibility standard deviation, sR (g/l)\n0,79\n0,92\n4,18\n9,94\n16,11\n4,63\nReproducibility relative standard deviation, RSDR (%)\n7,31\n3,76\n4,05\n2,84\n5,04\n4,64\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n2,22\n2,57\n11,7\n27,84\n45,12\n12,97\nTable 3\nTotal Sugars\n(Note: this data was calculated for total sugars, not invert sugar as defined in Section 8 above.)\nsplit level.\nSamples\nPastis\nOuzo\nAniseed-flavoured spirit drink\nCherry liqueur\nCrème de Menthe\nCrème de Cassis\nStandard (220 g/l)\nMean value (g/l)\n10,86\n29,2\n19,7\n31,59\n103,33\n349,73\n509,69\n218,78\nNo of Labs without outliers\n20\n19\n20\n20\n18\n18\n19\nRepeatability standard deviation, sr (g/l)\n0,13\n0,75\n0,77\n2,17\n5,89\n5,59\n2,71\nRepeatability relative standard deviation, RSDr (%)\n1,16\n3,07\n2,45\n2,1\n1,69\n1,1\n1,24\nRepeatability limit, r (g/l)\n(r = 2,8 × sr)\n0,35\n2,1\n2,17\n6,07\n16,5\n15,65\n7,59\nReproducibility standard deviation sR (g/l)\n0,79\n0,92\n1,51\n4,18\n9,98\n14,81\n8,53\nReproducibility relative standard deviation, RSDR (%)\n7,25\n3,76\n4,79\n4,04\n2,85\n2,91\n3,9\nReproducibility limit R (g/l)\n(R = 2,8 × sR)\n2,21\n2,57\n4,24\n11,7\n27,94\n41,48\n23,89\n’\n(4) The following Chapter X is added:\n‘X.\nDETERMINATION 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\n1.\nScope\nThe method pertains to the determination of furfural, 5-hydroxymethylfurfural, 5-methylfurfural, vanillin, syringaldehyde, coniferaldehyde, sinapaldehyde, gallic acid, ellagic acid, vanillic acid, syringic acid and scopoletin, by high-performance liquid chromatography.\n2.\nNormative reference\nAnalytical method recognised by the General Assembly of the International Organisation of Vine and Wine (OIV) and published by OIV under the reference OIV-MA-BS-16: R2009.\n3.\nPrinciple\nDetermination by high-performance liquid chromatography (HPLC), with detection by ultraviolet spectrophotometry at several wavelengths and by spectrofluorimetry.\n4.\nReagents\nThe reagents must be of analytical quality. The water used must be distilled water or water of at least equivalent purity. It is preferable to use microfiltered water with a resistivity of 18,2 M Ω.cm.\n4.1.\n96 % vol. alcohol.\n4.2.\nHPLC-quality methanol (Solvent B).\n4.3.\nAcetic acid diluted to 0,5 % vol. (Solvent A).\n4.4.\nMobile phases: (given as an example only).\nSolvent A (0,5 % acetic acid) and solvent B (pure methanol). Filter through a membrane (porosity 0,45 μm). Degas in an ultrasonic bath, if necessary.\n4.5.\nReference standards of 99 % minimum purity: furfural, 5-hydroxymethyl furfural, 5-methylfurfural, vanillin, syringaldehyde, coniferaldehyde, sinapaldehyde, gallic acid, ellagic acid, vanillic acid, syringic acid and scopoletin.\n4.6.\nReference solution: the standard substances are dissolved in a 50 % vol. aqueous-alcoholic solution. The final concentrations in the reference solution should be of the order of:\nfurfural: 5 mg/l; 5-hydroxymethyl furfural: 10 mg/l; 5-methylfurfural 2 mg/l; vanillin: 5 mg/l; syringaldehyde: 10 mg/l; coniferaldehyde: 5 mg/l; sinapaldehyde: 5 mg/l; gallic acid: 10 mg/l; ellagic acid: 10 mg/l; vanillic acid: 5 mg/l; syringic acid: 5 mg/l; scopoletin: 0,5 mg/l.\n5.\nApparatus\nStandard laboratory apparatus\n5.1.\nA high-performance liquid chromatograph capable of functioning in binary gradient mode and equipped with:\n5.1.1. A spectrophotometric detector capable of measuring at wavelengths from 260 to 340 nm. It is however preferable to work with a multiple wavelength detector with a diode array or similar, in order to confirm the purity of the peaks.\n5.1.2. A spectrofluorimetric detector — excitation wavelength: 354 nm, emission wavelength: 446 nm (for the trace determination of scopoletin; which is also detectable at 313 nm by spectrophotometry).