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31974L0203

Fifth Commission Directive 74/203/EEC of 25 March 1974 establishing Community methods of analysis for the official control of feedingstuffs

Official Journal L 108 , 22/04/1974 P. 0007 - 0024 Finnish special edition: Chapter 3 Volume 5 P. 0210  Greek special edition: Chapter 03 Volume 10 P. 0168  Swedish special edition: Chapter 3 Volume 5 P. 0210  Spanish special edition: Chapter 03 Volume 7 P. 0191  Portuguese special edition Chapter 03 Volume 7 P. 0191

FIFTH COMMISSION DIRECTIVE  of 25 March 1974  establishing Community methods of analysis for the official control of feedingstuffs  (74/203/EEC)  THE COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community;  Having regard to the Council Directive of 20 July 1970 (1), on the introduction of Community methods of sampling and analysis for the official control of feedingstuffs, as last amended by the Act (2) annexed to the Treaty (3) concerning the Accession of new Member States to the European Economic Community and the European Atomic Energy Community, and in particular Article 2 thereof;  Whereas that Directive requires that official controls of feedingstuffs be carried out using Community methods of sampling and analysis for the purpose of checking compliance with requirements arising under the provisions laid down by law, regulation or administrative action concerning the quality and composition of feedingstuffs;  Whereas Directives No 71/250/EEC of 15 June 1971 (4), No 71/393/EEC of 18 November 1971 (5), No 72/199/EEC of 27 April 1972 (6) and No 73/46/EEC of 5 December 1972 (7) have already established a number of Community methods of analysis ; whereas the progress of work since then makes it advisable to adopt a fifth set of methods;  Whereas the measures provided for in this Directive are in accordance with the Opinion of the Standing Committee for Feedingstuffs,  HAS ADOPTED THIS DIRECTIVE:    Article 1 The Member States shall require that analyses for official controls of feedingstuffs as regards the content of starch and of starch degradation products of high molecular weight in feedingstuffs containing beet cossettes, beet bulp, dried beet tops or leaves, potato pulp, dried yeasts, products rich in inulin or greaves be carried out according to the method described in Annex I to this Directive.  The general provisions set out in Part 1 (Introduction) of the Annex to the First Commission Directive No 71/250/EEC of 15 June 1971 shall be applicable to the method described in Annex I to this Directive.   Article 2 The Member States shall require that analyses for official controls of feedingstuffs as regard their contents of amprolium, ethopabate, dinitolmide (DOT), nicarbazin and menadione (vitamin K3) be carried out according to the methods described in Annex II to this Directive.  The general provisions set out in Part 1 (Introduction) of the Annex to the First Commission Directive No 71/250/EEC of 15 June 1971, with the exception of the part dealing with preparation of the sample to be analysed, shall be applicable to the methods described in Annex II to this Directive.   Article 3 The Member States shall, not later than 1 November 1974, bring into force the laws, regulations or administrative provisions necessary to comply with this Directive. They shall forthwith notify the Commission thereof.   Article 4 This Directive is addressed to the Member States.     Done at Brussels, 25 March 1974.  For the Commission  The President  François-Xavier ORTOLI  (1)OJ No L 170, 3.8.1970, p. 2. (2)OJ No L 73, 27.3.1972, p. 14. (3)OJ No L 73, 27.3.1972, p. 5. (4)OJ No L 155, 12.7.1971, p. 13. (5)OJ No L 279, 20.12.1971, p. 7. (6)OJ No L 123, 29.5.1972, p. 6. (7)OJ No L 83, 30.3.1973, p. 21.     ANNEX I DETERMINATION OF STARCH - pancreatic method -    1. Purpose and field of application  The method makes it possible to determine the content of starch and of starch degradation products of high molecular weight in feedingstuffs containing beet cossettes, beet pulp, dried beet tops or leaves, potato pulp, dried yeasts, products rich in inulin (e.g. cossettes and meal of Jerusalem artichoke) and products containing greaves. The determination should only be carried out when microscopic examination shows that significant quantities of starch are present in the sample.       2. Principle  Sugars present in the sample are extracted with ethanol. The starch in the extracted residue is reduced to sugar with pancreatin. The sugars formed are hydrolysed with hydrochloric acid and the glucose formed is determined by the Luff-Schoorl method. The quantity of glucose thus obtained, multiplied by a constant factor, gives the starch content of the sample.       3. Reagents      3.1. 90 % (v/v) ethanol, neutral to phenolphthalein.           3.2. Pentan-1-01 (amyl alcohol) a.p.           3.3. Toluene           3.4. Butter solution : dissolve in water 9.078 g potassium dihydrogen phosphate KH2PO4 and 11.876 g disodium hydrogen phosphate Na2HPO4 . 2H2O. Make up to 1 litre with water.           3.5. Sodium chloride solution 0 72 N.           3.6. Carrez I solution : dissolve in water 21 79 g zinc acetate Zn(CH3COO)2 . 2H2O and 3 g glacial acetic acid. Make up to 100 ml with water.           3.7. Carrez II solution : dissolve in water 10.6 g potassium ferrocyanide K4 [Fe (CN6)] 3H2O. Make up to 100 ml with water.           3.8. Hydrochloric acid N.           3.9. Hydrochloric acid a.p., approximately 8 N, d : 1 7125.           3.10. Sodium hydroxide solution a.p., approximately 10 N, d : 1.33.           3.11. Indicator : 0.1 % (w/v) methylorange solution.           3.12. Pancreatin in powder form, as per the directions in point 8. Keep in stoppered flasks, protected from light and moisture.           3.13. Luff-Schoorl reagent : Pour the citric acid solution (3.13.2) into the sodium carbonate solution (3.13.3) stirring carefully during the addition. Then add the copper sulphate solution (3.13.1) and make up to 1 litre with water. Leave to stand overnight and filter. Check the normality of the reagent thus obtained (Cu 0 71 N ; Na2 CO3 2N). The pH of the solution must be approximately 9.4.        3.13.1. Copper sulphate solution : dissolve 25 g copper sulphate a.p. Cu SO4 . 5H2O in 100 ml water.               3.13.2. Citric acid solution : dissolve 50 g citric acid a.p. C6H8O7 . H2O in 50 ml water.               3.13.3. Sodium carbonate solution : dissolve 143.8 g anhydrous sodium carbonate a.p. in approximately 300 ml hot water. Leave to cool.                          3.14. Granules of pumice stone purified by boiling in hydrochloric acid, washing in water and drying.           3.15. 30 % (w/v) solution of potassium iodide a.p.            3.16. Sulphuric acid, approximately 6 N, d : 1 718.           3.17. Sodium thiosulphate solution 0 71 N.           3.18. Starch solution : add a mixture of 5 g soluble starch in 30 ml water to 1 litre boiling water. Boil for 3 minutes, leave to cool. This solution should be freshly prepared.                  4. Apparatus      4.1. Extractor (see diagram p. 12), consisting of:        4.1.1. A wide-necked 500 ml conical flask;               4.1.2. A reflux condenser fitted with a bung to the conical flask;               4.1.3. A sliding spindle in the centre of the reflux condenser, fitted with a hook at its lower end. A peg to hold the spindle firm;               4.1.4. A metal container for suspending on the spindle hook (4.1.3) and holding the filtration crucible (4.1.5);               4.1.5. A filtration crucible for rapid filtration ; max. size of pores : 90 to 150 microns (e.g. porosity one, approximately 30 ml in capacity;               4.1.6. Filter papers, suitable in shape and size for the filtration crucible.                          4.2. Incubator, set at 38 ºC.           4.3. 200 ml graduated flasks with a standard ground glass joint and reflux condenser.           4.4. 100 ml graduated flasks with a standard ground glass joint and reflux condenser.                  5. Procedure      5.1. Preparation of the sample  Crush the sample so that the whole of it will pass through a 0 75 mm sieve. (ISO sieve of R 565 conforms).           5.2. Extraction  Weigh to the nearest mg 2 g of the sample and place in the filtration crucible (4.1.5), the bottom of which has first been covered with a filter paper (4.1.6) moistened with ethanol (3.1). Place in the conical flask (4.1.1) 55 ml ethanol (3.1) and a few granules of pumice stone (3.14). Place the filtration crucible in the metal container (4.1.4) and suspend the latter on the spindle hook (4.1.3). Place the reflux condenser over the conical flask and lower the spindle so that the bottom of the crucible just touches the surface of the ethanol. Peg the spindle firmly at this level. Bring the ethanol to boiling point and keep boiling for 3 hours. Then leave to cool and raise the spindle (4.1.3) to bring the crucible as high up as possible in the conical flask. Carefully unstopper the conical flask and allow 45 ml water to flow down along the sides of the flask. Replace the reflux condenser over the Erlenmeyer flask and keep the filtration crucible 10 cm above the surface of the liquid. Bring the liquid to boiling point and keep boiling for 3 hours. Then leave to cool, unstopper the conical flask and withdraw the crucible from the container.           5.3. Saccharification and hydrolysis  Place the crucible on a vacuum flask and dry under suction. Transfer the extraction residue to a mortar and grind finely. Using approximately 60 ml water, transfer the powder quantitatively to a 200 ml graduated flask with a standard ground glass joint and add a few drops of amyl alcohol (3.2). Connect a reflux condenser to the flask. Heat to boiling point and keep boiling for 1 hour. Then leave to cool and disconnect the reflux condenser. Add 25 ml buffer solution (3.4), 250 mg pancreatin (3.12), 2.5 ml sodium chloride solution (3.5) and 10 drops toluene (3.3). Shake for 2 minutes, place the flask in the incubator (4.2) and keep there for 21 hours, shaking occasionally. Then leave to cool to room temperature.  Add 5 ml Carrez I solution (3.6) and shake for one minute. Then add 5 ml Carrez II solution (3.7) and shake once again for one minute. Make up to volume with water, mix and filter. Using a pipette, take 50 ml filtrate and place in a 100 ml graduated flask (one may also work on 100 ml filtrate in a 200 ml graduated flask). Add a few drops of indicator (3.11) and acidify with hydrocholoric acid 8 N (3.9) until the indicator turns red. Then add an extra 6.25 ml hydrochloric acid 8 N (3.9) (12.50 ml if working on 100 ml filtrate). Connect the reflux condenser to the flask, bring the solution to boiling point and keep boiling for 1 hour. Leave to cool, neutralize with the sodium hydroxide solution 10 N (3.10) until the indicator turns yellow. Then acidify slightly by adding a little hydrochloric acid N ('3.8), make up to volume with water and mix. Determine the glucose content according to the Luff-Schoorl method as shown in 5.4.            