diff --git "a/36_years1985-10.jsonl" "b/36_years1985-10.jsonl"
new file mode 100644--- /dev/null
+++ "b/36_years1985-10.jsonl"
@@ -0,0 +1,464 @@
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/97226364-a0a8-4665-aad7-64f1d25d5fcd", "title": "First Commission Directive 85/503/EEC of 25 October 1985 on methods of analysis for edible caseins and caseinates", "langIdentifier": "ENG", "mtypes": "fmx4,html,pdfa1b,print,xhtml", "workTypes": "http://publications.europa.eu/ontology/cdm#directive,http://publications.europa.eu/ontology/cdm#legislation_secondary,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Commission", "date": "1985-10-25", "subjects": "analytical chemistry,approximation of laws,food chemistry,milk by-product", "workIds": "celex:31985L0503,oj:JOL_1985_308_R_0012_011", "eurovoc_concepts": ["analytical chemistry", "approximation of laws", "food chemistry", "milk by-product"], "url": "http://publications.europa.eu/resource/cellar/97226364-a0a8-4665-aad7-64f1d25d5fcd", "lang": "eng", "formats": ["fmx4", "html", "pdfa1b", "print", "xhtml"], "text": "L_1985308EN. 01001201. xml\n\n\n\n\n\n\n\n\n\n\n20. 11. 1985\u00a0\u00a0\u00a0\n\n\nEN\n\n\nOfficial Journal of the European Communities\n\n\nL 308/12\n\n\n\n\n\nFIRST COMMISSION DIRECTIVE\nof 25 October 1985\non methods of analysis for edible caseins and caseinates\n(85/503/EEC)\nTHE COMMISSION OF THE EUROPEAN COMMUNITIES,\nHaving regard to the Treaty establishing the European Economic Community,\nHaving regard to Council Directive 83/417/EEC of 25 July 1983 on the approximation of the laws of the Member States relating to certain lactoproteins (caseins and caseinates) intended for human consumption\u00a0(1), and in particular Article 9 (b) thereof;\nWhereas Article 9 (b) of Directive 83/417/EEC requires that Community methods of analysis be determined for checking the composition of certain edible caseins and caseinates;\nWhereas it is possible to adopt an initial series of methods in respect of which studies have been completed;\nWhereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Foodstuffs,\nHAS ADOPTED THIS DIRECTIVE:\nArticle 1\nMember States shall take all measures necessary to ensure that the analyses necessary for verification of the criteria set out in Annex I are carried out in accordance with the methods described in Annex II. Article 2\nMember States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive by 1 May 1987 at the latest. They shall forthwith inform the Commission thereof. Article 3\nThis Directive is addressed to the Member States. Done at Brussels, 25 October 1985. For the Commission\n\nCOCKFIELD\n\nVice-President\n\n\n\n\n\n(1)\u00a0\u00a0OJ No L 237, 26. 8. 1983, p. 25. ANNEX I\nSCOPE OF THE FIRST COMMUNITY METHODS OF ANALYSIS DIRECTIVE FOR EDIBLE CASEINS AND CASEINATES\n\n\n\n\n\n\n\nI. General Provisions\n\n\n\n\n\n\n\n\n\n\n\n\nII. Determination of moisture in:\n\n\n\n\n\n\n\n\u2014\n\n\nacid caseins using method 1, Annex II\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nrennet caseins using method 1, Annex II\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ncaseinates using method 1, Annex II\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\nIII. Determination of protein content in:\n\n\n\n\n\n\n\n\u2014\n\n\nacid caseins using method 2, Annex II\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nrennet caseins using method 2, Annex II\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ncaseinates using method 2, Annex II\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\nIV. Determination of titratable acidity in:\n\n\n\n\n\n\n\n\u2014\n\n\nacid caseins using method 3, Annex II\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\nV. Determination of ash (including P2O5) in:\n\n\n\n\n\n\n\n\u2014\n\n\nacid caseins using method 4, Annex II\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nrennet caseins using method 5, Annex II\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\nVI. Determination of pH in:\n\n\n\n\n\n\n\n\u2014\n\n\ncaseinates using method 6, Annex II\n\n\n\n\n\n\n\n\n\n\n\nANNEX II\nMETHODS OF ANALYSIS RELATING TO THE COMPOSITION OF EDIBLE CASEINS AND CASEINATES\n\nGENERAL PROVISIONS\n\n1. PREPARATION OF THE ANALYSIS SAMPLE\n1. 1. General\n\nThe mass of the sample presented to the laboratory for analysis shall be at least 200 grams. 1. 2. Preparation of the sample for analysis in the laboratory\n\n\n\n\n\n\n\n\n\n1. 2. 1. Thoroughly mix and break down any lumps, etc. , in the laboratory sample by repeatedly shaking and inverting the container (if necessary, after having transferred all of the laboratory sample to an air-tight container of sufficient capacity (twice Volume of sample) to allow this operation to be carried out). 1. 2. 2. Transfer a representative portion of the sample, i. e. about 50 grams of the thoroughly mixed laboratory sample (1. 2. 1) to the test sieve (3. 3). 1. 2. 3. If the 50 gram portion completely or almost completely passes (at least 95 % by weight) through the sieve (3. 3), use for the determination the sample as prepared in 1. 2. 1. 1. 2. 4. Otherwise, grind the 50 gram portion, using the grinding device (3. 4), until it satisfies the sieving criterion (1. 2. 3). Immediately transfer all the sieved sample to an air-tight container of sufficient capacity (twice volume of sample) and mix thoroughly by repeated shaking and inverting. During these operations, take precautions to avoid any change in the moisture content of the product. 1. 2. 5. After the test sample has been prepared, any determination should be proceeded with as soon as possible. 1. 3. Containers\n\nThe sample shall always be kept in an air-tight and moisture-tight container. 2. REAGENTS\n2. 1. Water\n\n\n\n\n\n\n\n\n\n2. 1. 1. Wherever mention is made to water for solution, dilution or washing purposes, distilled water, or de-mineralized water of at least equivalent purity, shall be used. 2. 1. 2. Wherever reference is made to \u2018solution\u2019 or \u2018dilution\u2019 without further indication, \u2018solution in water\u2019 or \u2018dilution with water\u2019 is meant. 2. 2. Chemicals\n\nAll chemicals used shall be of recognized analytical reagent quality except where otherwise specified. 3. EQUIPMENT\n3. 1. Lists of equipment\n\nThe lists of equipment contain only those items with a specialized use and items to a particular specification. 3. 2. Analytical balance\n\nAnalytical balance means a balance capable of weighing to at least 0,1 mg. 3. 3. Test sieve\n\nThe test ieves to be used are to be fitted with a lid, to be of diameter 200 mm, to be constructed of wire cloth with a nominal aperture size of 500 urn. The aperture tolerances and wire diameters to be permitted are as given in ISO 3310/1. (Test sieves \u2014 Technical requirements and testing \u2014 Part 1: Metal wire cloth. ISO 3310/1 \u2014 1975). The sieves are to be fitted with a receiver. 3. 4. Grinding device\n\nFor grinding the laboratory sample if necessary (see 1. 2. 4), without development of undue heat and without loss or absorption of moisture, a hammer mill shall not be used. 4. EXPRESSION OF RESULTS\n4. 1. Results\n\nThe result stated in the analytical report is to be the mean value obtained from two determinations which satisfy the repeatability criterion for that method. 4. 2. Calculation of percentage\n\nExcept where otherwise specified, the result shall be calculated as a percentage by mass of the sample. 5. TEST REPORT\nThe test report shall identify the method of analysis used as well as the results obtained. In addition, it shall mention all details of procedure not specified in the method of analysis or which are optional, as well as any circumstances that may have influenced the results obtained. The test report shall give all the information necessary for the complete identification of the sample. METHOD 1\n\nDETERMINATION OF MOISTURE CONTENT\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method determines the moisture content in:\n\n\n\n\n\n\n\u2014\n\n\nacid caseins\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nrennet caseins\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ncaseinates\n\n\n\n\n2. DEFINITION\nThe moisture content of caseins and caseinates: the loss of mass as determined by the method specified. 3. PRINCIPLE\nThe residual mass of a test portion is determined after drying at atmospheric pressure in an oven at 102 oC \u00b1 1 oC to constant mass. The loss of mass is calculated as a percentage by mass of the sample. 4. APPARATUS\n4. 1. Analytical balance\n\n\n\n\n\n\n\n\n\n4. 2. Dishes, flat-bottomed and of material non-corrodible under the conditions of test e. g. nickel, aluminium, stainless steel or glass. The dishes must have lids which fit tightly but which can readily be removed. Suitable dimensions are: diameter 60 to 80 mm and depth about 25 mm. 4. 3. Atmospheric pressure drying oven, well ventilated, thermostatically controlled with temperature regulation (at 102 oC \u00b1 1 oC). The temperature should be uniform throughout the oven. 4. 4. Desiccator, containing freshly activated silica gel with a water content indicator or an equivalent desiccant. 4. 5. Suitable device for handling dishes, e. g. laboratory tongs. 5. PROCEDURE\n5. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 5. 2. Preparation of the dish\n\n\n\n\n\n\n\n\n\n5. 2. 1. Heat the uncovered dish and its lid (4. 2) in the oven (4. 3), controlled at 102 oC \u00b1 1 oC, for at least one hour. 5. 2. 2. Place the lid on the dish, transfer the covered dish to the desiccator (4. 4), allow to cool to the temperature of the balance room and weigh to the nearest 0,1 mg (m0). 5. 3. Test portion\n\nPlace 3 to 5 grams of the test sample (5. 1) into the dish, cover with the lid and weigh to the nearest 0,1 mg (m1). 5. 4. Determination\n\n\n\n\n\n\n\n\n\n5. 4. 1. Uncover the dish and place it with its lid in the oven (4. 3), controlled at 102 oC \u00b1 1 oC, for four hours. 5. 4. 2. Replace the lid on the dish, transfer to the desiccator, allow to cool to the temperature of the balance room and weigh to the nearest 0,1 mg. 5. 4. 3. Uncover the dish and heat it again, with its lid, in the oven for one hour. Then repeat operation 5. 4. 2. 5. 4. 4. If the mass obtained in 5. 4. 3 is less than the mass obtained in 5. 4. 2 by more than 1 mg, repeat operation 5. 4. 3. If an increase in mass occurs, use the lowest recorded mass in the calculation (6. 1). Let the final weight recorded be m2g. The total drying time should not normally exceed six hours. 6. EXPRESSION OF RESULTS\n6. 1. Method of calculation\n\nThe loss of mass on drying of the sample, expressed as a percentage by mass, is given by:\n\n\n\n\u00d7\n\n\n\n\n\n\n\nm0\n\n\n\n=\n\n\nmass, in g of the dish and its lid after process 5. 2;\n\n\n\n\nm1\n\n\n\n=\n\n\nmass, in g of the dish, its lid and the test portion before drying (process 5. 3);\n\n\n\n\nm2\n\n\n\n=\n\n\nmass, in g of the dish, its lid and the test portion after drying (process 5. 4. 