\n5.1.3. An injection device capable of introducing 10 or 20 μl (for example) of the test sample.\n5.1.4. A high-performance liquid chromatography column, RP C18 type, 5 μm maximum particle size.\n5.2.\nSyringes for HPLC.\n5.3.\nDevice for membrane-filtration of small volumes.\n5.4.\nIntegrator-computer or recorder with performance compatible with the entire apparatus, and in particular, it must have several acquisition channels.\n6.\nProcedure\n6.1.\nPreparation of the solution to be injected\nThe reference solution and the spirit drink are filtered, if necessary, through a membrane with a maximum pore diameter of 0,45 μm.\n6.2.\nChromatographic operating conditions: carry out the analysis at ambient temperature by means of the equipment described in (5.1) and using the mobile phases (4.4) with a flow of approximately 0,6 ml per minute following the gradient below (given as an example only)\nTime: 0 min 50 min 70 min 90 min\nsolvent A (water-acid): 100 % 60 % 100 % 100 %\nsolvent B (methanol): 0 % 40 % 0 % 0 %\nNote that in certain cases this gradient should be modified to avoid co-elutions.\n6.3.\nDetermination\n6.3.1.\nInject the reference standards separately, then mixed.\nAdapt the operating conditions so that the resolution factors of the peaks of all the compounds are equal to at least 1.\n6.3.2.\nInject the sample as prepared in 6.1.\n6.3.3.\nMeasure the area of the peaks in the reference solution and the spirit drink and calculate the concentrations.\n7.\nExpression of results\nExpress the concentration of each constituent in mg/l.\n8.\nPerformance characteristics of the method (precision)\nThe following data were obtained in 2009 from an international method-performance study on a variety of spirit drinks, carried out following internationally-agreed procedures (1) (2).\n8.1.\nFurfural\nAnalyte\nFurfural\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n15\n15\n15\n15\n15\n15\nNo of results accepted (laboratories)\n14\n12\n13\n14\n13\n13\nMean value (mg/l)\n2,9\n1,2\n1,7\n10,6\n15,3\n13,9\nRepeatability standard deviation, sr (mg/l)\n0,04\n0,05\n0,04\n0,18\n0,23\n0,20\nRepeatability relative standard deviation, RSDr (%)\n1,4\n4,5\n2,3\n1,7\n1,5\n1,5\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,1\n0,2\n0,1\n0,5\n0,6\n0,6\nReproducibility standard deviation, sR (mg/l)\n0,24\n0,18\n0,09\n1,4\n0,49\n0,69\nReproducibility relative standard deviation, RSDR (%)\n8\n15\n5\n13\n3\n5\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,7\n0,5\n0,3\n3,8\n1,4\n1,9\n8.2.\n5-Hydroxymethylfurfural\nAnalyte\n5-Hydroxymethylfurfural\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n16\n16\n16\n16\n16\n16\nNo of results accepted (laboratories)\n14\n14\n14\n14\n14\n14\nMean value (mg/l)\n5,0\n11,1\n9,4\n33,7\n5,8\n17,5\nRepeatability standard deviation, sr (mg/l)\n0,09\n0,09\n0,09\n0,42\n0,07\n0,13\nRepeatability relative standard deviation, RSDr (%)\n1,7\n0,8\n1,0\n1,3\n1,2\n0,8\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,2\n0,3\n0,3\n1,2\n0,2\n0,4\nReproducibility standard deviation, sR (mg/l)\n0,39\n1,01\n0,50\n4,5\n0,4\n1,6\nReproducibility relative standard deviation, RSDR (%)\n8\n9\n5\n13\n7\n9\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n1,1\n2,8\n1,4\n12,5\n1,1\n4,6\n8.3.\n5-Methylfurfural\nAnalyte\n5-Methylfurfural\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n11\n11\n11\n11\n11\n11\nNo of results accepted (laboratories)\n11\n11\n8\n11\n10\n11\nMean value (mg/l)\n0,1\n0,2\n0,1\n0,5\n1,7\n0,8\nRepeatability standard deviation, sr (mg/l)\n0,01\n0,01\n0,02\n0,02\n0,03\n0,07\nRepeatability relative standard deviation, RSDr (%)\n10,7\n6,1\n13,6\n4,7\n2,0\n10,0\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,0\n0,0\n0,1\n0,1\n0,1\n0,2\nReproducibility standard deviation, sR (mg/l)\n0,03\n0,04\n0,03\n0,18\n0,20\n0,26\nReproducibility relative standard deviation, RSDR (%)\n35\n18\n22\n39\n12\n35\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,1\n0,1\n0,1\n0,5\n0,6\n0,7\n8.4.