5.4 Titration according to Luff-Schoorl  Using a pipette, take 25 ml Luff-Schoorl reagent (3.13) and place in a 300 ml conical flask ; add 25 ml, accurately measured, of the solution obtained in 5.3, this should not contain more than 60 mg of glucose. Add two granules of pumice stone (3.14), heat, while shaking manually, over a medium flame and bring the liquid to boiling point in approximately 2 minutes. Immediately place the conical flask on a wire gauze fitted with an asbestos screen which has a hole approximately 6 cm in diameter. Under the wire gauze a flame has first been lit, and this is regulated in such a way that only the bottom of the conical flask is heated. Then connect a reflux condenser to the conical flask. As soon as this is done, boil for 10 minutes exactly. Cool immediately in cold water and after approximately 5 minutes, titrate as follows:  Add 10 ml potassium iodide solution (3.15) and, immediately afterwards, but with care, (because of the risk of extensive foaming) 25 ml sulphuric acid 6 N (3.16). Then titrate with the sodium thiosulphate solution 0.1 N (3.17) until a dull yellow colouring appears, add a few drops of starch indicator (3.18) and complete the titration.  Carry out the same titration on an accurately measured mixture of 25 ml Luff-Schoorl reagent (3.13) and 25 ml water, after adding 10 ml potassium iodide solution (3.15) and 25 ml sulphuric acid 6 N (3.16), without bringing to the boil.           5.5. Blank test  Carry out a blank test, applying the procedure described in 5.3 and 5.4, but without a sample.       6. Calculation of results  Using the table in the Annex, determine the quantity of glucose in mg corresponding to the difference between the results of the two titrations (expressed in ml of sodium thiosulphate 0 71 N) and relating both to the sample analysis and the blank test.  The content of starch as a percentage of sample is given by the formula:  0 772 (a - b)  where:  a = mg of glucose relating to the sample;  b = mg of glucose relating to the blank test (see observation 7.2).       7. Observations      7.1 Where partially or totally dextrinated starch and lactose are simultaneously present in the sample, the result may be high by 0 75 to 3 70 %. In such cases, the actual starch content is obtained as follows:        (a) Determine the content of reducing sugars in the ethanolic extract obtained in 5.2, and express the result as a percentage of glucose;               (b) Determine the content of water-soluble reducing sugars in the sample, and express the result as a percentage of glucose;               (c) Deduct the result obtained in (a) from that obtained in (b) and multiply the difference by 0.9;               (d) Deduct the value obtained in (c) from the starch content obtained by applying the method and calculating as shown in 6.                          7.2 The quantity of glucose in relation to the blank test is normally 0 725 mg. It may not be greater than 0 750 mg.                  8. Directions relating to pancreatin  Physical aspect : yellowish-white, amorphous powder.  Glucose content : the quantity of glucose of the blank test (see 5.5) is normally 0 725 mg. A result greater than 0 750 mg indicates that pancreatin can no longer be used.  Check for iodine consumption : suspend 62 75 mg pancreatin in approximately 50 ml water heated to 25 to 30 ºC. Add 1 ml iodine solution 0 71 N. Stir for 2 minutes. Titrate with a solution of sodium thiosulphate 0 71 N in the presence of starch indicator. Consumption of iodine solution by pancreatin must not exceed 0 75 ml.  Check for amylolytic activity : mix 100 ml starch solution (3.18), 5 ml buffer solution (3.4), 0 75 ml sodium chloride solution (3.5) and 62 75 mg pancreatin. Heat the mixture to 25 to 30 ºC, stir for 2 minutes. Add 1 ml iodine solution 0 71 N. The blue colouration must have disappeared within 15 minutes exactly of the addition of the iodine solution.   Table of values for 25 ml Luff-Schoorl reagent ml of Na2S2O3 0 71 N ; 2 minutes heating ; 10 minutes boiling >PIC FILE= "T0005512">   >PIC FILE= "T0005513">     ANNEX II  1. DETERMINATION OF AMPROLIUM [Chloride hydrochloride of 1-(4-amino-2-propyl-5-pyrimidylmethyl-2-picolinium]     1.  Purpose and scope  The method makes it possible to determine the quantity of amprolium in feedingstuffs, concentrates and premixes. The lower limit of the determination is 40 ppm.    2.  Principle  The sample is extracted with diluted methanol. The extract is purified on a column of aluminium oxide and treated with a methanol solution of 2,7-dihydroxydnapthalene, potassium ferricyanide, potassium cyanide and sodium hydroxide, forming a purple colour complex. Amprolium is determined by spectrophotometry at 530 nm.    3.  Reagents    3.1. Methanol a.p.       3.2. Diluted methanol : mix two volumes of methanol (3.1) with one volume of water.       3.3. 0 72 % solution (w/v) of potassium ferricyanide K3Fe (CN)6 a.p. This solution is stable for two weeks.       3.4. 1 % solution (w/v) of potassium cyanide a.p. This solution is stable for two weeks.       3.5. 1 7125 % solution (w/v) of sodium hydroxide a.p.       3.6. Methanolic sodium hydroxide solution : dilute 15 ml of the solution (3.5) to 200 ml with methanol (3.1).       3.7. 0.0025 % solution (w/v) of 2,7-dihydroxynapthalene : dissolve 25 mg of 2,7-dihydroxynaphthalene a.p. in methanol (3.1) and make it up to 1 000 ml with methanol (3.1).       3.8. Colour reagent : Transfer 90 ml of 2,7-dihydroxynaphthalene solution (3.7) to a 250 ml conical flask (4.1), add 5 ml of potassium ferricyanide solution (3.3) and mix well. Then add 5 ml of potassium cyanide solution (3.4), stopper the flask and mix well. Leave to stand for 30 to 35 minutes, add 100 ml of methanolic sodium hydroxide solution (3.6), mix and filter through a filter crucible (4.3). Use this reagent in the 75 minutes following filtration.       3.9. Aluminium oxide for column chromatography. Before use, stir 100 g of aluminium oxide with 500 ml of water for 30 minutes, filter the slurry, wash the aluminium oxide on the filter 3 times with 50 ml of methanol (3.1) drying each time by suction, leave to stand overnight and then dry for 2 hours at 100 ºC in a vacuum drier. Put in a desiccator to cool. Check strength by subjecting a specified quantity of standard solution (3.11) to analysis, starting from point 5.2. The recovery rate of the amprolium must be 100 % ± 4 %.       3.10. Standard substance : pure amprolium complying with the characteristics below.  Melting point (decomposition) : 248 ºC. >PIC FILE= "T0005532">        3.11. Standard solution : Weigh out to within 0.1 mg, 50 mg of standard substance (3.10). Dissolve in diluted methanol (3.2) in a 500 ml volumetric flask, make up the volume with the same solvent and homogenize. Dilute 10.0 ml to 50 ml with diluted methanol (3.2) in a volumetric flask and mix well. 1 ml of this solution contains 20 ¶g of amprolium.            4. Apparatus    4.1. 50, 250 and 500 ml conical flasks with ground-glass stoppers.       4.2. Stirrer.       4.3. Filtering crucible, porosity G3, diameter : 60 mm.       4.4. Glass tube for chromatography (interior diameter : 9 mm, length : 400 to 500 mm).       4.5. Centrifuge with 25 ml tubes with ground-glass stoppers.       4.6. Spectrophotometer, with 10 mm cells.           5.  Procedure    5.1. Extraction and purification      5.1.1. Feedingstuffs and premixes  Weigh out to within 1 mg, 10 g of the finely divided and homogenized sample. For premixes weigh out 3 to 6 grams, within 1 mg. Place the test portion in a 250 ml conical flask (4.1) and add exactly 100 ml of diluted methanol (3.2). Shake for 60 minutes and filter. Dilute with diluted methanol (3.2) if necessary to obtain a solution containing 5 to 15 ¶g of amprolium per ml.  Insert a cotton wool plug into the lower end of a chromatographic tube (4.4), and tamp in 5 g of aluminium oxide (3.9) and then run in 25.0 ml of the extract. Let the liquid run through the column, discard the first 5 ml and collect the next 12 ml in a graduated test-tube.           5.1.2. Concentrates  Weigh out to within 1 mg 0 75 g of the finely divided and homogenized sample, place it in a 500 ml conical flask (4.1), add 250 ml of diluted methanol (3.2) shake or stir for 60 minutes and filter. Dilute 5 70 ml of the filtrate to 200 ml with diluted methanol (3.2) in a volumetric flask.       5.2. Development of colour and measurement of the optical density  Transfer 5 70 ml of the solution obtained in 5.1.1 or 5.1.2 into centrifuge tube A (4.5). Place 5 70 ml of diluted methanol (3.2) in centrifuge tube B (4.5). Add to each tube 10.0 ml of colouring reagent (3.8), stopper the tubes, mix and leave to stand for 18 minutes. Then centrifuge for 3 minutes and decant solutions A and B in 50 ml conical flasks (4.1).  Immediately measure the optical density of solution A at 530 nm in the spectrophotometer, using solution B as a control. Determine the quantity of amprolium by referring to the calibration curve (5.3).       5.3. Calibration curve  Pipette into centrifuge tubes (4.5) volumes of 1 70, 2 70, 3 70, 4 70 and 5 70 ml respectively of the standard solution (3.11). Make the volumes of the first four tubes up to 5 70 ml with diluted methanol (3.2). Add to all five tubes 10 70 ml of colouring reagent (3.8), stopper the tubes, mix and leave to stand for 18 minutes. Then centrifuge for 3 minutes and decant the solutions into 50 ml conical flasks (4.1).  Immediately measure the optical density of the solutions at 530 nm in the spectrophotometer, using a mixture of 5 ml ciluted methanol (3.2) and 10 ml of colour reagent (3.8) as a control. Plot the calibration curve, using the optical density values as the ordinates and the corresponding quantities of amprolium in mg as the abcissa.    6.  Calculation of results    6.1. Feedingstuffs and premixes  The amprolium content in mg per kg of sample is given by the formula >PIC FILE= "T0005514">   in which:  A = quantity of amprolium in mg as determined by photometric measurement.  W = weight of the test portion in g.  F = coefficient of dilution (possibly worked out in. 5.1.1).        6.2. Concentrates  The amprolium content per cent of sample is given by the formula >PIC FILE= "T0005515">   in which:  A = quantity of amprolium in mg as determined by phototmetric measurement.  W = weight of the test portion in g.    7.  Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed:  10 ppm, in absolute value, for amprolium contents below 100 ppm;  10 %, in relative value, for contents between 100 and 5 000 ppm;  500 ppm, in absolute value, for contents between 5 000 and 10 000 ppm;  5 %, in relative value, for contents above 10 000 ppm.   2. DETERMINATION OF ETHOPABATE (methyl-4-acetamido-2-ethoxybenzoate)    1. Purpose and scope  The method makes it possible to determine the quantity of ethopabate in feedingstuffs, concentrates and premixes. The lower limit of the determination is 2 ppm.       2. Principle  The sample is extracted with diluted methanol. The solution is acidified and extracted with chloroform. The chloroform extract is washed first with an alkaline solution and then with water. The purified extract is concentrated, the ethopabate is hydrolysed with diluted hydrochloric acid. The amino derivative thus formed is diazotized and coupled with 2-aminoethyl-1-naphthylamine. The coloured complex is extracted with butanol and the optical density of the solution is measured at 555 nm.       3. Reagents      3.1. Methanol a.p.           3.2. 50 % (v/v) methanol : mix equal volumes of methanol (3.1) and water.           3.3. Hydrochloric acid a.p., d : 1 719.           3.4. 1/10th dilute hydrochloric acid : Dilute 10 70 ml of hydrochloric acid (3.3), to 100 ml with water.           3.5. Approximately 0 73 N hydrochloric acid : Dilute 25 ml of hydrochloric acid (3.3), to 1 000 ml with water.           3.6. Chloroform a.p.           3.7. 4 % (w/v) sodium carbonate solution : Dissolve 40 70 g of anhydrous sodium carbonate a.p. in water and make up to 1 000 ml with water.           3.8. 