3 or 5. 4. 4). Calculate the loss on drying to the nearest 0,01 %. 6. 2. Repeatability\n\nThe difference in results between two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,1 g of moisture per 100 grams of product. This repeatability interval should be achieved in 95 % of the times that the method is carried out. METHOD 2\n\nDETERMINATION OF PROTEIN CONTENT\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method determines the protein content of:\n\n\n\n\n\n\n\u2014\n\n\nacid caseins,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nrennet caseins,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ncaseinates,\n\n\n\n\nexcept those containing ammonium caseinate or other ammonium or nitrogenous non-protein compounds. 2. DEFINITION\nThe protein content: the nitrogen content as determined by the method specified and then multiplied by 6,38 and expressed as a percentage by mass. 3. PRINCIPLE\nA test portion is digested with a mixture of potassium sulphate and sulphuric acid, in the presence of copper (II) sulphate as catalyst, to convert organic nitrogen to ammoniacal nitrogen. The ammonia is distilled and absorbed into boric acid solution and then titrated with standard hydrochloric acid solution. The nitrogen content is converted to protein content by multiplying by 6,38. 4. REAGENTS\n\n\n\n\n\n\n\n\n4. 1. Sulphuric acid, concentrated, S2O 1,84 g/ml. 4. 2. Potassium sulphate, anhydrous (K2SO4). 4. 3. Copper (II) sulphate pentahydrate (CuSO45H2O). 4. 4. Sucrose (C12H22O11). 4. 5. Boric acid, 40-g/l solution. 4. 6. Sodium hydroxide, concentrated aqueous solution 30 % (m/m), carbonate free. 4. 7. Hydrochloric acid, 0,1 mol/1. 4. 8. Mixed indicator. Mix equal volumes of a 2 g/1 solution of methyl red in at least 95 % (V/V) ethanol and a 1 g/1 solution of methylene blue in at least 95 % (V/V) ethanol. 5. APPARATUS\n5. 1. Analytical balance\n\n\n\n\n\n\n\n\n\n5. 2. Kjeldahl flask, 500 ml capacity. 5. 3. Digestion apparatus to hold the Kjeldahl flask (5. 2) in an inclined position and with a heating device which will not heat the part of the flask above the surface of the liquid contents. 5. 4. Condenser with straight inner tube. 5. 5. Outlet tube with safety bulb connected to the lower end of the condenser (5. 4) by a ground glass joint or a rubber tube. If rubber tubing is used, the glass ends must be near one another. 5. 6. Splash-head connected to the Kjeldahl flask (5. 2) and to the condenser (5. 4) by soft, close-fitting rubber or other appropriate stoppers. 5. 7. Conical flask, 500 ml capacity. 5. 8. Graduated cylinders, 50 ml and 100 ml capacity. 5. 9. Burette, 50 ml capacity, graduated in 0,1 ml. 5. 10. Boiling aids:\n\n\n\n\n\n\n\n\n\n5. 10. 1. For the digestion: small pieces of hard porcelain, or glass beads. 5. 10. 2. For the distillation; freshly calcined pieces of pumice. 6. PROCEDURE\n6. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 6. 2. Test for presence of ammoniacal nitrogen\n\nIf the presence of ammonium caseinate or other ammonium compounds is suspected, carry out the following test. Add to 1 gram of sample in a small conical flask 10 ml of water and 100 mg of magnesium oxide. Rinse down any magnesium oxide adhering to the walls and close the flask with a cork stopper, inserting a piece of moistened red litmus paper between the stopper and the neck of the flask. Mix the contents of the flask carefully and heat the flask in a water bath at 60 to 65 o C. If the litmus paper colours blue within 15 minutes ammonia is present, and the method is not applicable (see Section 1). 6. 3. Blank test\n\nAt the same time as the determination of the nitrogen content of the sample perform a blank determination using 0,5 grams of the sucrose (4. 4) instead of the test portion, using the same apparatus, the same quantities of all reagents and the same procedure as described in 6. 5. If the titration in the blank determination exceeds 0,5 ml of 0,1 mol/1 acid, the reagents shall be checked and the impure reagent or reagents purified or replaced. 6. 4. Test portion\n\nTransfer to the Kjeldahl flask (5. 2) 0,3 to 0,4 grams of the test sample (6. 1), weighed to the nearest 0,1 mg. 6. 5. Determination\n\n\n\n\n\n\n\n\n\n6. 5. 1. Transfer to the flask a few pieces of porcelain or a few glass beads (5. 10. 1) and about 10 grams of the anhydrous potassium sulphate (4. 2). Add 0,2 g of the copper (II) sulphate (4. 3) and wash down the neck of the flask with a little water. Add 20 ml of the concentrated sulphuric acid (4. 1). Mix the contents of the flask. Heat gently on the digestion apparatus (5. 3) until any frothing has ceased, boil gently until the solution is clear and a pale green-blue colour persists. During heating, swirl the flask occasionally. Continue the boiling, regulating the heating so as to condense the vapours in the middle of the flask neck. Continue the heating for 90 minutes avoiding local overheating. Allow to cool to room temperature. Carefully add about 200 ml of water and a few pieces of pumice (5. 10. 2). Mix and cool again. 6. 5. 2. Transfer into the conical flask (5. 7) 50 ml of the boric acid solution (4. 5) and four drops of the indicator (4. 8). Mix. Place the conical flask under the condenser (5. 4) so that the tip of the outlet tube (5. 5) is immersed in the boric acid solution. Using a graduated cylinder (5. 8), add to the Kjeldahl flask 80 ml of the sodium hydroxide solution (4. 6). During this operation, hold the flask in an inclined position so that the sodium hydroxide solution runs down the side of the flask to form a bottom layer. Immediately connect the Kjeldahl flask to the condenser by means of the splash-head (5. 6). Gently rotate the Kjeldahl flask to mix its contents. Boil gently at first, avoiding any frothing. Continue the distillation so that 150 ml of distillate are collected in approximately 30 minutes. The distillate should have a temperature below 25 o C. About two minutes before the end of the distillation, lower the conical flask so that the tip of the outlet tube is no longer immersed in the acid solution, and rinse the tip with a little water. Stop heating, remove the outlet tube and rinse its outer and inner walls with a little water, collecting the washings in the conical flask. 6. 5. 3. Titrate the distillate in the conical flask, using the standard volumetric hydrochloric acid solution (4. 7). 7. EXPRESSION OF RESULTS\n7. 1. Formula and method of calculation\n\nThe protein content of the sample, expressed as a percentage by mass, is given by:\n\n\n\nwhere:\n\n\n\n\n\n\nV1\n\n\n\nis the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4. 7) used in the determination (6. 5);\n\n\n\n\nV2\n\n\n\nis the volume, in millilitres, of the standard volumetric hydrochloric acid solution (4. 7) used in the blank test (6. 3);\n\n\n\n\nT\n\n\nis the strength of the standard volumetric hydrochloric acid solution (4. 7) in mol/1;\n\n\n\n\nm\n\n\nis the mass, in grams, of the test portion. Calculate the protein content to the nearest 0,1 %. 7. 2. Repeatability\n\nThe difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst under the same conditions shall not exceed 0,5 grams of protein per 100 grams of product. This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out. METHOD 3\n\nDETERMINATION OF TITRATABLE ACIDITY\n\n1. SCOPE AND FIELD OF APPLICATION\nThe method determines the titratable acidity of:\n\n\n\n\n\n\n\u2014\n\n\nacid caseins. 2. DEFINITION\nThe titratable acidity of acid caseins: the volume in millilitres, of a 0,1 mol/1 standard sodium hydroxide solution required to neutralize an aqueous extract of 1 gram of the product. 3. PRINCIPLE\nAn aqueous extract of the sample at 60 o C is obtained and filtered. The filtrate is titrated against standard sodium hydroxide using phenolphtalein indicator. 4. REAGENTS\nAny water used in the method procedure or in the preparation of reagents shall be freed from carbon dioxide by boiling for 10 minutes before use. 4. 1. Sodium hydroxide solution: 0,1 Mol/1. 4. 2. Phenolphtalein indicator solution, 10 g/1 in ethanol (95 % V/V) neutralized to the indicator. 5. APPARATUS\n5. 1. Analytical balance\n\n\n\n\n\n\n\n\n\n5. 2. Conical flask, 500 ml capacity, with ground neck and fitted with a ground glass stopper. 5. 3. One-mark pipette, 100 ml capacity. 5. 4. Pipette, suitable for measuring 0,5 ml of indicator solution (4. 2). 5. 5. Conical flask, 250 ml capacity. 5. 6. Measuring cylinder, 250 ml capacity. 5. 7. Burette, graduated in 0,1 ml. 5. 8. Water bath, capable of being controlled at a temperature of 60 oC \u00b1 2 oC. 5. 9. Appropriate filter\n\n\n\n\n6. PROCEDURE\n6. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 6. 2. Test portion\n\nWeigh about 10 grams of the test sample (6. 1) to the nearest 10 mg and transfer it to the conical flask (5. 2). 6. 3. Determination\n\nUsing the 250 ml measuring cylinder (5. 6), add 200 ml of freshly boiled and cooled water, previously heated to 60 o C. Stopper the flask, mix by swirling and place in the water bath at 60 o C (5. 8) for 30 minutes. Shake the flask at intervals of about 10 minutes. Filter, and cool the filtrate to about 20 oC. The filtrate must be clear. Transfer 100 ml of the cooled filtrate into the conical flask (5. 5), using the pipette (5. 3). Add 0,5 ml of the phenolphtalein indicator solution (4. 2), using the pipette (5. 4). Titrate with the standard volumetric sodium hydroxide solution (4. 1), until the appearance of a faint pink colour, persisting for at least 30 seconds. Determine and record the volume used to the nearest 0,01 ml. 7. EXPRESSION OF RESULTS\n7. 1. Formula and method of calculation\n\nThe titratable acidity of the acid casein is given by:\n\n\n\nwhere:\n\n\n\n\n\n\nV\n\n\nis the volume, in millilitres, of the standard volumetric sodium hydroxide solution (4. 1) used;\n\n\n\n\nT\n\n\nis the strength of the standard volumetric sodium hydroxide solution (4. 1) in mol/1;\n\n\n\n\nm\n\n\nis the mass, in grams, of the test portion. Calculate the titratable acidity to two decimal places. 7. 2. Repeatability\n\nThe difference in results between two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,02 ml of 0,1 mol/1 sodium hydroxide per 1 gram of product. This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out. METHOD 4\n\nDETERMINATION OF ASH (including P2O5)\n\n1. SCOPE AND FIELD OF APPLICATION\nThe method determines the ash (including P2O5) content of:\n\n\n\n\n\n\n\u2014\n\n\nacid caseins\n\n\n\n\n2. DEFINITION\nThe ash (including P2O5) content: the content of ash as determined by the method specified. 3. PRINCIPLE\nA portion of the sample is incinerated at 825 o C \u00b1 25 o C in the presence of magnesium acetate to bind all phosphorus of organic origin. The final ash is calculated after the weighing of the residue and subtraction of the mass of ash originating from the magnesium acetate. 4. REAGENTS\n\n\n\n\n\n\n\n\n4. 1. Magnesium acetate tetrahydrate solution, 120 g/1. Dissolve 120 grams of magnesium acetate tetrahydrate [Mg (CH3 CO2)2 4 H2 O] in water and make up one litre with water. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Analytical balance\n\n\n\n\n\n\n\n\n\n\n\n\n5. 2. One-mark pipette, 5 ml. 5. 3. Silica or platinum dishes, about 70 mm diameter and 25 to 50 mm deep. 5. 4. Drying oven, capable of being controlled at 102 oC \u00b1 1 oC. 5. 5. Electrical furnace, capable of being controlled at 825 oC \u00b1 25 oC. 5. 6. Boiling water bath\n\n\n\n\n\n\n\n\n\n\n\n\n5. 7. Desiccator containing freshly activated silica gel with a water content indicator or an equivalent desiccant. 6. PROCEDURE\n6. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 6. 2. Preparation of the dishes\n\nHeat two dishes (A,B) (5. 3) in the electrical furnace (5. 5), controlled at 825 o C \u00b1 25 o C, for 30 minutes. Allow the dishes to cool somewhat and then place in the desiccator (5. 7) to the temperature of the balance room and weigh to the nearest 0,1 mg. 6. 3. Test portion\n\nWeigh, to the nearest 0,1 mg approximately 3 grams of the test sample (6. 1), directly into one of the prepared dishes (A). 6. 4. Determination\n\nUsing the pipette (5. 2), add to the dish (A) exactly 5 ml of the magnesium acetate solution (4. 1) so as to wet all of the test portion, and allow to stand for 20 minutes. To the other prepared dish (B), add with the pipette (5. 2) exactly 5 ml of the magnesium acetate solution (4. 1). Evaporate the contents of both dishes (A and B) to dryness on the boiling water bath (5. 6). Place both dishes in the oven (5. 4), controlled at 102 oC \u00b1 1 oC, for 30 minutes. Heat dish A with its contents on a low flame, a hot plate or under an I/R lamp, until the test portion is completely charred, taking care that it does not burst into flame. Transfer both dishes (A and B) to the electrical furnace (5. 5), controlled at 825 oC \u00b1 25 oC, and heat for at least one hour until all carbon has disappeared from dish A. Allow both dishes to cool somewhat and then place in the desiccator (5. 7) to the temperature of the balance room and weigh to the nearest 0,1 mg. Repeat the operations of heating for approximately 30 minutes, in the electrical furnace (5. 5), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass. 7. EXPRESSION OF RESULTS\n7. 1. Method of calculation\n\nThe content of ash, including P2O5, in the sample, as a percentage by mass, is given by:\n\n\n\nwhere:\n\n\n\n\n\n\nm0\n\n\n\nis the mass, in grams, of the test portion;\n\n\n\n\nm1\n\n\n\nis the mass, in grams, of dish A and residue;\n\n\n\n\nm2\n\n\n\nis the mass, in grams, of the prepared dish A;\n\n\n\n\nm3\n\n\n\nis the mass, in grams, of dish B and residue;\n\n\n\n\nm4\n\n\n\nis the mass, in grams, of the prepared dish B. Calculate the final result to the nearest 0,01 %. 7. 2. Repeatability\n\nThe difference in results between the determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,1 grams per 100 grams of product. The repeatability interval should be achieved in 95 % of the times that the method is correctly carried out. METHOD 5\n\nDETERMINATION OF ASH (including P2O5)\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method determines the ash (including P2O\n5) content of:\n\n\n\n\n\n\n\u2014\n\n\nrennet casein\n\n\n\n\n2. DEFINITION\nThe ash (including P2O5) content: the content of ash as determined by the method specified. 3. PRINCIPLE\nA portion of the sample is incinerated at 825 oC \u00b1 25 oC to constant mass. The residue is determined by weighing and calculated as a percentage by mass of the sample. 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Analytical balance\n\n\n\n\n\n\n\n\n\n\n\n\n4. 2. Silica or platinum dish, about 70 mm diameter and 25 to 50 mm deep. 4. 3. Electrical furnace with air circulation, capable of being controlled at 825 oC \u00b1 25 oC. 4. 4. Desiccator, containing freshly activated silica gel with a water content indicator or an equivalent desiccant. 5. PROCEDURE\n5. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 5. 2. Preparation of the dish\n\nHeat the dish (4. 2) in the electrical furnace (4. 3), controlled at 825 oC \u00b1 25 oC, for 30 minutes. Allow the dish to cool somewhat and then place in the desiccator (4. 4) to the temperature of the balance room and weigh to the nearest 0,1 mg. 5. 3. Test portion\n\nWeigh, to the nearest 0,1 mg approximately 3 grams of the test sample (5. 1) directly into the prepared dish. 5. 4. Determination\n\nHeat the dish with its contents on a low flame, a hot plate or an I/R lamp until the test portion is completely charred, taking care that it does not burst into flame. Transfer the dish to the electrical furnace (4. 3), controlled at 825 oC \u00b1 25 oC, and heat for at least one hour until all carbon has disappeared from the dish. Allow the dish to cool somewhat and then place in the desiccator (4. 4) to the temperature of the balance room and weigh to the nearest 0,1 mg. Repeat the operations of heating for approximately 30 minutes, in the electrical furnace (4. 3), cooling and weighing, until the mass remains constant to within 1 mg or begins to increase. Record the minimum mass. 6. EXPRESSION OF RESULTS\n6. 1. Method of calculation and formula\n\nThe ash content of the sample, including P2O5, as a percentage per mass, is given by:\n\n\n\nwhere:\n\n\n\n\n\n\nm0\n\n\n\nis the mass, in grams, of the test portion;\n\n\n\n\nm1\n\n\n\nis the mass, in grams, of the dish and residue;\n\n\n\n\nm2\n\n\n\nis the mass, in grams, of the prepared dish. Calculate the final result to the nearest 0,01 %. 6. 2. Repeatability\n\nThe difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,15 grams of ash per 100 grams of product. This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out. METHOD 6\n\nDETERMINATION OF pH\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method determines the pH of:\n\n\n\n\n\n\n\u2014\n\n\ncaseinates. 2. DEFINITION\nThe pH of caseinates: the pH, at 20 oC, of an aqueous solution of caseinates, as determined by the method specified. 3. PRINCIPLE\nThe electrometric determination of pH of an aqueous solution of caseinate, using a pH meter. 4. REAGENTS\nAny water used in the preparation of the reagents or in the Procedure (6) shall be recently distilled water that has been protected from carbon dioxide absorption. 4. 1. Buffer solutions, for calibration of the pH meter (5. 2)\nTwo standard buffer solutions with pH values at 20 oC which are known to the second decimal place and will bracket the pH value of the sample under test, for example phtalate buffer solution of pH approximately 4 and a borax buffer solution of pH approximately 9. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Balance, accuracy 0,1 grams. 5. 2. pH meter, minimum sensitivity 0,05 pH unit, with a suitably calibrated elecrode, e. g. glass electrode and a calomel or other reference electrode. 5. 3. Thermometer, accuracy 0,5 oC. 5. 4. Conical flask, capacity 100 ml, fitted with a ground glass stopper. 5. 5. Beaker, capacity 50 ml. 5. 6. Mixer\n\n\n\n\n\n\n\n\n\n5. 7. Beaker, for the mixer (5. 6) of at least 250 ml capacity. 6. PROCEDURE\n6. 1. Preparation of the test sample\n\nAs described in Section 1. 2 of the General Provisions. 6. 2. Determination\n\n6. 2. 1. Calibration of pH meter\n\nAdjust the temperature of the buffer solutions (4. 1) to 20 oC and calibrate the pH meter in accordance with the manufacturer's instructions. NOTES\n\n\n\n\n\n\n\n1. The calibration should be carried out while the flasks are standing for 20 mintues (see 6. 2. 2). 2. If a series of samples is being tested, check the calibration of the pH meter with one or more of the standard buffer solutions at least every 30 minutes. 6. 2. 2. Preparation of the test solution\n\nTransfer to the beaker (5. 7) 95 ml of water, add 5,0 grams of the test sample (6. 1), and mix using the mixer (5. 6) for 30 seconds. Allow to stand for 20 minutes at about 20 oC, covered with a watch glass. 6. 2. 3. Measurement of pH\n\n\n\n\n\n\n\n\n\n6. 2. 3. 1. Pour about 20 ml of the solution into the beaker (5. 5) and immediately determine the pH of this liquid, using the pH meter (5. 2) after having rinsed the glass electrode carefully with water. 6. 2. 3. 2. Measure the pH. 7. EXPRESSION OF RESULTS\n7. 1. Recording of pH\n\nRecord, as the pH of the aqueous solution of caseinate, the value read from the dial of the pH meter to at least two decimal places. 7. 2. Repeatability\n\nThe difference between the results of two determinations carried out simultaneously or in rapid succession on the same sample, by the same analyst, under the same conditions, shall not exceed 0,05 pH unit. This repeatability interval should be achieved in 95 % of the times that the method is correctly carried out"}
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/bfcd48c2-b003-4198-b971-e0ecbec51360", "title": "Commission Regulation (EEC) No 2894/85 of 17 October 1985 amending Regulations (EEC) No 2121/85 and (EEC) No 2122/85 as regards the time limit for the purchase of pigmeat by the Belgian intervention agency", "langIdentifier": "ENG", "mtypes": "html,pdfa1b,print", "workTypes": "http://publications.europa.eu/ontology/cdm#legislation_secondary,http://publications.europa.eu/ontology/cdm#regulation,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Commission", "date": "1985-10-17", "subjects": "intervention buying,pigmeat,storage", "workIds": "celex:31985R2894,oj:JOL_1985_278_R_0011_011", "eurovoc_concepts": ["intervention buying", "pigmeat", "storage"], "url": "http://publications.europa.eu/resource/cellar/bfcd48c2-b003-4198-b971-e0ecbec51360", "lang": "eng", "formats": ["html", "pdfa1b", "print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/3779fcec-a2c1-4956-b83f-c150a5789ae8", "title": "Council Regulation (EEC) No 2919/85 of 17 October 1985 laying down the conditions for access to the arrangements under the Revised Convention for the navigation of the Rhine relating to vessels belonging to the Rhine Navigation", "langIdentifier": "ENG", "mtypes": "fmx4,html,pdfa1b,print,xhtml", "workTypes": "http://publications.europa.eu/ontology/cdm#legislation_secondary,http://publications.europa.eu/ontology/cdm#regulation,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "Council of the European Union", "date": "1985-10-17", "subjects": "inland waterway shipping,international convention,navigational code", "workIds": "celex:31985R2919,oj:JOL_1985_280_R_0004_005", "eurovoc_concepts": ["inland waterway shipping", "international convention", "navigational code"], "url": "http://publications.europa.eu/resource/cellar/3779fcec-a2c1-4956-b83f-c150a5789ae8", "lang": "eng", "formats": ["fmx4", "html", "pdfa1b", "print", "xhtml"], "text": "L_1985280EN. 01000401. xml\n\n\n\n\n\n\n\n\n\n\n22. 10. 