\nVanillin\nAnalyte\nVanillin\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n16\n15\n16\n16\n16\n16\nNo of results accepted (laboratories)\n16\n15\n16\n16\n16\n16\nMean value (mg/l)\n0,5\n0,2\n1,2\n1,2\n3,2\n3,9\nRepeatability standard deviation, sr (mg/l)\n0,03\n0,02\n0,06\n0,11\n0,11\n0,09\nRepeatability relative standard deviation, RSDr (%)\n6,8\n9,6\n4,6\n8,9\n3,5\n2,3\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,1\n0,1\n0,2\n0,3\n0,3\n0,3\nReproducibility standard deviation, sR (mg/l)\n0,09\n0,06\n0,18\n0,27\n0,41\n0,62\nReproducibility relative standard deviation, RSDR (%)\n19\n25\n15\n22\n13\n16\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,3\n0,2\n0,5\n0,8\n1,2\n1,7\n8.5.\nSyringaldehyde\nAnalyte\nSyringaldehyde\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n16\n15\n16\n16\n16\n16\nNo of results accepted (laboratories)\n13\n13\n13\n12\n14\n13\nMean value (mg/l)\n1,0\n0,2\n4,8\n3,2\n10,5\n9,7\nRepeatability standard deviation, sr (mg/l)\n0,03\n0,02\n0,04\n0,08\n0,10\n0,09\nRepeatability relative standard deviation, RSDr (%)\n2,6\n8,1\n0,8\n2,6\n0,9\n0,9\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,1\n0,1\n0,1\n0,2\n0,3\n0,3\nReproducibility standard deviation, sR (mg/l)\n0,08\n0,07\n0,23\n0,19\n0,39\n0,43\nReproducibility relative standard deviation, RSDR (%)\n8\n33\n5\n6\n4\n4\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,2\n0,2\n0,7\n0,5\n1,1\n1,2\n8.6.\nConiferaldehyde\nAnalyte\nConiferaldehyde\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n13\n12\n13\n12\n13\n13\nNo of results accepted (laboratories)\n12\n12\n13\n12\n13\n13\nMean value (mg/l)\n0,2\n0,2\n0,6\n0,8\n4,6\n1,3\nRepeatability standard deviation, sr (mg/l)\n0,02\n0,02\n0,03\n0,03\n0,09\n0,06\nRepeatability relative standard deviation, RSDr (%)\n9,2\n9,8\n4,6\n4,3\n1,9\n4,5\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,04\n0,04\n0,07\n0,09\n0,24\n0,16\nReproducibility standard deviation, sR (mg/l)\n0,04\n0,04\n0,11\n0,18\n0,38\n0,25\nReproducibility relative standard deviation, RSDR (%)\n23\n27\n21\n23\n8\n19\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,1\n0,1\n0,3\n0,5\n1,1\n0,7\n8.7.\nSinapaldehyde\nAnalyte\nSinapaldehyde\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n14\n14\n14\n14\n15\n14\nNo of results accepted (laboratories)\n14\n13\n12\n13\n13\n12\nMean value (mg/l)\n0,3\n0,2\n0,2\n1,6\n8,3\n0,3\nRepeatability standard deviation, sr (mg/l)\n0,02\n0,01\n0,02\n0,06\n0,14\n0,03\nRepeatability relative standard deviation, RSDr (%)\n7,5\n4,6\n11,2\n3,7\n1,6\n11,4\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,06\n0,03\n0,06\n0,17\n0,38\n0,08\nReproducibility standard deviation, sR (mg/l)\n0,09\n0,05\n0,08\n0,20\n0,81\n0,18\nReproducibility relative standard deviation, RSDR (%)\n31\n27\n46\n13\n10\n73\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,2\n0,2\n0,2\n0,6\n2,3\n0,5\n8.8.\nGallic acid\nAnalyte\nGallic acid\nSample\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n16\n15\n16\n16\n16\n16\nNo of results accepted (laboratories)\n15\n14\n16\n16\n16\n16\nMean value (mg/l)\n1,2\n0,4\n2,0\n6,1\n7,3\n21,8\nRepeatability standard deviation, sr (mg/l)\n0,07\n0,04\n0,06\n0,18\n0,18\n0,60\nRepeatability relative standard deviation, RSDr (%)\n6,1\n8,1\n2,9\n3,0\n2,4\n2,8\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,2\n0,1\n0,2\n0,5\n0,5\n1,7\nReproducibility standard deviation, sR (mg/l)\n0,43\n0,20\n0,62\n3,3\n2,2\n7,7\nReproducibility relative standard deviation, RSDR (%)\n36\n47\n31\n53\n30\n35\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n1,2\n0,6\n1,7\n9,1\n6,2\n21,7\n8.9.