0 72 % (w/v) sodium nitrite solution : Dissolve 100 mg of sodium nitrite a.p. in water and make up to 50 ml with water in a volumetric flask. Prepare immediately before use.           3.9. 1 70 % (w/v) ammonium sulphamate solution : Dissolve 500 mg of ammonium sulphamate a.p. in water and make up to 50 ml water in a volumetric flask. Prepare immediately before use.           3.10. 0 72 % (w/v) 2-aminoethyl-1-naphthylamine solution : Dissolve 100 mg of 2-aminoethyl-1-naphthylamine a.p. in water and make up to 50 ml with water in a volumetric flask. Prepare immediately before use.           3.11. Anhydrous sodium chloride a.p.           3.12. n-butanol a.p.           3.13. Standard substance : pure ethopabate.           3.14. Standard solutions:        3.14.1 Solution of 0 7040 mg of ethopabate per ml : Weigh out 40 mg to within 0 71 mg of standard substance (3.13). Dissolve in methanol (3.2) in a 100 ml volumetric flask ; make up the volume with the same solvent and mix. Dilute 10 70 ml to 100 ml with methanol (3.2) in a volumetric flask and mix. This solution is stable for a month.          3.14.2. Solution of 0 7016 mg of ethopabate per 20 ml : Dilute 5 70 ml of the solution (3.14.1) to 250 ml with methanol (3.2) in a volumetric flask and mix well. Prepare before use.       4. Apparatus      4.1. 250 ml conical flasks, with ground-glass stoppers.           4.2. 100 ml separating funnels, with ground-glass stoppers.           4.3. Shaker.            4.4. Rotary vacuum evaporator, with 250 ml flasks.           4.5. Water bath.           4.6. Centrifuge, with 50 ml and 15 ml tubes, with ground-glass stoppers.           4.7. Air condenser, with ground-glass joint.           4.8. Spectrophotometer, with 10 mm cells.                  5. Procedure      5.1. Extraction  Weigh out to within 1 mg, a quantity of the finely divided and homogenized sample, containing about 80 ¶g of ethopabate. Place the test portion in a 250 ml conical flask (4.1) and add 100 70 ml of diluted methanol (3.2). Mix, stopper the flask and shake for 1 hour with the aid of a shaker (4.3). Decant, filter and discard the first mls of the filtrate.           5.2. Purification  N.B. All operations under this point must be carried out rapidly.  Transfer 20 70 ml of the clear extract into a 100 ml separating funnel (4.2), add 5.0 ml of 1/10th diluted hydrochloric acid (3.4) and 20 70 ml of chloroform (3.6). Shake, first carefully and then vigorously for 3 minutes. Leave to stand until the zones separate and collect the chloroform phase in a second 100 ml separating funnel (4.2).  Extract the acid phase twice more with 20.0 ml of chloroform (3.6). Collect the chloroform extracts in the second separating funnel and discard the acid phase. Add to the combined chloroform solution 10 ml of sodium carbonate solution (3.7), shake for 3 minutes and leave to stand until the phases separate. Collect the chloroform phase in a third 100 ml separating, funnel (4.2) and discard the aqueous phase. Add to the chloroform solution 10 ml of sodium carbonate solution (3.7), shake for 3 minutes and leave to stand until the phases separate.  Collect the chloroform phase in a fourth 100 ml separating funnel (4.2), wash twice consecutively with 25 70 ml of water each time, separate the aqueous phases and quantitatively collect the chloroform extract in a 250 ml balloon flask (4.4). Combine the aqueous phases together, in one of the separating funnels ; rinse each empty funnel with a few ml chloroform ; shake the aqueous phase with the same ml chloroform, allow phases to separate, and transfer the chloroform phase to the chloroform extract collected in the flask.           5.3. Hydrolysis  Evaporate the chloroform extract down to about 2 ml on a 50 ºC water bath with the aid of the rotary vacuum evaporator (4.4). Dissolve the residue in 2 to 3 ml of methanol (3.1), and transfer quantitatively the solution in a 50 ml centrifuge tube (4.6) with the aid of two 10 ml portions and one 5 ml portion of 0.3 N hydrochloric acid (3.5). Fit the air condenser (4.7), add a few glass beads, shake well, plunge the tube in a bath of boiling water and keep it there for 45 minutes. Then cool under a stream of cold running water.           5.4. Development of colour, and measurement of the optical density  Add 1 70 ml of sodium nitrite solution (3.8), stir and leave to stand for 2 minutes. Add 1 70 ml of ammonium sulphamate solution (3.9), shake and leave to stand for 2 minutes. Add 1 70 ml of 2-aminoethyl-1-naphthylamine solution (3.10), stir and leave to stand for 10 minutes. Add 5 70 g of sodium chloride (3.11) and 10.0 ml of n-butanol (3.12), shake vigorously until the sodium chloride has completely dissolved.  Draw off the supernatant butanolic solution with the aid of a pipette, and transfer it to a 15 ml centrifuge tube (4.6) and centrifuge. Then measure the optical density EA with a spectrophotometer at 555 nm using n-butanol (3.12) as blank.           5.5. Control test  Carry out a control test, using the same procedure, starting from point 5 72, on 20 70 ml of diluted methanol (3.2). Measure the optical density FB at 555 nm using n-butanol (3.12) as blank.           5.6. Standard test  Carry out a standard test, using the same procedure, starting from point 5 72, on 20 70 ml of standard solution (3.14.2). Measure the optical density EC at 555 nm using n-butanol (3.12) as blank.        6. Calculation of results  The ethopabate content in mg per kg of sample is given by the formula >PIC FILE= "T0005516">   in which:  EA = optical density of the solution from the sample.  EB = optical density of the solution resulting from the control test.  EC = optical density of the solution resulting from the standard test.  W = weight of test portion in g.       7. Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed:  20 %, in relative value, for contents of ethopabate below 7 75 ppm;  1 75 ppm, in absolute value, for contents between 7 75 and 10 ppm;  15 %, in relative value, for contents above 10 ppm.   3. DETERMINATION OF DINITOLMIDE (DOT) (3.5-dinitro-o-toluamide)    1. Purpose and scope  The method makes it possible to determine the quantity of dinitolmide (DOT) in feedingstuffs, concentrates and premixes. Nitrofurane derivatives may interfere. The lower limit of the determination is 40 ppm.       2. Principle  The sample is extracted with acetronitrile. The extract is purified on aluminium oxide and filtered. An aliquot of the filtrate is evaporated to dryness. The residue is dissolved in dimethylformamide and treated with ethylenediamine forming a purple complex. Dinitolmide is determined by spectrophotometry at 560 nm.       3. Reagents      3.1. 85 % (v/v) acetonitrile : mix 850 ml of pure acetonitrile and 150 ml of water. Distil the mixture and collect the fraction which boils between 75 and 77 ºC before use.           3.2. Aluminium oxide for column chromatography. Calcinate at 750 ºC for at least 2 hours, cool in desiccator and keep in a brown glass bottle with a ground-glass stopper. Before use humidify as follows : place in a brown glass bottle 10 g of aluminium oxide and 0.7 ml of water, stopper, heat for 5 minutes in a bath of boiling water, shaking virgorously, let it cool, still shaking. Check strength by subjecting to analysis, starting from point 5.1, a determined quantity of standard solution (3.6). The recovery rate of the dinitolmide must be 100 % ± 2 %.           3.3. 95 % (v/v) N,N-dimethylformamide : mix 95 70 ml of N,N-dimethylformamide a.p. and 5 70 ml of water.           3.4. Diaminoethane a.p. maximum water content : 2.0 %.           3.5. Standard substance : pure 3.5-dinitro-o-toluamide complying with the characteristics below: >PIC FILE= "T0005533">            3.6. Standard solution : weigh out, to within 0.1 mg, 40 mg of standard substance (3.5), dissolve with acetonitrile (3.1) in a 200 ml volumetric flask, make up the volume with the same solvent and mix. Dilute 20 70 ml to 100 ml with acetonitrile (3.1) in a volumetric flask and mix. 1 ml of this solution contains 40 ¶g of dinitolmide.                  4. Apparatus      4.1. 250 ml conical flask with ground-glass stopper. 4.2. Reflux condenser with ground-glass joint.           4.3. Filtering crucible, porosity G 3, diameter 60 mm.           4.4. Vacuum filter (such as Witt apparatus)           4.5. Water bath, set at 50 ºC.           4.6. Spectrophotometer, with 10 mm cells.                  5. Procedure      5.1. Extraction and purification  Weigh out to within 1 mg, 10 g of the finely divided and homogenized sample. For concentrates and premixes, weigh out 1 g, to within 1 mg. Place the test portion in a 250 ml conical flask (4.1) and add 65 ml of acetonitrile (3.1). Mix, fit reflux condenser (4.2) to the flask and heat in the water bath (4.5) for 30 minutes, shaking continuously. Cool under stream of cold water. Add 20 g of aluminium oxide (3.2), shake for 3 minutes, leave to settle.   Place a 100 ml-volumetric flask in the vacuum filter (4.4), fit filtering crucible (4.3) and filter the solution, using suction. Then transfer the remaining solids into the crucible with the aid of a few ml of acetonitrile (3.1) and suck the residue dry. Release the vacuum, suspend the cake again in a few ml of acetonitrile (3.1) and evacuate again. Repeat these last operations until the volume of the filtrate reaches about 95 ml. Make up to 100 ml with acetonitrile (3.1) and mix. If necessary, dilute an aliquot with acetonitrile (3.1) to obtain a solution containing 5 to 15 ¶g of dinitolmide per ml.           5.2. Development of colour and measurement of the optical density  Pipette into three 50 ml beakers A, B and C respectively, 4 70 ml of the solution obtained in 5.1. Also add to beaker C only 1 70 ml of standard solution (3.6). Place the three beakers on the water bath (4.5), placed under a well ventilated hood, and evaporate until dry in a current of dry air. Cool the three beakers to room temparature.  Add 10 70 ml of N,N-dimethylformamide (3.3) in beaker A and 2 70 ml in beakers B and C respectively, leave in contact for a few minutes, stirring a little, until the residue completely dissolves. Then add 8 70 ml of diaminoethane (3.4) in beakers B and C and mix. Exactly 5 minutes after adding the diaminoethane measure the optical density of the three solutions in the spectrophotometer (4.6) at 560 nm using the N,N-dimethylformamide (3.3) as a blank.       6. Calculation of results  The dinitolmide content in mg per kg of sample is given by the formula: >PIC FILE= "T0005517">   in which:  EA = optical density of solution A (blank).  EB = optical density of solution B (sample).  EC = optical density of solution C (internal standard).  W = weight of test portion in grams.  F = coefficient of dilution (possibly worked out in 5.1).       7. Repeatability The difference between the results of two parallel determinations carried out on the same sample must not exceed:  10 ppm, in absolute value, for contents of dinitolmide below 100 ppm;  10 %, in relative value, for contents between 100 and 5 000 ppm;  500 ppm, in absolute value, for contents between 5 000 and 10 000 ppm;  5 %, in relative value, for contents above 10 000 ppm.   4. DETERMINATION OF NICARBAZIN (equimolecular mixture of 4,4'-dinitrocarbanilide and 2-hydroxy-4,6-dimethylpyrimidine)    1. Purpose and scope  The method makes it possible to determine the quantity of nicarbazin in feedingstuffs, concentrates and premixes containing not more than 5 % grassmeal. Nitrofuran derivatives, acetylenheptine and carbadox may interfere. The lower limit of the determination is 20 ppm.       2. Principle  The sample is extracted with N,N-dimethylformamide. The extract is purified by chromatography on a column of aluminium oxide ; the nicarbazin is eluted with ethanol. The eluate is treated with ethanolic sodium hydroxide ; forming a yellow colour. Nicarbazin is determined by spectrophotometry at 430 nm.       3. Reagents      3.1. N,N-dimethylformamide a.p.           3.2. Aluminium oxide for column chromatography. Calcinate at 750 ºC for at least 2 hours, cool in desiccator and keep in a brown glass bottle with a ground-glass stopper. Before use, check strength by subjecting to analysis, starting from point 5.2, a determined quantity of standard solution (3.8.3). The recovery rate of the nicarbazin must be 100 % ± 2 %.           