1985\u00a0\u00a0\u00a0\n\n\nEN\n\n\nOfficial Journal of the European Communities\n\n\nL 280/4\n\n\n\n\n\nCOUNCIL REGULATION (EEC) No 2919/85\nof 17 October 1985\nlaying down the conditions for access to the arrangements under the Revised Convention for the navigation of the Rhine relating to vessels belonging to the Rhine Navigation\nTHE COUNCIL OF THE EUROPEAN COMMUNITIES,\nHaving regard to the Treaty establishing the European Economic Community, and in particular Article 75 thereof,\nHaving regard to the proposal from the Commission,\nHaving regard to the opinion of the European Parliament\u00a0(1),\nHaving regard to the opinion of the Economic and Social Committee\u00a0(2),\nWhereas the six Contracting States to the Revised Convention for the navigation of the Rhine, that is to say five Member States of the European Communities (Belgium, Germany, France, the Netherlands and the United Kingdom) and Switzerland amended that Convention by Additional Protocol 2 signed in Strasbourg on 17 October 1979;\nWhereas the said Additional Protocol stipulates that only vessels belonging to the Rhine Navigation shall be authorized to transport merchandise and persons between two points situated on the navigable inland waterways referred to in the first paragraph of Article 3 of the Convention; whereas vessels are considered to belong to the Rhine Navigation if they carry a document issued by the competent authority;\nWhereas the Protocol of Signature to the abovementioned Additional Protocol provides that the document certifying that a vessel belongs to the Rhine Navigation shall be issued by the competent authority of the State concerned only to vessels which have with that State a genuine link the constituent factors of which are to be determined on the basis of equal treatment between Contracting States to the Convention; whereas, under the terms of the Protocol of Signature, the same treatment must be accorded to vessels which have a genuine link with any Member State; whereas, to that effect, these other Member States are accorded equal status with the Contracting States to the Convention;\nWhereas the Contracting States to the Convention have drawn up, within the Central Commission for the Navigation of the Rhine (CCR), implementing provisions determining the conditions under which the abovementioned document should be issued; whereas, by Decision of 8 November 1984, the Council, acting on a proposal from the Commission, defined the common action under which Member States which are Contracting Parties to the Convention adopted these provisions in the form of a resolution of the CCR;\nWhereas, in order to ensure that the implementing provisions are put into effect throughout the Community, it is necessary to incorporate them into Community law by means of a Council Regulation adopted under Article 75 of the Treaty fixing the detailed rules required to take into account Community rules and procedures;\nWhereas provision should be made for Member States to send the Commission a copy of the information they send the CCR in accordance with this Rgulation,\nHAS ADOPTED THIS REGULATION:\nArticle 1\nThe provisions contained in the Annex shall be applicable in the Community in accordance with the provisions of this Regulation. Article 2\n1. For the purposes of implementing Articles 2 (4) and 8 (1) of the Annex, each Member State shall at the same time send to the Commission the information which it must send to the CCR under the terms of those provisions. 2. For the purpose of implementing the first sentence of Article 3 (4) of the Annex, the Member State concerned shall also forward to the Commission a copy of the dossier concerning its request for consultation of the CCR. Article 3\nIf the CCR should envisage establishing the general conditions referred to in the second sentence of Article 3 (4) of the Annex, the Council, acting by a qualified majority on a proposal from the Commission, shall decide on the joint position to be adopted within the CCR by the Member States which are also Contracting Parties to the Convention. These conditions will be introduced in the appropriate way at Community level by the Council acting in accordance with the arrangements set out in the first paragraph. Article 4\nThis Regulation shall enter into force on the day of its publication in the Official Journal of the European Communities. However, Article 7 (2) of the Annex shall not apply until 1 February 1987. This Regulation shall be binding in its entirety and directly applicable in all Member States. Done at Luxembourg, 17 October 1985. For the Council\n\n\nThe President\n\nJ. F. POOS\n\n\n\n\n(1)\u00a0\u00a0OJ No C 262, 14. 10. 1985. (2)\u00a0\u00a0OJ No C 169, 8. 7. 1985, p. 7. ANNEX\nREGULATION IMPLEMENTING\nthe provisions of the third paragraph of Article 2 of the Revised Convention for the navigation of the Rhine and of paragraphs 1 and 3 of the Protocol of Signature of Additional Protocol 2 to the said Convention of 17 October 1979\nArticle 1\nFor the purpose of this Regulation the States referred to in the first sentence of paragraph 3 of the Protocol of Signature of Additional Protocol 2 of 17 October 1979 to the Revised Convention for the navigation of the Rhine shall be accorded equal status with the Contracting States of the said Convention. The expression \u2018Contracting State\u2019 in this Regulation shall always include each of those States as are accorded equal status. Article 2\n1. The authorities of the Contracting State in which a vessel is registered in a public register shall alone be competent to issue and withdraw the document provided for in the third paragraph of Article 2 of the Revised Convention for the navigation of the Rhine, establishing that the vessel belongs to Rhine navigation. 2. In the absence of a public register or in the event of a vessel not being registered in a Contracting State, the authorities of the Contracting State in which the owner of the vessel or, in the case of joint ownership, the first joint owner to apply for the document referred to in the preceding paragraph to be issued, has his domicile, usual residence or registered office shall be competent to issue, cancel and withdraw the said document. 3. The \u2018document\u2019 may take the form either of a special document in accordance with the third paragraph of Article 2 of the Revised Convention for the navigation of the Rhine or of an entry on another document already issued for the vessel, to the effect that the vessel belongs to Rhine navigation. 4. Each Contracting State shall make known to the other Contracting States, through the Central Commission for the navigation of the Rhine, a list of its designated competent authorities. Article 3\n1. The document referred to in the first paragraph of Article 2 shall not be issued for a vessel unless the owner of that vessel:\n\n\n\n\n\n\n(a)\n\n\nas a natural person, is a national of one of the Contracting States and has his domicile or usual residence in a Contracting State; or\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nas a legal person governed by public law, is established under the laws of a Contracting State and has its registered office in that State; or\n\n\n\n\n\n\n\n\n\n\n(c)\n\n\nas a legal person or a company or firm governed by private law;\n\n\n\n\n\n\n(aa)\n\n\nis established in a Contracting State under its laws;\n\n\n\n\n\n\n\n\n\n\n(bb)\n\n\nhas its registered office, its principal place of business and the place from which the vessel is operated in that Contracting State, and\n\n\n\n\n\n\n\n\n\n\n(cc)\n\n\nis managed and directed by persons the majority of whom are nationals of Contracting States and who have their domicile or usual residence and, in the case of legal persons, their registered office, in one of those States. 2. However, no document shall be issued in respect of a vessel belonging to a legal person or a company or firm governed by private law either if it is so constituted that the persons holding directly or indirectly a majority share in the beneficial ownership of the undertaking or holding the majority of shares conferring voting rights or the majority of voting rights, are not nationals of Contracting States or do not have their domicile, registered office or usual residence in one of those States. 3. In the case of trusts or similar arrangements, the conditions laid down above must also be fulfilled in respect of the persons on whose behalf such transactions are performed. 4. A Contracting State may exceptionally, after consulting the Central Commission, grant exceptions to the majority required in paragraphs 1 (c) (cc) and 2 above on condition that the objective of Additional Protocol 2 to the Revised Convention for the navigation of the Rhine is not affected. The Central Commission may establish the general conditions under which these exceptions will be granted. Article 4\n1. In the case of a vessel under joint ownership, a joint owner or joint owners who hold a majority share in the joint ownership and who manage the joint ownership must fulfil the conditions set out in Article 3. 2. If there are legal persons or companies of firms governed by private law among the joint owners concerned, the persons who manage and direct those undertakings and the persons who hold directly or indirectly a share in their beneficial ownership must all be nationals of Contracting States and have their domicile, registered office or usual residence in one of those States. Article 5\n1. The operator of a vessel must also fulfil the same conditions as the owner in order to obtain the document referred to in the first paragraph of Article 2 for the vessel which he is operating. 2. The authorities of the Contracting State in which the operator has his domicile or usual residence, or in which the registered office of the undertaking is situated, shall be competent to issue and withdraw the relevant document. Article 6\n1. The owner, joint owner or operator of a vessel shall apply to the competent authority for the document referred to in the first paragraph of Article 2 to be issued and shall furnish all true and necessary information to that end. 2. The owner, joint owner or operator of the vessel, in so far as it relates to him, must inform the competent authority which issued the document, immediately and in writing, of any change in the circumstances on the basis of which the document was issued. 3. The competent authorities may at any time verify whether the conditions laid down in Articles 3, 4 and 5 are still fulfilled; if they are not, they shall withdraw the document. Article 7\n1. The document certifying that the vessel belongs to Rhine Navigation must identify the vessel, its owner and, where appropriate, the operator by stating inter alia:\n\n\n\n\n\n\n\u2014\n\n\nthe name, number, place of registration, type and category of the vessel,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nthe name, business name, domicile, usual residence or registered office of the owner and, where appropriate, of the operator. 2. The document must be kept on board the vessel and must be produced on demand to the inspecting authorities. Article 8\n1. The Contracting States shall adopt the provisions necessary to give effect to this Regulation, in particular as regards the procedure and the burden of proof. These provisions shall be notified to the other Contracting States through the Central Commission for the Navigation of the Rhine. 2. To ensure application of this Regulation, the competent authorities of the Contracting States shall cooperate within the framework of their national legislation and shall communicate the necessary information to one another, subject to commercial confidentiality. Article 9\n1. This Regulation shall enter into force on the day on which Additional Protocol 2 to the Revised Convention for the navigation of the Rhine, signed at Strasbourg on 17 October 1979, enters into force. 2. The provision contained in Article 7 (2) of this Regulation shall, however, apply only on the expiry of a transitional period of two years from the date of entry into force. 3. This Regulation may be amended or supplemented according to the same procedure by which it was enacted"}