\nEllagic acid\nAnalyte\nEllagic acid\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n7\n7\n7\n7\n7\n7\nNo of results accepted (laboratories)\n7\n7\n7\n7\n7\n6\nMean value (mg/l)\n3,2\n1,0\n9,5\n13\n13\n36\nRepeatability standard deviation, sr (mg/l)\n0,20\n0,16\n0,30\n0,41\n0,95\n0,34\nRepeatability relative standard deviation, RSDr (%)\n6,3\n16\n3,2\n3,2\n7,4\n1,0\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,6\n0,4\n0,9\n1,1\n2,7\n1,0\nReproducibility standard deviation, sR (mg/l)\n1,41\n0,42\n4,0\n5,0\n4,9\n14\nReproducibility relative standard deviation, RSDR (%)\n44\n43\n42\n39\n39\n40\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n4,0\n1,2\n11\n14\n14\n40\n8.10.\nVanillic acid\nAnalyte\nVanillic acid\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n15\n15\n15\n15\n15\n15\nNo of results accepted (laboratories)\n12\n11\n14\n14\n15\n14\nMean value (mg/l)\n0,2\n0,2\n1,5\n0,8\n2,4\n2,7\nRepeatability standard deviation, sr (mg/l)\n0,03\n0,04\n0,03\n0,10\n0,13\n0,21\nRepeatability relative standard deviation, RSDr (%)\n14,2\n16,5\n2,3\n12,6\n5,3\n7,7\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,1\n0,1\n0,1\n0,3\n0,4\n0,6\nReproducibility standard deviation, sR (mg/l)\n0,06\n0,05\n0,51\n0,2\n1,22\n0,70\nReproducibility relative standard deviation, RSDR (%)\n28\n20\n35\n31\n51\n26\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,2\n0,1\n1,4\n0,7\n3,4\n2,0\n8.11.\nSyringic acid\nAnalyte\nSyringic acid\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n16\n15\n16\n16\n16\n16\nNo of results accepted (laboratories)\n16\n15\n15\n15\n16\n15\nMean value (mg/l)\n0,4\n0,2\n2,5\n1,4\n3,4\n4,8\nRepeatability standard deviation, sr (mg/l)\n0,03\n0,02\n0,06\n0,13\n0,08\n0,11\nRepeatability relative standard deviation, RSDr (%)\n6,7\n12,6\n2,3\n9,0\n2,3\n2,3\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,1\n0,1\n0,2\n0,4\n0,2\n0,3\nReproducibility standard deviation, sR (mg/l)\n0,08\n0,05\n0,29\n0,26\n0,43\n0,67\nReproducibility relative standard deviation, RSDR (%)\n19\n29\n11\n18\n13\n14\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,2\n0,1\n0,8\n0,7\n1,2\n1,9\n8.12.\nScopoletin\nAnalyte\nScopoletin\nSamples\nWhisky\nBrandy\nRum\nCognac 1\nBourbon\nCognac 2\nNo of laboratories participating\n10\n10\n10\n10\n10\n10\nNo of results accepted (laboratories)\n9\n8\n9\n8\n8\n8\nMean value (mg/l)\n0,09\n0,04\n0,11\n0,04\n0,65\n0,15\nRepeatability standard deviation, sr (mg/l)\n0,0024\n0,0008\n0,0018\n0,0014\n0,0054\n0,0040\nRepeatability relative standard deviation, RSDr (%)\n2,6\n2,2\n1,6\n3,3\n0,8\n2,7\nRepeatability limit, r (mg/l)\n(r = 2,8 × sr)\n0,007\n0,002\n0,005\n0,004\n0,015\n0,011\nReproducibility standard deviation, sR (mg/l)\n0,01\n0,01\n0,03\n0,01\n0,09\n0,02\nReproducibility relative standard deviation, RSDR (%)\n15\n16\n23\n17\n15\n15\nReproducibility limit, R (g/l)\n(R = 2,8 × sR)\n0,04\n0,02\n0,07\n0,02\n0,26\n0,06\n(1)\n“Protocol for the design, conduct and interpretation of method-performance studies”, Horwitz, W. (1995) Pure and Applied Chemistry, 67, 332-343.\n(2)\nHorwitz, W. (1982) Analytical Chemistry, 54, 67A-76A.’",
  "extent": "E+W+S+N.I.",
  "status": null,
  "version": "current",
  "annotations": [
    {
      "type": "footnote",
      "label": "f1",
      "text": "split level."
    },
    {
      "type": "footnote",
      "label": "f2",
      "text": "split level."
    }
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  "outstanding_effects": [],
  "provenance": {
    "source": "legislation.gov.uk",
    "source_url": "https://www.legislation.gov.uk/eur/2016/635/annex",
    "retrieved_at": "2026-11-01T14:45:52.694376+00:00"
  },
  "licence": "Open Government Licence v3.0",
  "licence_url": "https://www.nationalarchives.gov.uk/doc/open-government-licence/version/3/",
  "attribution": "Contains public sector information licensed under the Open Government Licence v3.0. Source: legislation.gov.uk, The National Archives."
}