3.3. 95 % (v/v) ethanol.           3.4. 80 % (v/v) ethanol.           3.5. 50 % (w/v) sdium hydroxide a.p. solution.           3.6. 1 % (w/v) ethanolic sodium hydroxide : put 1 ml of sodium hydroxide solution (3.5) in a 50 ml volumetric flask ; make up the volume with 80 % ethanol (3.4). Prepare at the time of use.  >PIC FILE= "T0005534">    3.8.  Standard solutions:      3.8.1. Solution of 1 725 mg of nicarbazin per ml : weigh out, to within 0 71 mg, 125 mg of standard substance (3 77). Dissolve in 75 ml of N,N-dimethylformamide (3.1) in a 100 ml volumetric flask, heating slightly, Allow to cool, make up the volume with the same solvent and mix. Keep away from light.           3.8.2. Solution of 0 7125 mg of nicarbazin per ml : Dilute 10 70 ml of the solution (3.8.1), to 100 ml with N,N-dimethylformamide (3.1) in a volumetric flask and mix.           3.8.3. Solution of 0 7025 mg of nicarbazin per ml : Dilute 20 70 ml of the solution (3.8.2), to 100 ml with N,N-dimethylformamide (3.1) in a volumetric flask and mix.                  4. Apparatus      4.1. 250 ml conical flask, with ground-glass stopper.           4.2. Reflux condenser with ground-glass joint.           4.3. Boiling water bath.           4.4. Centrifuge, with 120 ml tubes.           4.5. Glass tube for chromatography (interior diameter : 25 mm, length : 300 mm).           4.6. Spectrophotometer, with 10 mm cells.           4.7. Burette marked in 1/10th mls.                  5. Procedure      5.1. Extraction  Weigh out, to within 1 mg, 10 g of the finely divided and homogenized sample. For concentrates and premixes, weigh out 1 g, to within 1 mg. Place the test portion in a 250 ml conical flask (4.1) and add exactly 100 ml of N,N-dimethylformamide (3.1). Mix, fit reflux  condenser (4.2) on the flask and heat on the water-bath (4.3) for 15 minutes, shaking from time to time. Cool under a stream of cold water. Then pour the supernatant layer into a centrifuge tube (4.4) and centrifuge for about 3 minutes. If necessary, dilute 25 70 ml of the supernatant layer with N,N-dimethylformamide (3.1), to obtain a solution containing 2 70 to 10 ¶g of nicarbazin per ml.           5.2 Chromatography  Run into a tube for chromatography (4.5) a slurry of 30 g of aluminium oxide (3.2) in N,N-dimethylformamide (3.1). Let the liquid level fall to 1 cm above the column of aluminium oxide and then put into the column 25.0 ml of the extract obtained in 5.1. Allow the liquid to flow through, not letting the column get dry, and wash the column with three 10 ml portions of N,N-dimethylformamide (3.1). Then elute with 70 ml of 95 % ethanol (3.3). Eliminate the first 10 ml of the eluate and collect the rest, dividing it up as follows:  one 5 ml portion (a);  one 50 ml portion (b) in a volumetric flask;  one 5 ml portion (c).  Check that portions (a) and (c) do not turn yellow when ethanolic sodium hydroxide (3.6) is added. Continue the operations on portion (b) as shown in 5.3.           5.3 Development of colour and measurement of the optical density  Pipette 20 70 ml of portion (b) of the eluate in two separate 25 ml volumetric flasks A and B. Add to flask A 50 ml of ethanolic sodium hydroxide (3.6) and to flask B 5.0 ml of 95 % methanol (3.3).  Mix well.  Within the next five minutes measure the optical density of both solutions at 430 nm, using a mixture of 20 70 ml of 95 % methanol (3.3) and 5 70 ml of ethanol solution of sodium hydroxide (3.6) as a blank.  Subtract the value of the optical density of solution B from that of solution A. From this value determine the quantity of nicarbazin referring to the calibration curve (5.4).           5.4 Calibration  Subject 25 70 ml of the standard solution (3.8.3) to chromatography as shown in 5.2. Pour portion (b) of the eluate into the graduated burette (4.7) and distribute it in 25 ml volumetric flasks in respective volumes of 2 70, 4 70, 6 70, 8 70 and 10 70 ml (corresponding to 0 7025, 0 7050, 0 7075, 0 7100 and 0 7125 mg of nicarbazin respectively). To each flask add 5.0 ml of ethanolic sodium hydroxide (3.6), make the volume up with 95 % ethanol (3.3) and mix well.  Within the next five minutes measure the optical density of the solutions at 430 nm, using a mixture of 20 70 ml of 95 % ethanol (3.3) and 5.0 ml of ethanolic sodium hydroxide (3.6) as a control.  Trace the calibration curve, using the optical density values as the ordinates and the corresponding quantities of nicarbazin in mg as the abcissa.       6. Calculation of results  The nicarbazin content in mg per kg of sample is given by the formula >PIC FILE= "T0005518">   in which:  A = quantity of nicarbazin in mg as determined by photometric measurement;  W = weight of test portion in grams;  F = coefficient of dilution (possibly worked out in 5.1).       7. Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed:  10 ppm, in absolute value, for contents of nicarbazin below 100 ppm;  10 %, in relative value, for contents between 100 and 5 000 ppm;  500 ppm, in absolute value, for contents between 5 000 and 10 000 ppm;  5 %, in relative value, for contents above 10 000 ppm.   5. DETERMINATION OF MENADIONE (VITAMIN K3)    1. Purpose and scope  The method makes it possible to determine the quantity of menadione (vitamin K3) in feedingstuffs, concentrates and premixes. The lower limit of the determination is 1 ppm.       2. Principle  The sample is extracted with diluted ethanol. The mixture is clarified with tannin solution and centrifuged. The extract is treated with a solution of sodium carbonate ; the liberated menadione is extracted with 1,2-dichloroethane. The dichloroethane extract is treated, according to its menadione content, either directly or after evaporation, with 2,4-dinitrophenylhydrazine in solution in ethanol acidified with hydrochloric acid. The obtained hydrazone treated with ammonia in excess gives rise to a blue-green coloured complex the optical density of which is measured at 635 nm.       3. Reagents      3.1. 96 % (v/v) ethanol.           3.2. Ethanol (3.1) diluted to 40 % with water.           3.3. 10 % (w/v) tannin solution, prepared from purified powdered tannin.           3.4. 1,2-dichloroethane a.p.           3.5. 10 % (w/v) solution of anhydrous sodium carbonate p.a.           3.6. 37 % (w/v) hydrochloric acid, d = 1.19.           3.7. Absolute ethanol a.p.           3.8. 2,4-dinitrophenylhydrazine reagent : Dissolve 40 mg 2,4-dinitrophenylhydrazine a.p. in about 40 ml boiling absolute ethanol (3.7), allow to cool and transfer into a 50 ml volumetric flask. Add 1 ml hydrochloric acid (3.6) and make up to volume with absolute ethanol (3.7). Prepare immediately before use.           3.9. 25 % (w/v) ammonia, d = 0.91.           3.10. Ammoniacal ethanol : mix one volume of ethanol (3.7) with one volume of ammonia (3.9).           3.11. Standard solutions of menadione : Dissolve 20 mg menadione (vitamin K3) in 1,2-dichloroethane (3.4) and make up to 200 ml. Dilute aliquots of this stock solution with 1,2-dichloroethane (3.4) to obtain a series of solutions with menadione concentrations between 2 and 10 ¶g per ml. These solutions must be freshly prepared.                  4. Apparatus      4.1. Mechanical shaker.           4.2. Centrifuge (3 000 to 5 000 r.p.m.).           4.3. 100 and 250 ml separators, with ground glass stoppers.           4.4. Rotary vacuum evaporator, with 250 ml flasks.           4.5. Water bath.           4.6. Spectrophotometer, with 10 mm cells.                  5. Procedure  N.B. All operations must be carried out away from direct light, using apparatus of amber glass where necessary.      5.1. Test Sample  From the finely divided sample, take a test sample according to the presumed menadione content, e.g.: 0.1 to 5.0 g for concentrates and premixes;  20 to 30 g for feedingstuffs.  Transfer the test sample to a 250 ml flask with ground glass stopper without delay.            5.2 Extraction  Add to the test sample exactly 96 ml dilute ethanol (3.2) and shake mechanically for 15 minutes at room temperature. Then add 4.0 ml tannin solution (3.3), mix, transfer the extract into a centrifuge tube, centrifuge at 3 000 to 5 000 r.p.m. and decant.  Place 20 to 40 ml, accurately measured, of the extract in a 250 ml separator, add by pipette 50 ml 1,2-dichloroethane (3.4), mix and add by pipette 20 ml sodium carbonate solution (3.5). Shake vigorously for 30 seconds and then collect the dichloroethane phase in a 100 ml separator. Add 20 ml water, shake again for 15 seconds, collect the dichloroethane phase and remove traces of water with strips of filter paper.  For concentrates and premixes, take an aliquot part of the extract and dilute with 1,2-dichloroethane (3.4) to obtain a menadione concentration of 2 to 10 ¶g per ml. For feedingstuffs, evaporate to dryness an aliquot part of the extract under reduced pressure in an atmosphere of nitrogen on a water bath at 40 ºC. Rapidly treat the residue with 1,2-dichloroethane (3.4) to obtain a solution containing 2 to 10 ¶g menadione per ml.           5.3. Hydrazone formation  Transfer 2.0 ml of the dichloroethane extract obtained in 5.2 to a 10 ml volumetric flask and add 3.0 ml 2,4-dinitrophenylhydrazine reagent (3.8), securely stopper the flask with a cork or teflon stopper so as to prevent evaporation and heat for two hours at 70 ºC on a water bath. Allow to cool, add 3.0 ml ammoniacal ethanol (3.10), mix, make up to volume with absolute ethanol (3.7) and mix again.           5.4. Measurement of the optical density  Measure the optical density of the blue-green coloured complex by the spectrophotometer at 635 nm by comparison with a reagent blank obtained by treating 2.0 ml 1,2-dichloroethane (3.4) as indicated in 5.3.  Determine the quantity of menadione by reference to a calibration curve established for each series of analyses.           5.5. calibration curve  Treat 2.0 ml of the menadione standard solutions (3.11) as described in 5.3. Measure the optical density as indicated in 5.4. Plot the calibration curve with the optical density values as ordinates and the corresponding quantities of menadione in ¶g as abscissae.       6. Calculation of results  Calculate the menadione content of the sample by taking account of the weight of the test sample and of the dilations carried out in the course of analysis.  Express the result in mg menadione per kg.       7. Repeatability  The difference between the results of two parallel determinations carried out on the same sample must not exceed:    - 20 %, in relative value, for menadione contents less than 10 ppm;       - 2 ppm, in absolute value, for contents between 10 and 14 ppm;       - 15 %, in relative value, for contents between 14 and 100 ppm;       - 15 ppm, in absolute value, for contents between 100 and 150 ppm;       - 10 %, in relative value, for contents greater than 150 ppm.