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/de9b6051-7779-4881-be88-6ab76ea6bf07", "title": "Commission Regulation (EEC) No 2858/85 of 11 October 1985 on the sale of pigmeat held by the Belgian intervention agency pursuant to Regulations (EEC) No 772/85, (EEC) No 978/85 and (EEC) No 1477/85", "langIdentifier": "ENG", "mtypes": "html,pdfa1b,print", "workTypes": "http://publications.europa.eu/ontology/cdm#legislation_secondary,http://publications.europa.eu/ontology/cdm#regulation,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Commission", "date": "1985-10-11", "subjects": "Belgium,intervention stock,pigmeat", "workIds": "celex:31985R2858,oj:JOL_1985_274_R_0022_008", "eurovoc_concepts": ["Belgium", "intervention stock", "pigmeat"], "url": "http://publications.europa.eu/resource/cellar/de9b6051-7779-4881-be88-6ab76ea6bf07", "lang": "eng", "formats": ["html", "pdfa1b", "print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/70aba212-14e3-4546-a198-ec2bc9afc678", "title": "RESOLUTION ON JAMMING STATIONS IN EUROPE", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#act_preparatory,http://publications.europa.eu/ontology/cdm#resolution_other_ep,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,Political Affairs Committee", "date": "1985-10-11", "subjects": "Bulgaria,Czechoslovakia,Eastern Bloc countries,OSCE,Poland,USSR,broadcasting,freedom of expression,human rights,information", "workIds": "celex:51985IP0103(01)", "eurovoc_concepts": ["Bulgaria", "Czechoslovakia", "Eastern Bloc countries", "OSCE", "Poland", "USSR", "broadcasting", "freedom of expression", "human rights", "information"], "url": "http://publications.europa.eu/resource/cellar/70aba212-14e3-4546-a198-ec2bc9afc678", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/c0bc5fa6-af22-489c-b021-f1060443fefd", "title": "RESOLUTION EMBODYING THE OPINION OF THE EUROPEAN PARLIAMENT, IN ACCORDANCE WITH THE PROCEDURE WITHOUT REPORT, ON THE PROPOSAL FROM THE COMMISSION OF THE EUROPEAN COMMUNITIES TO THE COUNCIL (DOC. C 2-72/85 - COM(85) 193 FINAL) ON A DRAFT DECISION ON THE ASSOCIATION OF THE OVERSEAS COUNTRIES AND TERRITORIES WITH THE EUROPEAN ECONOMIC COMMUNITY", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#act_preparatory,http://publications.europa.eu/ontology/cdm#resolution_legislative_ep,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "Committee on Development,European Parliament", "date": "1985-10-11", "subjects": "development policy,economic relations,overseas countries and territories,third Lom\u00e9 Convention,trade relations", "workIds": "celex:51985AP0072(01)", "eurovoc_concepts": ["development policy", "economic relations", "overseas countries and territories", "third Lom\u00e9 Convention", "trade relations"], "url": "http://publications.europa.eu/resource/cellar/c0bc5fa6-af22-489c-b021-f1060443fefd", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/695dcd1d-34b6-480c-bac0-19de15b0972e", "title": "RESOLUTION ON MONETARY STABILITY", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#act_preparatory,http://publications.europa.eu/ontology/cdm#resolution_initiative_own_ep,http://publications.europa.eu/ontology/cdm#resolution_other_ep,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,Liberal and Democratic Group", "date": "1985-10-11", "subjects": "European Monetary System,United Kingdom,economic policy,euro,exchange control,monetary cooperation", "workIds": "celex:51985IP0981", "eurovoc_concepts": ["European Monetary System", "United Kingdom", "economic policy", "euro", "exchange control", "monetary cooperation"], "url": "http://publications.europa.eu/resource/cellar/695dcd1d-34b6-480c-bac0-19de15b0972e", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/959863a3-1bb7-48f0-a247-12689f5d79c4", "title": "Fourth Commission Directive 85/490/EEC of 11 October 1985 on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products", "langIdentifier": "ENG", "mtypes": "fmx4,html,pdfa1b,print,xhtml", "workTypes": "http://publications.europa.eu/ontology/cdm#directive,http://publications.europa.eu/ontology/cdm#legislation_secondary,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Commission", "date": "1985-10-11", "subjects": "analytical chemistry,approximation of laws,cosmetic product", "workIds": "celex:31985L0490,oj:JOL_1985_295_R_0030_018", "eurovoc_concepts": ["analytical chemistry", "approximation of laws", "cosmetic product"], "url": "http://publications.europa.eu/resource/cellar/959863a3-1bb7-48f0-a247-12689f5d79c4", "lang": "eng", "formats": ["fmx4", "html", "pdfa1b", "print", "xhtml"], "text": "L_1985295EN. 01003001. xml\n\n\n\n\n\n\n\n\n\n\n7. 11. 1985\u00a0\u00a0\u00a0\n\n\nEN\n\n\nOfficial Journal of the European Communities\n\n\nL 295/30\n\n\n\n\n\nFOURTH COMMISSION DIRECTIVE\nof 11 October 1985\non the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products\n(85/490/EEC)\nTHE COMMISSION OF THE EUROPEAN COMMUNITIES,\nHaving regard to the Treaty establishing the European Economic Community,\nHaving 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\u00a0(1), as last amended by Directive 85/391/EEC\u00a0(2), and in particular Article 8 (1) thereof,\nWhereas Directive 76/768/EEC provides for the official testing of cosmetic products with the aim of ensuring that the conditions laid down by Community provisions concerning the composition of cosmetic products are satisfied;\nWhereas all the necessary methods of analysis should be laid down as quickly as possible; whereas three steps towards the attainment of this objective having already been taken through the definition of certain methods in Commission Directive 80/1335/EEC\u00a0(3), 82/434/EEC\u00a0(4) and 83/514/EEC\u00a0(5), the fourth step is to consist in the definition of methods for the identification and determination of glycerol 1-(4-aminobenzoate), the determination of chlorobutanol, the identification and determination of quinine, the identification and determination of inorganic sulphites and hydrogen sulphites, the identification and determination of chlorates of the alkali metals and the identification and determination of sodium iodate;\nWhereas the measures provided for in this Directive are in accordance with the opinion of the Committee on the Adaptation of Directive 76/768/EEC to Technical Progress,\nHAS ADOPTED THIS DIRECTIVE:\nArticle 1\nMember States shall take all necessary steps to ensure that during official testing of cosmetic products:\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of glycerol l-(4-aminobenzoate),\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ndetermination of chlorobutanol,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of quinine,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of inorganic sulphites and hydrogen sulphites,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of chlorates of the alkali metals, and\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of sodium iodate are performed in accordance with the methods described in the Annex. Article 2\nMember States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive not later than 31 December 1986. They shall forthwith inform the Commission thereof. Article 3\nThis Directive is addressed to the Member States. Done at Brussels, 11 October 1985. For the Commission\n\nStanley CLINTON-DAVIS\n\nMember of the Commission\n\n\n\n\n\n(1)\u00a0\u00a0OJ No L 262, 27. 9. 1976, p. 169. (2)\u00a0\u00a0OJ No L 224, 22. 8. 1985, p. 40. (3)\u00a0\u00a0OJ No L 383, 31. 12. 1980, p. 27. (4)\u00a0\u00a0OJ No L 185, 30. 6. 1982, p. 1. (5)\u00a0\u00a0OJ No L 291, 24. 10. 1983, p. 9. ANNEX\n\nIDENTIFICATION AND DETERMINATION OF GLYCEROL l-(4-AMINOBENZOATE)\n\nA. IDENTIFICATION\n1. SCOPE AND FIELD OF APPLICATION\nThis method will detect alpha-monoglyceryl 4-aminobenzoate (glycerol 1-(4-aminobenzoate). It will also detect ethyl 4-aminobenzoate (benzocaine INN) which may be present as an impurity. 2. PRINCIPLE\nThis identification is done by thin layer chromatography on silica gel with a fluorescent indicator and detection of the free primary amine group by formation of a diazo dye on the plate. 3. REAGENTS\nAll reagents should be of analytical purity. 3. 1. Solvent mixture: cyclohexane/propan-2-ol/stabilized dichloromethane 48/64/9 (v/v/v). 3. 2. Development solvent: petroleum ether (40-60)/benzene/acetone/ammonium hydroxide solution (minimum 25 % NH3): 35/35/35/1 (v/v/v/v). 3. 3. Developing solution\n\n\n:\n\n\n\n\n\n\n\n\n(a)\n\n\nsodium nitrite: 1 g in 100 ml of 1 M hydrochloric acid (prepared immediately before use);\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\n2-naphthol: 0,2 g in 100 ml of 1 M potassium hydroxide. 3. 4. Standard solutions:\n\n\n\n\n\n\n\u00a0\n\n\nalpha-monoglyceryl 4-aminobenzoate: 0,05 g in 100 ml of mixed solvent 3. 1;\n\n\n\n\n\n\n\n\n\n\n\u00a0\n\n\nethyl 4-aminobenzoate: 0,05 g in 100 ml of mixed solvent 3. 1. 3. 5. Silica gel 60 F254 plates, 0,25 mm thick, 200 mm \u00d7 200 mm. 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Normal apparatus for thin layer chromatography. 4. 2. Ultrasonic vibrator. 4. 3. Millipore filter FH 0,5 \u03bcm or equivalent. 5. PROCEDURE\n5. 1. Sample preparation\n\nWeigh 1,5 g of the product to be analyzed in a 10 ml stoppered graduated flask. Make up to the mark with the solvent 3. 1. Stopper and leave for one hour at room temperature in an ultrasonic vibrator (4. 2). Filter through a Millipore filter (4. 3) and use the filtrate for chromatography. 5. 2. Thin layer chromatography\n\nDeposit 10 \u03bcl of sample solution (5. 1) and of each standard solution (3. 4) on the plate (3. 5). Develop the chromatogram to a height of 150 mm in a tank previously saturated with solvent 3. 2. Allow the plate to dry at ambient temperature. 5. 3. Development\n\n\n\n\n\n\n\n\n\n5. 3. 1. Observe the plate under 254 nm UV light. 5. 3. 2. Spray the completely dried plate with the solution 3. 3 (a). Allow to dry at room temperature for 1 minute and immediately spray with the solution 3. 