Avis juridique important

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31994L0017

Commission Directive 94/17/EC of 22 April 1994 amending Council Directive 70/524/EEC concerning additives in feedingstuffs (Text with EEA relevance)

Official Journal L 105 , 26/04/1994 P. 0019 - 0025 Finnish special edition: Chapter 3 Volume 56 P. 0339  Swedish special edition: Chapter 3 Volume 56 P. 0339

COMMISSION DIRECTIVE 94/17/EC of 22 April 1994 amending Council Directive 70/524/EEC concerning additives in feedingstuffs (Text with EEA relevance)THE COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Community,  Having regard to Council Directive 70/524/EEC of 23 November 1970 concerning additives in feedingstuffs (1), as last amended by Directive 93/114/EC (2), and in particular Article 7 thereof,  Whereas Directive 70/524/EEC provides for regulart amendment of the content of its Annexes to take account of advances in scientific and technical knowledge; whereas the Annexes were consolidated by Commission Directive 91/248/EEC (3);  Whereas the use of certain additives belonging to the groups of emulsifiers, stabilizers, thickeners and gelling agents, colouring matters including pigments and acidity regulators has been widely tested in various Member States; whereas, on the basis  of experience gained, it appears that these new uses can be authorized throughout the Community;  Whereas new uses for additives belonging to the groups of colouring matters including pigments, binders, anti-caking agents and coagulants, enzymes and micro-organisms have been successfully tested in certain Member States; whereas the new uses should  be authorized provisionally at national level in anticipation of their approval at Community level;  Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee on Feedingstuffs,  HAS ADOPTED THIS DIRECTIVE:   Article 1  The Annexes to Directive 70/524/EEC are hereby amended as set out in the Annex to this Directive.   Article 2  Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive by 30 November 1994 at the latest. They shall immediately inform the Commission thereof.  When Member States adopt these measures, they shall contain a reference to this Directive or shall be accompanied by such reference at the time of their official publication. The procedure for such reference shall be adopted by Member States.   Article 3  This Directive shall enter into force on the third day following its publication in the Official Journal of the European Communities.  Done at Brussels, 22 April 1994.  For the Commission René STEICHEN Member of the Commission  (1) OJ No L 270, 14. 12. 1970, p. 1.  (2) OJ No L 334, 31. 12. 1993, p. 24.  (3) OJ No L 124, 18. 5. 1991, p. 1.      ANNEX  The Annexes to Directive 70/524/EEC are hereby amended as follows:  1. In Annex I:  1.1. In Part A, 'Antibiotics', against item E 713 'Tylosin phosphate', the following phrase is inserted in the 'Other provisions' column: 'The minimum and maximum contents are expressed as tylosing base';  1.2. In Part E, 'Emulsifers, stabilizers, thickeners and gelling agents', the following item is added:   "> ID="6.2">mg/kg of complete feedingstuffs" ID="1">'E 418> ID="2">Gellan gum> ID="3">Polytetrasaccharide containing glucose, glucuronic acid and rhamnose (2: 1: 1) produced by Pseudomonas elodea (ATCC 31466)> ID="4">Dogs, cats> ID="5">->  ID="6">-> ID="7">-> ID="8">Only canned feedingstuffs'">       1.3. Part F, 'Colouring matters including pigments' is replaced by the following text:   "> ID="6.2">mg/kg of complete feedingstuffs" ID="1""> ID="1">'F. Colouring matters including pigments"> ID="2">1. Carotenoids and xanthophylls:"> ID="1">E 160 c> ID="2">Copsanthin> ID="3">C40H56O3> ID="5">-> ID="6">-> ID="8">-"> ID="1">E 160  e> ID="2">Beta-apo-8'-carotenal> ID="3">C30H40O> ID="5">-> ID="6">-> ID="7">80 (alone or with the other carotenoids and xanthophylls)> ID="8">-"> ID="1">E 160 f> ID="2">Ethyl ester of beta-apo-8'-carotenoico acid> ID="3">C32H44O2> ID="4">Poultry>  ID="5">-> ID="6">-> ID="8">-"> ID="1">E 161 b> ID="2">Lutein> ID="3">C40H56O2> ID="5">-> ID="6">-> ID="8">-"> ID="1">E 161 c> ID="2">Cryptoxanthin> ID="3">C40H56O> ID="5">-> ID="6">-> ID="8">-"> ID="1">E 161 g> ID="2">Canthoxanthin> ID="3">C40H52O2>  ID="4">(a) Poultry> ID="5">-> ID="6">-> ID="8">-"> ID="5">-> ID="6">-> ID="8">-"> ID="4">(b) Salmon, trout> ID="5">-> ID="6">-> ID="7">80> ID="8">Use permitted from the age of six months onwards."> ID="8">The mixture of canthaxanthin with astaxanthin  is allowed provided that the total concentration of the mixture does not exceed 100 mg/kg in the complete feedingstuff"> ID="4">(c) Dogs, cats and ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 161 h> ID="2">Zeaxanthin>  ID="3">C40H56O2> ID="4">Poultry> ID="5">-> ID="6">-> ID="7">80 (alone or with the other carotenoids and xanthophylls)> ID="8">-"> ID="1">E 161 i> ID="2">Citranaxanthin> ID="3">C33H44O> ID="4">Laying hens> ID="5">-> ID="6">-> ID="8">-"> ID="1">E 161 j>  ID="2">Astaxanthin> ID="3">C40H52O4> ID="4">(a) Salmon, trout> ID="5">-> ID="6">-> ID="7">100> ID="8">Use only permitted from the age of six months onwards."> ID="8">The mixture of astaxanthin with contaxanthin is allowed provided that the total  concentration of the mixture does not exceed 100 mg/kg in the complete feedingstuff"> ID="4">(b) Ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="2">2. Other colourants:"> ID="1">E 102> ID="2">Tartrazine> ID="3">C16H9N4O9S2Na3">  ID="1">E 110> ID="2">Sunset yellow FCF> ID="3">C16H10N2O7S2Na2"> ID="1">E 124> ID="2">Ponceau 4 R> ID="3">C20H11N2O10S3Na3> ID="4">Ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 127> ID="2">Erythrosine> ID="3">C20H6I4O5Na2H2O">  ID="1">E 131> ID="2">Patent Blue V> ID="3">Calcium salt of the disulphonic acid of mhydroxytetraethyldiamino triphenylcarbinol anhydride> ID="4">(a) All species or categories of animals with the exception of dogs and cats> ID="5">-> ID="6">-> ID="7">->  ID="8">Permitted in animal feedingstuffs only in products processed from:"> ID="8">(i) waste products of feedingstuffs;"> ID="8">(ii) denatured cereals or manioc flour; or"> ID="8">(iii) other base substances denatured by means of these agents or  coloured during technical preparation to ensure the necessary identification during manufacture"> ID="4">(b) Dogs and cats> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 132> ID="2">Indigotine> ID="3">C16H8N2O8S2Na2> ID="4">Ornamental fish>  ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 141> ID="2">Chlorophyll copper complex> ID="3">-> ID="4">Ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 142> ID="2">Acid brilliant green BS (Lissamine green)> ID="3">Sodium salt of  4,4'-bis (dimethylamino) diphenylmethylene-2-naphtol3,6-disulphonic acid> ID="4">(a) All species or categories of animals with the exception of dogs, cats and ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">Permitted in animal feedingstuffs only  in products processed from:"> ID="8">(i) waste products of foodstuffs;"> ID="8">(ii) denatured cereals or manioc flour; or"> ID="8">(iii) other base substances denatured by means of these agents or coloured during technical preparation to ensure the  necessary identification during manufacture"> ID="4">(b) Dogs, cats and ornamental fish> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 153> ID="2">Carbon black> ID="3">C> ID="5">-> ID="6">-> ID="7">-"> ID="1">E 160 B> ID="2">Bixin>  ID="3">C25H30O4> ID="4">Ornamental fish> ID="5">-> ID="6">-> ID="7">-"> ID="1">E 172> ID="2">Iron oxide, red> ID="3">Fe2O3> ID="5">-> ID="6">-> ID="7">-"> ID="2">3. Colouring agents authorized for colouring foodstuffs by Community rules, other than  Patent blue V and Acid brilliant green BS> ID="3">-> ID="4">(a) All species or categories of animals with the exception of dogs and cats> ID="5">-> ID="6">-> ID="7">-> ID="8">Permitted in animal feedingstuffs only in products processed from:">  ID="8">(i) waste products of foodstuffs; or"> ID="8">(ii) other base substances, with the exception of cereals and manioc flour, denatured by means of these agents of coloured during technical preparation to ensure the necessary identification during  manufacture"> ID="4">(b) Dogs and cats> ID="5">-> ID="6">-> ID="7">-> ID="8">-'""       1.4. In Part M, 'Acidity regulators' the following items are added:   "> ID="6.2">mg/kg of complete feedingstuffs" ID="1">'E 525> ID="2">Potassium hydroxide> ID="3">-> ID="4">Dogs and cats> ID="5">-> ID="6">-> ID="7">-> ID="8">-"> ID="1">E 526> ID="2">Calcium hydroxide> ID="3">-> ID="4">Dogs and cats> ID="5">->  ID="6">-> ID="7">-> ID="8">-'">        2. In Annex II:  2.1. In Part F, 'Colouring matters including pigments', the following item is added:   "> ID="6.2">mg/kg of complete feedingstuff" ID="1">'11> ID="2">Astaxanthin-rich Phaffia rhodozyma> ID="3">Concentrated biomass of the yeast Phaffia rhodozyma (CBS 116.94), killed, containing at least 2,5 g ostaxanthin per kilogram additive>  ID="4">Salmon, trout> ID="5">-> ID="6">-> ID="7">100> ID="8">The maximum content is expressed as astaxanthin.> ID="9">30. 11. 1994'"> ID="8">Use only permitted from the age of six months onwards."> ID="8">The mixture of the additive with canthaxanthin  is allowed provided that the total concentration of astaxanthin and canthaxanthin does not exceed 100 mg/kg in the complete feedingstuff">        2.2. In Part L, 'Binding agents, anti-caking agents and coagulents', the following item is added:   "> ID="6.2">mg/kg of complete feedingstuff" ID="1">'2 > ID="2">Natrolite-phonolite> ID="3">Natural mixture of aluminium silicates, alkalines and alkaline-earth and aluminium hydrosilicates, natrolite (43 % - 46,5 %) and feldspar> ID="4">All  animal species and categories> ID="5">-> ID="6">-> ID="7">25 000> ID="8">All feedingstuffs> ID="9">30. 11. 1994'">        2.3. the following group and item are added:   "> ID="6.2">Unit of activity per kg of complete feedingstuff" ID="2">'N. Enzymes" ID="1">1> ID="2">3-phytase (EC 3.1.3.8)> ID="3">Preparation of 3-phytase produced by Aspergillus niger (CBS 114.94) having a minimum phytase activity of 5 000  FTU/g for solid and liquid preparations> ID="4">Pigs (all categories of animals)> ID="5">-> ID="6">-> ID="7">-> ID="8">-> ID="9">30. 11. 1994"> ID="4">Chickens (all categories of animals)> ID="5">-> ID="6">-> ID="7">-> ID="8">-> ID="9">30. 11.  1994'""        2.4. the following group and item are added:   "> ID="6.2">Minimum" ID="1">Maximum"> ID="2">'O. Micro-organisms" ID="1">1> ID="2">Bacillus cereus var. toyoi (CNCM I-1012/NCIB 40112)> ID="3">Preparation of Bacillus cereus var. toyoi containing a minimum 1010CFU/g additive> ID="4">Piglets>  ID="5">Two months> ID="6">109> ID="7">109> ID="8">-> ID="9">30. 11. 1994"> ID="5">four months> ID="6">0,5×109> ID="7">109> ID="8">-"> ID="4">Pigs> ID="5">six months> ID="6">0,2×109> ID="7">109> ID="8">-> ID="9">30. 11. 1994"> ID="4">Sows> ID="5">->  ID="6">109> ID="7">2×109> ID="8">-> ID="9">30. 11. 1994'""


Avis juridique important

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31995L0017

Commission Directive 95/17/EC of 19 June 1995 laying down detailed rules for the application of Council Directive 76/768/EEC as regards the non- inclusion of one or more ingredients on the list used for the labelling of cosmetic products

Official Journal L 140 , 23/06/1995 P. 0026 - 0029

COMMISSION  DIRECTIVE 95/17/EC of 19 June 1995 laying down detailed rules for the application of Council  Directive 76/768/EEC as regards the non-inclusion of one or more ingredients on the list used for  the labelling of cosmetic products (Text with EEA relevance)THE COMMISSION OF THE  EUROPEAN COMMUNITIES, Having regard to the Treaty establishing the European Community, Having regard to Council Directive 76/768/EEC of 27 July 1976 on the approximation of the laws of  the Member States relating to cosmetic products  (1), as last amended by Commission Directive  94/32/EC  (2), and in particular Article 6 (1) (g) thereof, Whereas there is a need to specify the criteria and conditions under which a manufacturer may, for  reasons of trade secrecy, apply not to include one or more ingredients on the minimum list of  ingredients which must be included on the packaging of cosmetic products, or, where this is  impossible for practical reasons, on an enclosed leaflet, label, tape or card; Whereas approval of confidentiality should not, however, impinge on the other obligations pursuant  to Directive 76/768/EEC and the responsibilities arising from the Articles concerning the cosmetic  product's safety, from the Annexes, and from the provisions as to the information necessary for  appropriate medical treatment and the case-file to which the national monitoring authorities must  have access; Whereas approval of confidentiality should not be prejudicial to consumer safety; Whereas the request for confidentiality must be submitted in the Member State of manufacture or  initial importation into the Community market, which must also have access to the information  referred to in Article 7a of Directive 76/768/EEC, as amended by Directive 93/35/EEC  (3), for  control purposes; Whereas to be adequately assessed and monitored the request must include all the particulars  necessary for identifying the applicants, for the identification and human health assessment of the  ingredient as used in the cosmetic product(s) and for determining the intended use of the  ingredient concerned, as well as the grounds for confidentiality and the name(s) of the product  containing the ingredient; Whereas for economic reasons and in deference to his rights the competent authority should inform  the applicant, within a brief period of not more than four months, other than in exceptional cases,  of the ruling in this case; whereas any refusal to grant confidentiality should be duly reasoned  and the means of appeal and time limits clearly indicated; Whereas in the interests of transparency and monitoring, the competent authority should allocate a  registration number to each request it approves; whereas this number should replace the ingredient  in the list of ingredients referred to in Article 6 (1) (g) of Directive 76/768/EEC; Whereas all amendments to the particulars contained in the initial request must be communicated by  the applicant to the competent authority, which may then withdraw its approval of confidentiality  in view of those modifications, or if new information makes such a measure necessary for compelling  public health reasons; Whereas the duration of the right to confidentiality should not exceed five years, subject to the  option, in exceptional circumstances, of an extension for a further three years at the most; Whereas, in the interests of monitoring product safety and proper enforcement of the Directive, the  Commission and the other Member States should be adequately informed of the decisions taken by the  competent authority; whereas, on the other hand, such decisions should be recognized throughout the  Community territory, except for exceptional reasons; Whereas the measures provided for in this Directive are in accordance with the opinion of the  Committee on the Adaptation to Technical Progress of the Directives on the Removal of Technical  Barriers to Trade in the Cosmetics Products Sector, HAS ADOPTED THIS DIRECTIVE: Article 1 This Directive shall apply without prejudice to the other obligations  arising from Directive 76/768/EEC and the responsibilities arising therefrom, in particular from  Articles 2, 4, 5, 7 (3) and 7a thereof. Article 2 Any manufacturer or his agent or person on whose account a cosmetic product is  manufactured, or any person responsible for placing an imported cosmetic product on the Community  market, who, for reasons of trade secrecy, wishes not to include one or more ingredients of a  cosmetic product on the list referred to in Article 6 (1) (g) of Directive 76/768/EEC, shall submit  a request to that effect to the competent authority referred to in Article 10 of this Directive of  the Member State of the place of manufacture or initial importation, prior to placing the product  on the Community market. Article 3 The request referred to in Article 2 must include the following particulars: (a)  name or style and address or head office of the applicant; (b)  precise identification of the ingredient for which confidentiality is requested, namely: -  the CAS, Einecs and colour index numbers, the chemical name, the Iupac name, the INCI  (1) name,  the European Pharmacopoeia name, the international non-proprietary name recommended by the World  Health Organization, and the common nomenclature name referred to in Article 7 (2) of Directive  76/768/EEC, where they exist, -  the Elincs name and the official number allocated to it if it has been notified pursuant to  Council Directive 67/548/EEC  (2) and indication of approval or refusal to approve a request for  confidentiality pursuant to Article 19 of that Directive, -  where the names or numbers referred to in the first and second indents do not exist, as in the  case of certain ingredients of natural origin, the name of the base material, the name of the part  of the plant or animal used, and the names of the ingredient's components, such as solvents; (c)  the evaluation of the safety for human health of the ingredient as used in the finished  product(s), taking into account the ingredient's toxicological profile, chemical structure and the  level of exposure, as specified in Article 7a (1) (d) and (e) and Article 7a (2) of Directive  76/768/EEC; (d)  the envisaged use of the ingredient and in particular the different categories of products in  which it will be used; (e)  a detailed justification of why, by way of exception, confidentiality is sought; for example: -  the fact that the identity of the ingredient or its function in the cosmetic product to be  marketed has not been described in the literature and is unknown to others in the trade, -  the fact that the information is not yet in the public domain, even though a patent application  has been lodged for the ingredient or its use, -  the fact that if the information were known it would be easily reproducible, to the detriment of  the applicant; (f)  if known, the name of each product which is to contain the ingredient(s), and if different  names are to be used in the Community market, precise details on each one of them. If the name of a product is not yet known, it may be communicated at a later date, but at least 15  days before placing the product on the market. If the ingredient is used in several products, one request shall suffice, provided that the  products are clearly indicated to the competent authority; (g)  a statement setting out whether a request has been submitted to the competent authority of any  other Member State in respect of the ingredient for which confidentiality is sought, and  particulars on the outcome of any such request. Article 4 1.  After receipt of the request for confidentiality in accordance with Article 3 the  competent authority shall, within a period not exceeding four months, examine the request and  inform the applicant in writing of its decision. In the event of approval, the authority shall also  communicate the registration number it has allocated to the product in accordance with the  procedure laid down in the Annex. However, if there are exceptional reasons, the competent  authority may inform the applicant in writing that an additional period of two months will be  required for the examination of the request. 2.  Any refusal to grant a request for confidentiality must include a statement of reasons; appeal  procedures, together with their time limits, must be clearly explained to the applicant. Article 5 The registration number referred to in Article 4 (1) shall replace the ingredient in  question in the list referred to in Article 6 (1) (g) of Directive 76/768/EEC. Article 6 1.  All amendments to the information provided pursuant to Article 3 must be  communicated as rapidly as possible to the competent authority that has granted the request for  confidentiality. All changes to the names of cosmetic products containing the ingredient must be  communicated to the competent authority at least 15 days before those products are placed on the  market under their new name. 2.  Taking into consideration the amendments referred to in paragraph 1, or if new information  makes it imperative to do so, particularly for compelling reasons of public health, the competent  authority may withdraw its approval. In this event it shall inform the applicant of its new  decision within the time limits and in accordance with the procedure referred to in Article 4. Article 7 The decision granting the right to confidentiality shall be valid for a period of five  years. If the beneficiary of this decision considers that there are exceptional reasons justifying an  extension of this period, he may submit a reasoned request to the competent authority which  initially granted the request for confidentiality. The competent authority shall decide on this new request within the time limits and under the  conditions referred to in Article 4. The confidentiality period shall not be extended by more than three years. Article 8 1.  Member States shall inform the Commission and the other Member States of their  decisions to grant requests for confidentiality or to extend such approval, indicating the name or  style and address or head office of the applicants, the names of the cosmetic products containing  the ingredient in respect of which the request for confidentiality has been granted, and the  registration number referred to in Article 4 (1). The Commission and the other Member States may obtain, on request, a copy of the case file  containing the request for confidentiality together with the decision of the competent authority.  Particularly in this framework the competent authorities of the Member States and the Commission  shall make arrangements to ensure proper cooperation. 2.  Member States shall inform the Commission and the other Member States of their reasoned  decisions to refuse or to withdraw approval of confidentiality or to refuse to extend the  confidentiality period. 3.  Member States and the Commission shall take the necessary measures to ensure that confidential  data made known to them is not improperly disclosed. Article 9 Member States shall recognize the decisions taken by a competent authority as to the  approval of confidentiality or extension of the confidentiality period. However, if, after having been informed or after having received a copy of the case file in  accordance with the procedure under Article 8 (1), a Member State challenges a decision taken by  the competent authority of another Member State, it may ask the Commission to take a decision  pursuant to the procedure referred to in Article 10 of Directive 76/768/EEC. Article 10 Member States shall designate the competent authorities referred to in this Directive  and shall inform the Commission thereof, which shall publish them in the Official Journal of the  European Communities. A Member State may also designate the competent authority of another Member  State, willing to accept for the purposes of examination in exceptional cases the requests referred  to in Article 2. Article 11 1.  Member States shall bring into force the laws, regulations and administrative  provisions necessary to comply with this Directive not later than 30 November 1995. They shall  forthwith inform the Commission thereof. When Member States adopt these provisions, these shall contain a reference to this Directive or  shall be accompanied by such reference at the time of their official publication. The procedure for  such reference shall be adopted by Member States. 2.  Member States shall communicate to the Commission the text of the provisions of national law  which they adopt in the field covered by this Direcitve. Article 12 This Directive shall enter into force on the seventh day following its publication in  the Official Journal of the European Communities. Article 13 This Directive is addressed to the Member States. Done at Brussels, 19 June 1995. For the Commission Emma BONINO Member of the Commission  ANNEX PROCEDURE FOR GRANTING THE REGISTRATION NUMBER REFERRED TO IN ARTICLE 4 1.  The  registration number referred to in Article 4 consists of seven digits, the first two corresponding  to the year of approval of confidentiality, the second two to the code assigned to each Member  State pursuant to point 2, and the three final digits being assigned by the competent authority. 2.  The following codes are allocated to the Member States: 01  France 02  Belgium 03  Netherlands 04  Germany 05  Italy 06  United Kingdom 07  Ireland 08  Denmark 09  Luxembourg 10  Greece 11  Spain 12  Portugal 13  Finland 14  Austria 15  Sweden.