3 (b). Dry the plate in an oven at 60 oC. The spots appear an orange colour. Alpha-monoglyceryl 4-aminobenzoate: RF 0,07; ethyl 4-aminobenzoate: RF 0,55. B. DETERMINATION\n1. SCOPE AND FIELD OF APPLICATION\nThis method determines alpha monoglyceryl 4-aminobenzoate. It will also determine ethyl 4-aminobenzoate. It cannot determine more than 5 % (m/m) of alpha monoglyceryl 4-aminobenzoate and 1 % (m/m) of ethyl 4-aminobenzoate. 2. DEFINITION\nThe alpha monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents measured by this method are expressed as percentage by mass (% m/m) of the product. 3. PRINCIPLE\nThe product to be analyzed is suspended in methanol and after appropriate treatment of the sample it is determined by high-performance liquid chromatography (HPLC). 4. REAGENTS\nAll reagents should be of analytical purity and should be suitable for HPLC where appropriate. 4. 1. Methanol. 4. 2. Potassium dihydrogenorthophosphate (KH2PO4). 4. 3. Zinc di(acetate) (Zn(CH3COO)2 \u0387 2H2O). 4. 4. Acetic acid. 4. 5. Tetrapotassium hexacyanoferrate, (K4(Fe(CN)6) \u0387 3H2O). 4. 6. Ethyl 4-hydroxybenzoate. 4. 7. Alpha monoglyceryl 4-aminobenzoate. 4. 8. Ethyl 4-aminobenzoate. 4. 9. Phosphate buffer solution (0,02 M): dissolve 2,72 g of potassium dihydrogenorthophosphate (4. 2) in one litre of water. 4. 10. Eluant: phosphate buffer solution (4. 9)/methanol (4. 1) 61/39(v/v)\nThe composition of the mobile phase may be changed in order to achieve a resolution factor R \u2265 1,5. where\n\n\n\n\n\n\n\nR1 and R2\n\n\n\n=\n\n\nretention times, in minutes, of the peaks,\n\n\n\n\nW1 and W2\n\n\n\n=\n\n\npeak widths at half height, in milimetres,\n\n\n\n\nd'\n\n\n=\n\n\nthe chart speed, in millimetres per minute. 4. 11. Stock solution of alpha-monoglyceryl 4-aminobenzoate: weigh accurately about 40 mg of alpha-monoglyceryl 4-aminobenzoate and introduce it into a 100 ml graduated flask. Dissolve in 40 ml of methanol (4. 1). Make up to the mark with buffer solution (4. 9) and mix. 4. 12. Stock solution of ethyl 4-aminobenzoate: weigh accurately about 40 mg of ethyl 4-aminobenzoate and introduce it into a 100 ml graduated flask. Dissolve in 40 ml of methanol (4. 1). Make up to the mark with the buffer solution (4. 9) and mix. 4. 13. Internal standard solution: weigh accurately about 50 mg of ethyl 4-hydroxybenzoate (4. 6), transfer to a 100 ml standard flask, dissolve in 40 ml of methanol (4. 1), make up to the mark with the buffer solution (4. 9) and mix. 4. 14. Standard solutions: prepare four standard solutions by dissolving in 100 ml eluant (4. 10) according to the following table:\n\n\n\n\n\n\n\n\n\n\n\nStandard Solution\n\n\nAlpha-monoglyceryl 4-aminobenzoate\n\n\nEthyl 4-aminobenzoate\n\n\nEthyl 4-hydroxybenzoate\n\n\n\n\n(\u03bcg/ml)\u00a0(1)\n\n\n\nml (4. 11)\u00a0(1)\n\n\n\n(\u03bcg/ml)\u00a0(1)\n\n\n\nml (4. 12)\n\n\n(\u03bcg/ml)\u00a0(1)\n\n\n\nml (4. 13)\n\n\n\n\nI\n\n\n8\n\n\n2\n\n\n8\n\n\n2\n\n\n50\n\n\n10\n\n\n\n\nII\n\n\n16\n\n\n4\n\n\n12\n\n\n3\n\n\n50\n\n\n10\n\n\n\n\nIII\n\n\n24\n\n\n6\n\n\n16\n\n\n4\n\n\n50\n\n\n10\n\n\n\n\nIV\n\n\n40\n\n\n10\n\n\n20\n\n\n5\n\n\n50\n\n\n10\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n4. 15\n\n\nCarrez I solution: dissolve 26,5 g of tetrapotassium hexacyanoferrate (4. 5) in water and make up to 250 ml. 4. 16. Carrez II solution: dissolve 54,9 g of zinc di(acetate) (4. 3) and 7,5 ml of acetic acid (4. 4) in water and make up to 250 ml. 4. 17. Merck Lichrosorb RP-18, or equivalent, with an average particle size of 5 \u03bcm. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. The usual laboratory equipment. 5. 2. High-performance chromatography equipment with a variable wavelength UV detector and thermostatted chamber set at 45 oC. 5. 3. Stainless-steel column: length: 250 mm; internal diameter: 4,6 mm; packing: Lichrosorb RP \u2014 18 (4. 17). 5. 4. Ultrasonic bath. 6. PROCEDURE\n6. 1. Sample preparation\n\n\n\n\n\n\n\n\n\n6. 1. 1. Weigh accurately about 1 g of sample into a 100 ml beaker and add 10 ml of methanol (4. 1). 6. 1. 2. Place the beaker in the ultrasonic bath (5. 4) for 20 minutes to produce a suspension. Transfer the suspension thus obtained quantitatively into a 100 ml standard flask with not more than 75 ml of eluant (4. 10). Add in succession 1 ml of Carrez I solution (4. 15) and 1 ml of Carrez II solution (4. 16) and mix after each addition. Make up to the mark with eluant (4. 10), re-mix and filter through a pleated filter paper. 6. 1. 3. With a pipette, transfer 3,0 ml of the filtrate obtained in 6. 1. 2 and 5,0 ml of the internal standard solution (4. 13) into a 50 ml standard flask. Make up to the mark with eluant (4. 10) and mix. Use the solution thus obtained for carrying out the chromatography analysis described in 6. 2. 6. 2. Chromatography\n\n\n\n\n\n\n\n\n\n6. 2. 1. Adjust the flow rate of the mobile phase (4. 10) to 1,2 ml/min and set the column temperature to 45 oC. 6. 2. 2. Set the detector (5. 2) to 274 nm. 6. 2. 3. With a microsyringe, inject at least two times 20 \u03bcl of solution (6. 1. 3) into the chromatograph and measure the areas of the peaks. 6. 3. Calibration curve\n\n\n\n\n\n\n\n\n\n6. 3. 1. Inject 20 \u03bcl of each of the standard solutions (4. 14) and measure the peak area. 6. 3. 2. For each concentration calculate the ratio between the peak areas of alpha-monoglyceryl 4-aminobenzoate and the peak areas of the internal standard. Plot this ratio on the abscissa and on the ordinate the ratio of the corresponding masses. 6. 3. 3. Proceed in the same manner for ethyl 4-hydroxybenzoate. 7. CALCULATION\n\n\n\n\n\n\n\n\n7. 1. From the calibration curve obtained in 6. 3 read off the mass ratios (RP1, RP2) corresponding to the ratios between the areas of the peaks calculated in 6. 2. 3 where\n\n\n\n\n\n\n\nRP1\n\n\n=\n\n\nmass of alpha-monoglyceryl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate,\n\n\n\n\nRP2\n\n\n=\n\n\nmass of ethyl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate. 7. 2. From the mass ratios obtained in this way calculate the alpha-monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents, as mass percentages (% m/m) with the formulae:\n\n\n\n\n\n\n\n\n\n\n\n\n\nq\n\n\n=\n\n\nquantity of ethyl 4-hydroxybenzoate (internal standard) weighed, in milligrams, in 4. 12,\n\n\n\n\np\n\n\n=\n\n\nquantity of sample, in grams, weighed in 6. 1. 1. 8. REPEATABILITY\u00a0(2)\n\n\n\n\n\n\n\n\n\n8. 1. For a 5 % (m/m) content of alpha-monoglyceryl 4-aminobenzoate, the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,25 %. 8. 2. For a 1 % (m/m) content of ethyl 4-aminobenzoate the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,10 %. 9. NOTES\n\n\n\n\n\n\n\n\n9. 1. Before carrying out an analysis, check whether the sample contains substances likely to overlap with the peak of the internal standard (ethyl 4-aminobenzoate) on the chromatogram. 9. 2. In order to check the absence of any interference, repeat the determination by changing the proportion of methanol in the mobile phase by 10 % relative. DETERMINATION OF CHLOROBUTANOL\n\n\u00a0\n1. SCOPE AND FIELD OF APPLICATION\nThis method is suitable for the determination of chlorobutanol (INN) up to a maximum concentration of 0,5 % (m/m) in any cosmetic product, except aerosols. 2. DEFINITION\nThe content of chlorobutanol measured by this method is expressed as percentage by mass (% m/m) of product. 3. PRINCIPLE\nAfter appropriate treatment of the product to be analyzed the determination is done by gas chromatography using 2,2,2-trichloroethanol as the internal standard. 4. REAGENTS\nAll the reagents should be of analytical purity. 4. 1. Chlorobutanol (1,1,1-trichloro-2-methylpropan-2-ol). 4. 2. 2,2,2-Trichloroethanol. 4. 3. Absolute ethanol. 4. 4. Standard solution of chlorobutanol: 0,025 g in 100 ml ethanol (4. 3) (m/v). 4. 5. Standard solution of 2,2,2-trichloroethanol: 4 mg in 100 ml ethanol (4. 3) (m/v). 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Normal laboratory equipment. 5. 2. Gas chromatograph with electron detector, Ni 63. 6. PROCEDURE\n6. 1. Preparation of sample\n\nWeigh accurately between 0,1 and 0,3 g (p g) of the sample. Place in 100 ml volumetric flask. Dissolve it in ethanol (4. 3), add 1 ml of the internal standard solution (4. 5) and make up to the mark with ethanol (4. 3). 6. 2. Gas chromatography conditions\n\n\n\n\n\n\n\n\n6. 2. 1. The operating conditions must yield a resolution factor R \u2265 1,5. Where\n\n\n\n\n\n\n\nR1 and R2\n\n\n\n=\n\n\nretention times, in minutes, of the peaks,\n\n\n\n\nW1 and W2\n\n\n\n=\n\n\npeak widths at half height, in millimetres,\n\n\n\n\nd'\n\n\n=\n\n\nthe chart speed, in millimetres per minute. 6. 2. 2. As examples, the following operating conditions provide the required resolution:\n\n\n\n\n\n\n\nColumn\n\n\nI\n\n\nII\n\n\n\n\nMaterial\n\n\nGlass\n\n\nStainless steel\n\n\n\n\nLength\n\n\n1,80 m\n\n\n3 m\n\n\n\n\nDiameter\n\n\n3 mm\n\n\n3 mm\n\n\n\n\nStationary phase\n\n\n10 % Carbowax 20 M TPA on Gaschrom Q 80-100 mesh\n\n\n5 % OV 17 on Chromosorb WAW DMCS 80-100 mesh\n\n\n\n\nConditioning\n\n\n2 to 3 days at 190 oC\n\n\n\u00a0\n\n\n\n\nTemperature:\n\n\n\u00a0\n\n\n\u00a0\n\n\n\n\n\u2014 injector\n\n\n200 oC\n\n\n150 oC\n\n\n\n\n\u2014 column\n\n\n150 oC\n\n\n100 oC\n\n\n\n\n\u2014 detector\n\n\n200 oC\n\n\n150 oC\n\n\n\n\nCarrier gas\n\n\nNitrogen\n\n\nArgon/methane (95/5 v/v)\n\n\n\n\nFlowrate\n\n\n35 ml/min\n\n\n35 ml/min\n\n\n\n\n\n\n\n\n6. 3. Standard curve\n\nUsing five 100 ml volumetric flasks, add 1 ml of the standard solution (4. 5) and 0,2, 0,3, 0,4, 0,5, and 0,6 ml of solution 4. 4 respectively, and make up to the mark with ethanol (4. 3) and mix. Inject 1 \u03bcl of each of these solutions into the chromatograph in accordance with the operating conditions described in 6. 2. 2 and construct a calibration curve by plotting as the abscissa the ratio of the mass of chlorobutanol to that of 2,2,2-trichloroethanol and as the ordinate the ratio of the corresponding peak areas. 6. 4. Inject 1 \u03bcl of solution obtained in 6. 1 and proceed according to the conditions described in 6. 2. 2\n\n\n\n\n7. CALCULATION\n\n\n\n\n\n\n\n\n7. 1. Calculate from the standard curve (6. 3) the quantity \u2018a\u2019 expressed as \u03bcg of chlorobutanol, in the solution 6. 1. 7. 2. The content of chlorobutanol in the sample is calculated according to the formula:\n\n\n\n\n\n\n\n8. REPEATABILITY\u00a0(3)\n\nFor a chlorobutanol content of 0,5 % (m/m) the difference between the results of two determinations in parallel carried out on the same sample should not exceed 0,01 %. Note\n\nIf the result is equal to or exceeds the maximum permitted concentration it is necessary to check the absence of interferences. IDENTIFICATION AND DETERMINATION OF QUININE\n\nA. IDENTIFICATION\n1. SCOPE AND FIELD OF APPLICATION\nThis method is intended to detect the presence of quinine in shampoo and hair lotions. 2. PRINCIPLE\nIdentification is done by thin layer chromatography on silica gel. Detection of quinine is by the blue fluorescence of quinine in acidic conditions at 360 nm. For further confirmation, the fluorescence can be eliminated by bromine vapours, and ammonia vapours will cause a yellowish fluorescence to appear. 