Avis juridique important

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31975L0033

Council Directive 75/33/EEC of 17 December 1974 on the approximation of the laws of the Member States relating to cold-water meters

Official Journal L 014 , 20/01/1975 P. 0001 - 0009 Finnish special edition: Chapter 13 Volume 4 P. 0069  Greek special edition: Chapter 13 Volume 3 P. 0022  Swedish special edition: Chapter 13 Volume 4 P. 0069  Spanish special edition: Chapter 13 Volume 4 P. 0044  Portuguese special edition Chapter 13 Volume 4 P. 0044

COUNCIL DIRECTIVE  of 17 December 1974  on the approximation of the laws of the Member States relating to cold-water meters  (75/33/EEC)   THE COUNCIL OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community, and in particular Article 100 thereof;  Having regard to the proposal from the Commission;  Having regard to the Opinion of the European Parliament (1);  Having regard to the Opinion of the Economic and Social Committee (2);  Whereas in the Member States the construction and the methods of control of cold-water meters are subject to mandatory provisions which differ from one Member State to another and consequently hinder trade in such instruments ; whereas it is therefore necessary to approximate these provisions;  Whereas Council Directive No 71/316/EEC (3) of 26 July 1971 on the approximation of the laws of the Member States relating to common provisions for both measuring instruments and methods of metrological control, as amended by the Act of Accession (4), laid down the EEC pattern approval and EEC initial verification procedures ; whereas, in accordance with that Directive, the technical requirements for the design and functioning of cold-water meters should be laid down ; whereas such requirements must be met, and the controls must be carried out, and the appropriate signs and marks affixed, before these instruments can be freely imported, marketed and used,  HAS ADOPTED THIS DIRECTIVE:     Article 1 This Directive shall apply to cold-water meters, which are integrating measuring instruments for continuously determining the volume of water (and no other liquid) passing through them, and which comprise a measuring device linked to an indicating device. Water shall be considered to be "cold" when its temperature is in the range 0º to 30º C.   Article 2 Cold-water meters which may bear the EEC marks and signs are described in the Annex to this Directive. They shall be subject to EEC pattern approval and submitted to EEC initial verification.   Article 3 No Member State may refuse, prohibit or restrict the placing on the market or entry into service of (1)OJ No C 2, 9.1.1974, p. 62. (2)OJ No C 8, 31.1.1974, p. 6. (3)OJ No L 202, 6.9.1971, p. 1. (4)OJ No L 73, 27.3.1972, p. 14.   cold-water meters bearing the EEC pattern approval symbol and the EEC initial verification mark, on the grounds of their metrological properties.   Article 4 1. Member States shall put into force the laws, regulations and administrative provisions needed in order to comply with this Directive within 18 months of its notification and shall forthwith inform the Commission thereof.  2. Member States shall ensure that the texts of the main provisions of national law which they adopt in the field covered by this Directive are communicated to the Commission.   Article 5 This Directive is addressed to the Member States.     Done at Brussels, 17 December 1974.  For the Council  The President  M. DURAFOUR     ANNEX    I.  TERMINOLOGY AND DEFINITIONS    1.0. This Annex applies only to cold-water meters based on a direct mechanical process involving the use of volumetric chambers with mobile walls or the action of the velocity of the water on the rotation rate of a moving part (turbine, impeller etc...).       1.1. Flowrate  The flowrate is the volume of water passing through the meter per unit of time, the volume being expressed in cubic metres or litres and the time in hours, minutes or seconds.       1.2. Volume delivered  The volume delivered is the total volume of water which has passed through the meter in a given time.       1.3. Maximum flowrate (Qmax)  The maximum flowrate, Qmax, is the highest flowrate at which the meter can function over limited periods without damage, and without exceeding the maximum permissible errors and the maximum permissible value for loss of pressure.       1.4. Nominal flowrate (Qn)  The nominal flowrate, Qn, is equal to half the maximum flowrate, Qmax. It is expressed in cubic metres per hour and is used to designate the meter.  At the nominal flowrate, Qn, the meter should be able to function in normal use, i.e., in continuous and intermittent operating conditions, without exceeding the maximum permissible errors.       1.5. Minimum flowrate (Qmin)  The minimum flowrate, (Qmin), is the flowrate above which the meter must not exceed the maximum permissible errors, and is fixed as a function of Qn.       1.6. Flowrate range  The flowrate range of a water meter is bounded by the maximum and minimum flowrates, Qmax and Qmin. It is divided into two regions, termed upper and lower, with different maximum permissible errors.       1.7. Transitional flowrate : (Qt)  The transitional flowrate, Qt, is the flowrate which divides the upper and lower regions of the flow range and the rate at which the maximum permissible errors become discontinuous.       1.8. Maximum permissible error  The maximum permissible error is the limit of the error permitted by this Directive for EEC pattern approval and EEC initial verification of a water meter.        1.9. Loss of pressure  Loss of pressure means the loss which is caused by the presence of the water meter in the conduit.          II.  METROLOGICAL CHARACTERISTICS    2.1. Maximum permissible errors  The maximum error permitted in the lower region, from Qmin inclusive to Qt non-inclusive, is ± 5 %.  The maximum error permitted in the upper region, from Qt inclusive to Qmax inclusive, is ± 2 %.       2.2. Metrological classes  Water meters are divided, according to the values of Qmin and Qt defined above, into the three metrological classes in the following table: >PIC FILE= "T0006670">           III.  TECHNOLOGICAL CHARACTERISTICS    3.1. Construction - General provisions  The meters must be constructed in such a way as to:      (1) give long service and guarantee proof against fraud,           (2) conform with the provisions of this Directive, under normal conditions of use.             Where meters may be subjected to an accidental reversal of flows they must be capable of withstanding it without any deterioration or change in their metrological properties, and at the same time should record such a reversal.       3.2. Materials  The water meter must be made of materials of adequate strength and stability for the purpose for which the water meter is to be used. It must be constructed throughout of materials which are resistant to internal and normal external corrosion and if necessary be protected by some suitable surface treatment. Water temperature variations within the working temperature range must not adversely affect the materials used in the construction of the water meter.        3.3. Soundness - pressure tightness  A meter must be able to withstand constantly - without defects in its functioning, leakage, seepage through the walls or permanent deformation - the continuous water pressure for which it is designed, termed the maximum operating pressure. The minimum value for this pressure is 10 bars.       3.4. Loss of pressure  Loss of pressure through the meter is determined by EEC pattern approval tests, and must not exceed 0.25 bars at the nominal flowrate and one bar at the maximum flowrate.  On the basis of the test results meters are divided into one of four groups with the following maximum values for pressure loss : 1, 0.6, 0.3 and 0.1 bars. The relevant value must be indicated in the EEC pattern approval certificate.       3.5. Indicating mechanisms  The indicator must allow, by simple juxtaposition of its various constituent elements, a reliable, easy and unambiguous reading of the volume of water measured, expressed in cubic metres. The volume is given either by:      (a) the position of one or more pointers on circular scales;           (b) reading off a row of in-line consecutive digits in one or more apertures;           (c) a combination of these two systems.             The cubic metre and its multiples are indicated in black, and sub-multiples of the cubic metre in red.  The actual or apparent height of the digits must not be less than 4 mm.  On digital indicators (types (b) and (c)) visible displacement of all digits must be upwards in value. The advance of any given digital unit must be completed while the digit of the immediately next lower value describes the last tenth of its course ; the roller showing the digits of lowest value may move continuously in the case of type (c). The whole number of cubic metres must be clearly indicated.  Indicators with pointers (types (a) and (c)) should rotate in a clockwise direction. The value in cubic metres for each scale divison should be expressed as 10n, where n is a positive or negative whole number or zero, thereby establishing a system of consecutive decades. The following should be shown near each part of the scale : × 1000 - × 100 - × 10 - × 1 - × 0.1 - × 0.01 - × 0.001.  In both cases (dial and digital indicators):      - the unit symbol m3 should be shown either on the dial or in the immediate vicinity of the digital indication;           - the fastest-moving visible graduated element, the control element, the scale interval of which is known as the "verification scale interval", should move continuously. This control element may be permanent or may be fitted temporarily by adding detachable parts. These parts must not have any significant influence on the metrological properties of the meter.              The length of the verification scale interval should be not less than 1 mm and not more than 5 mm. The scale shall consist:      - either of lines of equal thickness not exceeding one quarter of the distance between the axes of two consecutive lines and differing only in length;           - or of contrasting bands of a constant width equal to the length of the scale division.             However, for a period of 6 1/2 years from the notification of this Directive:      (a) the downward movement of digits will be permitted, this movement being indicated by an arrow;           (b) the length of the scale division may be 0.8 mm.                  3.6. Number of figures in the verification scale division and their values  It must be possible for the indicating device to record a volume, expressed in cubic metres, corresponding to at least 1 999 hours' operation at the nominal flowrate, without returning to zero.  The size of the verification scale division must be based on the formula 1 × 10n or 2 × 10n or 5 × 10n. During verification, it must be small enough to ensure a measurement inaccuracy of not more than 0.5 % (allowing for a possible reading error of not more than half the length of the smallest scale division) and small enough so that at the minimum flowrate the test does not take more than 1 1/2 hours.  However, for a period of 6 1/2 years from the notification of this Directive a maximum duration of seven hours shall be permitted.  A supplementary device (star, disc with a reference mark, etc.) may be added in order to show the movement of the measuring device before this becomes clearly visible on the indicator.       3.7. Adjustment device  The meters may be fitted with an adjustment device with which it is possible to alter the relationship between the volume indicated and the volume actually passed. This device is compulsory for meters which make use of the action of the velocity of the water on the rotation of a moving part.       3.8. Accelerating device  The use of an accelerating device for increasing the speed of the meter below Qmin is prohibited.           IV.  MARKS AND INSCRIPTIONS    4.1. Identification inscriptions  It is compulsory for all meters to carry, in a legible and indelible manner, either separately or grouped together on the meter casing, the indicator dial, or the indication plate, the following information:      (a) the name or trade name of the manufacturer or his trademark;           (b) the metrological class and nominal flowrate Qn in cubic metres per hour;           (c) the year of manufacture, individual serial number;           (d) one or two arrows showing direction of flow;           (e) the EEC pattern approval symbol;            (f) the maximum operating pressure in bars if this can exceed 10 bars;           (g) the letter "V" or "H" if the meter can operate properly only in either the vertical (V) or horizontal (H) positions.                  4.2. Placing of verification marks  Space for the EEC verification marks should be provided on an essential part (normally the meter casing), which is visible without dismantling.       4.3. Sealing  Water meters shall have protective devices which can be sealed in such a way that after sealing, both before and after the water meter has been properly installed, there is no possibility of dismantling or altering the water meter or its adjustment device without damaging the protective devices.          V.  EEC PATTERN APPROVAL    5.1. Procedure  The procedure for EEC pattern approval will be carried out in accordance with Directive No 71/316/EEC.       5.2. Pattern tests  When it has been ascertained from the application file that the pattern conforms to the provisions of this Directive, laboratory tests will be carried out on a number of instruments under the following conditions:      5.2.1. Number of meters to be tested  The number of meters to be submitted by the manufacturer is as shown in the following table: >PIC FILE= "T0006671">            5.2.2. Pressure  For the metrological tests (point 5.2.4), the pressure at the meter outlet should be sufficiently high to prevent cavitation.           5.2.3. Test equipment  In general meters shall be tested individually and, in all cases, in such a way as to demonstrate the individual characteristics of each.  The metrological service of the Member State will take the necessary steps to ensure that the maximum relative inaccuracy in measuring the volume of water delivered does not exceed 0.2 %, including the various causes of error in installation.  The maximum permissible inaccuracy is 5 % in the case of measurement of pressure and 2.5 % in the case of measurement of loss of pressure.  During each test, the relative variation in the flowrates should not exceed 2.5 % between Qmin and Qt and 5 % between Qt and Qmax.   The equipment must be approved by the metrological service of the Member State concerned no matter where these tests are carried out.           5.2.4. Test procedure  The tests comprise the following operations, carried out in the order shown:        (1) pressure tightness test;               (2) determination of the error curves on the basis of the flowrate by ascertaining the effect of the pressure and taking into account the normal installation conditions for this type of meter (straight sections of piping upstream and downstream of the meter, constrictions, obstacles, etc.) stipulated by the manufacturer;               (3) determination of pressure losses;               (4) accelerated endurance test.                 The pressure tightness test consists of two parts:        (a) each meter should be able to withstand, without leakage or seepage through the walls, a pressure of 16 bars or 1.6 times the maximum operating pressure, applied for a period of 15 minutes (see point 4.1 (f));               (b) each meter should be able to withstand, without any damage or blockage, a pressure of 20 bars or twice the maximum operating pressure, applied for a period of one minute (see point 4.1 (f));                 The results of tests (2) and (3) should provide a sufficient number of points to enable the curves to be plotted accurately throughout the range.  The accelerated endurance test is to be carried out as follows: >PIC FILE= "T0006672">   Before the first test and after each series of tests the measuring errors must be determined, as a minimum requirement, at the following flowrates:  Qmin, Qt, 0.3 Qn, 0.5 Qn, 1 Qn, 2 Qn  In each test, the volume of water passed through the meter must be sufficient to rotate the pointer or the roller on the verification scale through one or more complete revolutions and to eliminate the effects of cyclic distortion.            5.2.5. Conditions for EEC pattern approval  A water meter pattern will be approved if it fulfils the following conditions:      (a) it conforms with the administrative, technical and metrological provisions of this Directive and its Annex;           (b) tests 1, 2 and 3 under point 5.2.4 show that it conforms with Parts II and III of this Annex as regards metrological and technological characteristics;           (c) after each accelerated endurance test:        1. no variation in relation to the initial curve greater than 1.5 % between Qt and Qmax or greater than 3 % between Qmin and Qt has been observed;               2. the maximum error of the meter between Qmin and Qt is ± 6 % and between Qt and Qmax ± 2.5 %.                                  VI. EEC INITIAL VERIFICATION This will be carried out in a place approved by the metrological service of the Member State. The layout of the premises and the test equipment should be such that verification may be carried out in safe, reliable conditions, and with no loss of time for the person responsible for the control. The provisions of point 5.2.3 should be complied with, but the meters may be tested in series if desired. If this method is employed the exit pressure of all the meters should be sufficient to prevent cavitation and special measures may be required to prevent interference between meters.  The complete unit may include automatic devices, by-pass valves, flow-restrictors, etc., provided that each test circuit between the meters to be verified and the control tanks is clearly defined and that it is possible to verify at any time its internal pressure absorption.  Any type of water supply system may be used, but if several test circuits are operated in parallel, there should be no interference incompatible with the provisions of point 5.2.3.  If a control tank is divided into several chambers, the separating walls should be sufficiently rigid to ensure that the volume of a chamber does not vary by more than 0.2 % according to whether the adjacent chambers are full or empty.  Verification includes an accuracy test at at least three flowrates:    (a) between 0.9 Qmax and Qmax;       (b) between Qt and 1.1 Qt;       (c) between Qmin and 1.1 Qmin.         The first of these tests involves the determination of pressure loss, which should be less than the value indicated in the EEC pattern approval certificate.  The maximum permissible errors are as shown in point 2.1.  In each test, the volume of water passed through the meter should be sufficient to rotate the pointer or roller on the verification scale through one or more complete revolutions and to eliminate the effects of cyclic distortion.  If all the errors are found to lie in one direction, then the water meter shall be adjusted so that not all the errors exceed one-half of the maximum permissible error.


Important legal notice

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31979L0268

Council Directive 79/268/EEC of 5 March 1979 amending Directive 77/504/EEC on pure-bred breeding animals of the bovine species

Official Journal L 062 , 13/03/1979 P. 0005 - 0005 Finnish special edition: Chapter 3 Volume 10 P. 0199  Greek special edition: Chapter 03 Volume 24 P. 0257  Swedish special edition: Chapter 3 Volume 10 P. 0199  Spanish special edition: Chapter 03 Volume 16 P. 0048  Portuguese special edition Chapter 03 Volume 16 P. 0048  Special edition in Czech Chapter 3 Volume 04 P. 48  - 48 Special edition in Estonian Chapter 3 Volume 04 P. 48  - 48 Special edition in Hungarian Chapter 3 Volume 04 P. 48  - 48 Special edition in Lithuanian Chapter 3 Volume 04 P. 48  - 48 Special edition in Latvian Chapter 3 Volume 04 P. 48  - 48 Special edition in Maltese Chapter 3 Volume 04 P. 48  - 48 Special edition in Polish Chapter 3 Volume 04 P. 48  - 48 Special edition in Slovakian Chapter 3 Volume 04 P. 48  - 48 Special edition in Slovenian Chapter 3 Volume 04 P. 48  - 48

		Council Directiveof 5 March 1979amending Directive 77/504/EEC on pure-bred breeding animals of the bovine species(79/268/EEC)THE COUNCIL OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Economic Community, and in particular Articles 43 and 100 thereof,Having regard to the proposal from the Commission [1],Having regard to the opinion of the European Parliament [2],Having regard to the opinion of the Economic and Social Committee [3],Whereas Council Directive 77/504/EEC of 25 July 1977 on pure-bred breeding animals of the bovine species [4] laid down the conditions for the progressive liberalization of intra-Community trade in this field;Whereas, pending the implementation of Community rules on the subject, the general principle has been adopted in accordance with Article 7 of the said Directive that imports from non-member States should not enjoy more favourable conditions than those applying to intra-Community trade;Whereas Community rules concerning trade between Member States have not yet been fully established, in particular as regards the criteria for entry in a herd-book; whereas they will not be so established until a number of implementing measures, particularly those provided for in Article 6 of the abovementioned Directive have been adopted; whereas provision should therefore be made for Article 7 of that Directive to be applied as and when intra-Community arrangements are introduced,HAS ADOPTED THIS DIRECTIVE:Article 1Article 9 of Directive 77/504/EEC shall be replaced by the following:"Article 9The Member States shall bring into force the laws, regulations and administrative provisions necessary to:(a) comply with this Directive, with the exception of Article 7, by 1 January 1979 at the latest;(b) comply with Article 7, as regards each of the points which it covers, on the same dates as those on which they comply with the corresponding provisions applicable in intra-Community trade, and in particular the decisions that are successively adopted pursuant to Article 6.They shall forthwith inform the Commission thereof".Article 2This Directive is addressed to the Member States.Done at Brussels, 5 March 1979.For the CouncilThe PresidentP. Mehaignerie[1] OJ No C 9, 11. 1. 1979, p. 4.[2] Opinion delivered on 16 February 1979 (not yet published in the Official Journal).[3] Opinion delivered on 21 and 22 February 1979 (not yet published in the Official Journal).[4] OJ No L 206, 12. 8. 1977, p. 8.--------------------------------------------------