3. REAGENTS\nAll reagents should be of analytical purity. 3. 1. Silica gel plates, without fluorescence indicators, 0,25 mm thick, 200 mm \u00d7 200 mm\n\n\n\n\n\n\n\n\n\n\n\n\n3. 2. Developing solvent: toluene /diethyl ether /dichloromethane /diethylamine /20/20/20/8 (v/v/v/v). 3. 3. Methanol. 3. 4. Sulphuric acid (96 %; \n\n). 3. 5. Diethyl ether. 3. 6. Developing agent: carefully add 5 ml of sulphuric acid (3. 4) to 95 ml of diethyl ether (3. 5) in a cooled container. 3. 7. Bromine. 3. 8. Ammonium hydroxide solution (28 %; \n\n). 3. 9. Quinine, anhydrous. 3. 10. Standard solution: weigh accurately about 100,0 mg of anhydrous quinine (3. 9) into a standard flask and dissolve in 100 ml of methanol (3. 3). 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Normal equipment for thin layer chromatography. 4. 2. Ultrasonic bath. 4. 3. Millipore filter, FH 0,5 \u0192m or equivalent with suitable filtration equipment. 5. PROCEDURE\n5. 1. Preparation of the sample\n\nWeigh accurately a quantity of the sample which may contain approximately 100 mg of quinine into a 100 ml standard flask, dissolve and make up to the mark with methanol (3. 3). Stopper the flask and leave for one hour at room temperature in an ultrasonic vibrator (4. 2). Filter (4. 3) and use the filtrate for the chromatography. 5. 2. Thin layer chromatography\n\nDeposit 1,0 \u03bcl of standard solution (3. 10) and 1,0 \u03bcl of sample solution (5. 1) on the silica gel plate (3. 1). Develop the chromatogram over a distance of 150 mm using solvent 3. 2. in a tank previously saturated with solvent (3. 2). 5. 3. Development\n\n\n\n\n\n\n\n\n\n5. 3. 1. Dry the plate at room temperature. 5. 3. 21. Spray with reagent 3. 6. 5. 3. 3. Leave the plate to dry for one hour at room temperature. 5. 3. 4. Observe under the light from a UV lamp adjusted to a wavelength of 360 nm. Quinine appears as a fluorescent intense blue spot. By way of example the table below gives the values of the RF of the main alkaloids related to quinine when developed with solvent 3. 2. Alkaloid\n\n\nRF\n\n\n\n\n\nQuinine\n\n\n0,20\n\n\n\n\nQuinidine\n\n\n0,29\n\n\n\n\nCinchonine\n\n\n0,33\n\n\n\n\nCinchonidine\n\n\n0,27\n\n\n\n\nHydroquinidine\n\n\n0,17\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n5. 3. 5. For further confirmation that quinine is present, the plate is exposed for approximately one hour to bromine vapour (3. 7). The fluorescence disappears. When the same plate is exposed to ammonia vapour (3. 8), the spots reappear with a brown colour, and when the plate is again examined under UV light at 360 nm a yellowish fluorescence can be observed. Detection limit: 0,1 \u03bcg of quinine. B. DETERMINATION\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes the determination of quinine. It may be used to determine the maximum permitted concentration of 0,5 % (m/m) in shampoos and 0,2 % in hair lotions. 2. DEFINITION\nThe quinine content determined by this method is expressed as a percentage by mass (% m/m) of the product. 3. PRINCIPLE\nAfter appropriate treatment of the product to be analyzed the determination is done by high-performance liquid chromatography (HPLC). 4. REAGENTS\nAll reagents should be of analytical purity and suitable for HPLC. 4. 1. Acetonitrile. 4. 2. Potassium dihydrogenorthophosphate (KH2PO4). 4. 3. Orthophosphoric acid (85 %; \n\n). 4. 4. Tetramethylaminium bromide. 4. 5. Quinine, anhydrous. 4. 6. Methanol. 4. 7. Orthophosphoric acid solution (0,1 M): weigh 11,53 g of orthophosphoric acid (4. 3) and dissolve in 1\u00a0000 nl of water in a graduated flask. 4. 8. Potassium dihyrogenorthophosphate solution (0,1 M): weigh 13,6 g of potassium dihydrogenorthophosphate (4. 2) and dissolve in 1\u00a0000 ml of water in a graduated flask. 4. 9. Tetramethylammonium bromide solution: dissolve 15,40 g of tetramethylammonium bromide (4. 4) in 1\u00a0000 ml of water in a graduated flask. 4. 10\n\n\nEluant: orthophosphoric acid (4. 7) /potassium dihydrogenorthophosphate (4. 8) /tetramethylammonium bromide (4. 9)/water/acetonitrile (4. 1) 10/50/100/340/90 (v/v/v/v/v). The composition of this mobile phase may be changed in order to achieve a resolution factor R \u2265 1,5. where\n\n\n\n\n\n\n\nR1 and R2\n\n\n\n=\n\n\nretention times, in minutes, of the peaks,\n\n\n\n\nW1 and W2\n\n\n\n=\n\n\npeak widths at half height, in millimetres,\n\n\n\n\nd'\n\n\n=\n\n\nthe chart speed, in millimetres per minute. 4. 11. Silica treated with octadecylsilane, 10 \u03bcm. 4. 12. Standard solutions: weigh accurately approximately 5,0, 10,0, 15,0 and 20,0 mg respectively of quinine anhydrous (4. 5) into a set of 100 ml standard flasks. Make up to the mark with methanol (4. 6) and shake the contents of the flasks until the quinine dissolves. Filter each sample through a 0,5 \u03bcm filter. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Usual laboratory equipment. 5. 2. Ultrasonic bath. 5. 3. High-performance liquid chromatography equipment with a variable wavelength detector. 5. 4. Column: length: 250 mm; internal diameter: 4,6 mm; filling: silica (4. 11). 5. 5. Millipore filter FH 0,5 \u03bcm, or equivalent, with suitable filtration apparatus. 6. PROCEDURE\n6. 1. Sample preparation\n\nWeigh accurately into a 100 ml standard flask a quantity of the product sufficient to contain 10,0 mg of anhydrous quinine, add 20 ml of methanol (4. 6) and place the flask in an ultrasonic bath (5. 2) for 20 minutes. Make up to the mark with methanol (4. 6). Mix the solution and then filter an aliquot (5. 5). 6. 2. Chromatography\n\n\n\n\n\n\n\n\u00a0\n\n\nFlowrate: 1,0 ml/min. Detector wavelength (5. 3): 332 nm. Injection volume: 10 \u03bcl of filtered solution (6. 1). Measurement: peak area. 6. 3. Calibration curve\n\nInject at least three times 10,0 \u03bcl of each reference solution (4. 12), measure the area of the peaks, and calculate the average area at each concentration. Produce the calibration curve and verify that it is rectilinear. 7. CALCULATION\n\n\n\n\n\n\n\n\n7. 1. From the calibration curve (6. 3) determine the quantity in \u03bcg of anhydrous quinine present in the volume injected (6. 2). 7. 2. The concentration of anhydrous quinine in the sample, as a percentage by mass (% m/m), is obtained by the following formula:\n\n\n\nwhere\n\n\n\n\n\n\nB\n\n\nis the quantity, in micrograms, of anhydrous quinine determined in the 10 microlitres of the filtered solution (6. 1). A\n\n\nis the mass of the sample in grams (6. 1). 8. REPEATABILITY\u00a0(4)\n\nFor an anhydrous quinine content of 0,5 % (m/m), the difference between the results of two determinations performed in parallel on the same sample must not exceed 0,02 %. For an anhydrous quinine content of 0,2 % (m/m), the difference between the results of two determinations performed in parallel on the same sample must not exceed 0,01 %. IDENTIFICATION AND DETERMINATION OF INORGANIC SULPHITES AND HYDROGEN SULPHITES\n\nSCOPE AND FIELD OF APPLICATION\nThe method describes the identification and determination of inorganic sulphites and hydrogen sulphites in cosmetic products. It is only applicable to products that have an aqueous or alcoholic phase and for concentrations up to 0,2 % sulphur dioxide. A. IDENTIFICATION\n1. PRINCIPLE\nThe sample is heated in hydrochloric acid, and sulphur dioxide liberated is identified either by its odour or its effect on an indicator paper. 2. REAGENTS\nAll reagents should be of analytical purity. 2. 1. Hydrochloric acid (4 M). 2. 2. Potassium iodate starch paper or other suitable alternative. 3. APPARATUS\n\n\n\n\n\n\n\n\n3. 1. Normal laboratory equipment. 3. 2. Flask (25 ml) fitted with a short reflux condenser. 4. PROCEDURE\n\n\n\n\n\n\n\n\n4. 1. Place about 2,5 g of sample in the flask (3. 2) with 10 ml of hydrochloric acid (2. 1). 4. 2. Mix and heat to boiling. 4. 3. Test for the emission of sulphur dioxide either by smell or indicator paper (2. 2). B. DETERMINATION\n1. DEFINITION\nThe sulphite or hydrogen sulphite content of the sample as determined by the method is expressed as percentage by mass of sulphur dioxide. 2. PRINCIPLE\nAfter acidification of the sample, sulphur dioxide liberated is distilled into a solution of hydrogen peroxide. Sulphuric acid formed is titrated against a standardized sodium hydroxide solution. 3. REAGENTS\nAll reagants should be of analytical purity. 3. 1. Hydrogen peroxide 0,2 % (m/v). Prepare daily. 3. 2. Orthophosphoric acid (\n\n ). 3. 3. Methanol. 3. 4. Sodium hydroxide (0,01 M) standardized solution. 3. 5. Nitrogen. 3. 6. Indicator: mixture 1: 1 (v/v) of methyl red (0,03 % m/v in ethanol) and methylene blue (0,05 % m/v in ethanol). Filter the solution. 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Normal laboratory equipment. 4. 2. Distillation apparatus (see figure). 5. PROCEDURE\n\n\n\n\n\n\n\n\n5. 1. Weigh accurately about 2,5 g of sample into the distillation flask A (see figure). 5. 2. Add 60 ml of water and 50 ml of methanol (3. 3) and mix. 5. 3. Place 10 ml of hydrogen peroxide (3. 1), 60 ml of water and a few drops of indicator (3. 6) in the distillation receiver D (see figure). Add a few drops of sodium hydroxide (3. 4) until the indicator turns green. 5. 4. Repeat 5. 3 for the wash bottle E (see figure). 5. 5. Assemble the apparatus and adjust the nitrogen (3. 5) flow to about 60 bubbles per minute. 5. 6. Run 15 ml of orthophosphoric acid (3. 2) from the funnel into the distillation flask A. 5. 7. Heat rapidly to boiling and then simmer gently for a total time of 30 minutes. 5. 8. Detach the distillation receiver D. Rinse the tube and then titrate with sodium hydroxide solution (3. 4) until the indicator turns green (3. 6). 6. CALCULATION\nCalculate the content of sulphite or hydrogen sulphite by mass in the sample by the expresssion:\n\n\n\nwhere\n\n\n\n\n\n\n\nM\n\n\n=\n\n\nmolar concentration of sodium hydroxide solution (3. 4),\n\n\n\n\nV\n\n\n=\n\n\nvolume of sodium hydroxide (3. 4) required for titration (5. 8), in millilitres,\n\n\n\n\nm\n\n\n=\n\n\nmass of sample (5. 1) in grams. 7. REPEATABILITY\u00a0(5)\n\nFor a content of 0,2 % m/m of sulphur dioxide the difference between two parallel determinations done on the same sample should not be greater than 0,006 %. Sulphurdioxide distillation apparatus according to Tanner\n\nAll dimensions in mm\n\n\n\n\nIDENTIFICATION AND DETERMINATION OF CHLORATES OF THE ALKALI METALS\n\nSCOPE AND FIELD OF APPLICATION\nThe method describes the identification and determination of chlorates in toothpastes and other cosmetic products. A. IDENTIFICATION\n1. PRINCIPLE\nChlorates are separated from other halates by thin layer chromatography and identified by the oxidation of iodide to form iodine. 2. REAGENTS\nAll reagents should be of analytical purity. 2. 1. Reference solutions: aqueous solutions of potassium chlorate, bromate and iodate (0,2 % m/v) prepared freshly. 2. 2. Development solvent: ammonia solution (28% m/v) acetone/butanol (60/130/30 v/v/v). 2. 3. Potassium iodide, aqueous solution (5 % m/v). 2. 4. Starch solution (1 to 5 % m/v). 2. 5. Hydrochloric acid (1 M). 2. 6. Ready-for-use cellulose thin-layer plates (0,25 mm). 3. APPARATUS\nNormal equipment for thin layer chromatography. 4. PROCEDURE\n\n\n\n\n\n\n\n\n4. 1. Extract about 1 g of the sample with water, filter, and dilute to about 25 ml. 4. 2. Deposit 2 (\u03bcl on the plate (2. 6) of the solution (4. 1) together with 2 \u03bcl aliquots of each of the three reference solutions (2. 1). 4. 3. Place the plate in a tank and develop by ascending chromatography about three-quarters of the length of the plate (2. 6) with solvent 2. 2. 4. 4. Remove from the tank and allow the solvent to evaporate. (NB: This may take up to two hours. )\n\n\n\n\n\n\n\n\n\n\n\n\n4. 5. Spray the plate with potassium iodide (2. 3) and allow to dry for about five minutes. 4. 6. Spray the plate with starch solution (2. 4) and allow to dry for about five minutes. 4. 7. Spray the plate with hydrochloric acid (2. 5). 5. EVALUATION\nIf the chlorate is present a blue spot (possibly a brown spot) will appear after half an hour with RF value approximately 0,7 to 0,8. Halates\n\n\nRF\n\n\n\n\n\nIodate\n\n\n0 to 0,2\n\n\n\n\nBromate\n\n\n0,5 to 0,6\n\n\n\n\nChlorate\n\n\n0,7 to 0,8\n\n\n\n\nIt should be noted that bromates and iodates give immediate reaction. Care should be taken not to confuse spots from bromates and chlorates. B. DETERMINATION\n1. DEFINITION\nThe chlorate content of the sample determined by this method is expressed as percentage by mass of chlorate. 2. PRINCIPLE\nChlorate is reduced by zinc powder under acid conditions. The formed chloride is measured by potentiometric titration using a silver nitrate solution. A similar determination before reduction permits the possible presence of halides. 3. REAGENTS\nAll reagents should be of analytical purity. 3. 1. Acetic acid, 80 % (m/m). 3. 2. Zinc powder. 3. 3. Silver nitrate standard solution (0,1 M). 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Normal laboratory equipment. 4. 2. Potentiometer equipped with a silver indicator electrode. 5. PROCEDURE\n5. 1. Sample preparation\n\nWeigh accurately a quantity \u2018m\u2019 of approximately 2 g in centrifuge tube. Add about 15 ml acetic acid (3. 1) and mix carefully. Wait 30 minutes and centrifuge for 15 minutes at 2\u00a0000 rev/min. Transfer the supernatant solution to a 50 ml volumetric flask. Repeat centrifuging twice by adding 15 ml acetic acid (3. 1) to the residue. Collect the solution containing chlorate in the same volumetric flask. Fill to the mark with acetic acid (3. 1). 5. 2. Reduction of chlorate\n\nTake 20 ml of solution 5. 1 and add 0,6 g of zinc powder (3. 2). Bring to the boil in a flask fitted with a condenser tube. After 30 minutes boiling, cool and filter. Rinse the flask with water. Filter and combine the filtrate with the rise's. 5. 3. Determination of chloride\n\nTitrate 20 ml solution 5. 2 with silver nitrate (3. 3) by using the potentiometer (4. 2). Titrate in the same way 20 ml of solution 5. 1 with silver nitrate (3. 3). NB: If the product contains bromine or iodine derivatives which can release bromides or iodides after reduction, the titration curve will have several inflexion points. In this case the volume of the titrated solution (3. 3) corresponding to chloride is the difference between the last and the penultimate inflexion points. 6. CALCULATION\nThe content of chlorate of the sample (% m/m) is calculated by the formula:\n\n\n\nwhere\n\n\n\n\n\n\n\nV\n\n\n=\n\n\nvolume in millilitres, of silver nitrate solution (3. 3) used to titrate solution 5. 2,\n\n\n\n\nV'\n\n\n=\n\n\nvolume, in millilitres, of silver nitrate solution (3. 3) used to titrate 20 millilitres of solution 5. 1,\n\n\n\n\nM\n\n\n=\n\n\nmolality of silver nitrate standard solution (3. 3),\n\n\n\n\nm\n\n\n=\n\n\nmass of sample, in grams. 7. REPEATABILITY\u00a0(6)\n\nFor a chlorate content of 3 to 5 % m/m the difference between the results of two determinations carried out in parallel on the same sample should not exceed 0,07 % m/m. IDENTIFICATION AND DETERMINATION OF SODIUM IODATE\n\nSCOPE AND FIELD OF APPLICATION\nThe method describes the procedure for identifying and determining rinse of cosmetic products containing sodium iodate. A. IDENTIFICATION\n1. PRINCIPLE\nSodium iodate is separated from other halates by thin layer chromatography and identified by the oxidation of iodide to form iodine. 2. REAGENTS\nAll reagents should be of analytical purity. 2. 1. Reference solutions. Aqueous solutions of potassium chlorate, bromate and iodate (0,01 % m/v) prepared freshly. 2. 2. Development solvent. Ammonia solution (28 % m/v) /acetone /butanol (60/130/30 v/v/v). 2. 3. Potassium iodide aqueous solution (5 % m/v). 2. 4. Starch solution (1 to 5 % m/v). 2. 5. Hydrochloric acid (1 M). 3. APPARATUS\n\n\n\n\n\n\n\n\n3. 1. Ready-for-use cellulose thin-layer chromatography (0,25 mm) plates. 3. 2. Normal equipment for thin layer chromatography. 4. PROCEDURE\n\n\n\n\n\n\n\n\n4. 1. Extract about 1 g of the sample with water, filter, and dilute to about 10 ml. 4. 2. Deposit 2 \u00b5l of this solution onto the base line of the plate (3. 1) together with 2 \u00b5l aliquots of each of the three reference solutions (2. 1). 4. 3. Place the plate in a tank and develop by ascending chromatography about three-quarters of the length of the plate with solvent (2. 2). 4. 4. Remove the plate from the tank and allow the solvent to evaporate at ambient temparature (NB: this may take up to two hours). 4. 5. Spray the plate with potassium iodide (2. 3) and allow to dry for about five minutes. 4. 6. Spray with starch (2. 4) and allow to dry for about five minutes. 4. 7. Finally spray with hydrochloric (2. 5). 5. EVALUATION\nIf iodate is present a blue spot (the colour may be brown or become brown on standing) will appear immediately with an RF value approximately 0 to 0,2. It should be noted that bromates give immediate reactions at RF values approximately at 0,5 to 0,6 and chlorates, after about 30 minutes, at RF values of 0,7 to 0,8 respectively. B. DETERMINATION\n1. DEFINITION\nThe sodium iodate content as determined by this method is expressed as a percentage by mass of sodium iodate. 2. PRINCIPLE\nSodium iodate is dissolved in water and determined by means of high-performance liquid chromatography, using in series, a reverse-phase C18 column and an anion-exchange column. 3. REAGENTS\nAll reagents should be of analytical purity and especially suitable for high-performance liquid chromatography (HPLC). 3. 1. Hydrochloric acid (4 M). 3. 2. Sodium sulphite aq, 5 % m/v. 3. 3. Sodium iodate stock solution. Prepare a stock solution containing 50 mg sodium iodate per 100 ml water. 3. 4. Potassium dihydrogenorthophosphate. 3. 5. Disodium hydrogenorthophosphate \u0387 2H2O. 3. 6. HPLC mobile phase: dissolve 3,88 g potassium dihydrogenorthophosphate (3. 4) and 1,19 g disodium hydrogenorthophosphate \u0387 2H2O (3. 5) in 1 litre water. The pH of the resulting solution is 6. 2. 3. 7. Universal indicator paper, pH 1-11. 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Ordinary laboratory apparatus. 4. 2. Circular filter paper, diameter 110 mm, Schleicher and Sch\u00fcll No 575, or equivalent. 4. 3. High-performance liquid chromatograph with a variable wavelength detector. 4. 4. Columns: length: 120 mm; internal diameter: 4,6 mm; number: two connected in series; first column \u2014 Necleosil R 5 C18 or equivalent; second column \u2014 Vydac (tm)-301-SB or equivalent. 5. PROCEDURE\n5. 1. Sample preparation\n\n5. 1. 1. Fluid samples (shampoos)\n\nWeigh accurately a test portion of approximately 1,0 g sample in a 10 ml glass stoppered calibrated tube or measuring flask. Fill up to the mark with water and mix. If necessary, filter the solution. Determine the iodate in the solution by means of HPLC as described in section 5. 2. 5. 1. 2. Solid samples (soap)\n\nFinely divide part of the sample and weigh accurately a test portion of approximately 1,0 g into a 100 ml glass stoppered measuring cylinder. Fill up to 50 ml with water and shake vigorously for one minute. Centrifuge and filter through a filter paper (4. 1) or allow the mixture to stand for at least one night. Shake the jellylike solution vigorously and filter it through a filter paper (4. 1). Determine the iodate in the filtrate by means of HPLC as described in section 5. 2. 5. 2. Chromatography\n\nFlowrate: 1 ml/min. Detector wavelength (4. 2): 210 nm. Injection volume: 10 \u00b5l. Measurement: peak area. 5. 3. Calibration\n\nPipette respectively 1,0, 2,0, 5,0, 10,0 and 20,0 ml of the sodium iodate stock solution (3. 3) into 50 ml volumetric flasks. Fill to the mark and mix. The solutions thus obtained, contain 0,01, 0,02, 0,05, 0,10 and 0,20 mg sodium iodate per ml respectively. Inject a 10 \u00b5l portion of each standard iodate solution into the liquid chromatograph (4. 2) and obtain a chromatogram. Determine the peak area for iodate and plot a curve relating the peak area to the sodium iodate concentration. 6. CALCULATION\nCalculate the sodium iodate content, in percentage by mass (% m/m), using the formula:\n\n\n\nwhere\n\n\n\n\n\n\nm\n\n\nis the mass, in grams, of the test portion (5. 1),\n\n\n\n\nV\n\n\nis the total volume of the sample solution, in millilitres, obtained as described in 5. 1,\n\n\n\n\nc\n\n\nis the concentration, in milligrams per millilitre of sodium iodate, obtained from the calibration curve (5. 3). 7. REPEATABILITY\u00a0(7)\n\nFor a sodium iodate content of 0,1 % (m/m) the difference between the results of two parallel determinations carried out on the same sample must not exceed 0,002 %. 8. CONFIRMATION\n8. 1. Principle\n\nIn an acidified solution of a cosmetic product, iodate (IO3-) is reduced to iodide (I\u2014) by sulphite and the resulting solution is investigated by means of HPLC. If a peak having a retention time corresponding to the retention time of iodate disappears after treatment with sulphite, the original peak can most probably be attributed to iodate. 8. 2. Procedure\n\nPipette a 5 ml portion of the sample solution obtained as described in section 5. 1 into a conical flask. Adjust the pH of the solution to a value of 3 or lower with hydrochloric acid (3. 1); universal indicator paper (3. 7). Add three drops of sodium sulphite solution (3. 2) and mix. Inject a 10 \u00b5l portion of the solution into the liquid chromatograph (4. 2). Compare this chromatogram with the chromatogram obtained as described in paragraph 5 for the same sample. (1)\u00a0\u00a0These values are given as an indication and correspond to the exact masses of 4. 11, 4. 12 and 4. 13. NB: These solutions may be prepared in a different way. (2)\u00a0\u00a0ISO 5725. (3)\u00a0\u00a0ISO 5725. (4)\u00a0\u00a0ISO 5725. (5)\u00a0\u00a0ISO 5725. (6)\u00a0\u00a0ISO 5725. (7)\u00a0\u00a0ISO 5725"}
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