diff --git "a/36_years1983-09.jsonl" "b/36_years1983-09.jsonl"
new file mode 100644--- /dev/null
+++ "b/36_years1983-09.jsonl"
@@ -0,0 +1,183 @@
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/60b5eb79-a38c-4887-85d6-b20cdae82131", "title": "WRITTEN QUESTION NO 1070/83 BY MR JAMES PROVAN TO THE COMMISSION: SUBJECT OF TOURING COACHES IN THE MEMBER STATES", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_written,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,PROVAN", "date": "1983-09-29", "subjects": "EU Member State,EU law,carriage of passengers,motor vehicle,national law,pipeline transport,public administration,road safety,road transport,supervisory power,tourism,transport policy,transport safety", "workIds": "celex:91983E001070", "eurovoc_concepts": ["EU Member State", "EU law", "carriage of passengers", "motor vehicle", "national law", "pipeline transport", "public administration", "road safety", "road transport", "supervisory power", "tourism", "transport policy", "transport safety"], "url": "http://publications.europa.eu/resource/cellar/60b5eb79-a38c-4887-85d6-b20cdae82131", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/a7d77bc8-7408-40c7-8451-13bfe69ebe8e", "title": "WRITTEN QUESTION NO 1091/83 BY MR ROBERT MORELAND TO THE COMMISSION: DUTY-FREE ENTITLEMENT", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_written,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,MORELAND", "date": "1983-09-29", "subjects": "EU Member State,airport,alcoholic beverage,approximation of laws,carriage of goods,customs,customs duties,duty-free sale,exemption from customs duties,fiscal policy,harbour installation,international transport,tax system,tax-free allowance,tobacco industry,wine", "workIds": "celex:91983E001091", "eurovoc_concepts": ["EU Member State", "airport", "alcoholic beverage", "approximation of laws", "carriage of goods", "customs", "customs duties", "duty-free sale", "exemption from customs duties", "fiscal policy", "harbour installation", "international transport", "tax system", "tax-free allowance", "tobacco industry", "wine"], "url": "http://publications.europa.eu/resource/cellar/a7d77bc8-7408-40c7-8451-13bfe69ebe8e", "lang": "eng", "formats": ["print"]}
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/96aa791b-ff43-4473-97b5-cc4322c42b7d", "title": "WRITTEN QUESTION NO 1106/83 BY MR DIETER ROGALLA TO THE COMMISSION: CUSTOMS CLEARANCE OF NORMAL CORRESPONDENCE", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_written,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,ROGALLA", "date": "1983-09-29", "subjects": "EU Member State,Germany,customs,customs formalities,customs union,frontier,intra-EU transport,postal and telecommunications services,postal service,supervisory power,tax evasion", "workIds": "celex:91983E001106", "eurovoc_concepts": ["EU Member State", "Germany", "customs", "customs formalities", "customs union", "frontier", "intra-EU transport", "postal and telecommunications services", "postal service", "supervisory power", "tax evasion"], "url": "http://publications.europa.eu/resource/cellar/96aa791b-ff43-4473-97b5-cc4322c42b7d", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/41e332f3-8c1a-4a0f-ac74-5586c4a09018", "title": "83/494/EEC: Commission Decision of 27 September 1983 concerning animal health conditions and veterinary certification for the importation of domestic animals of the bovine and porcine species from Canada", "langIdentifier": "ENG", "mtypes": "html,pdfa1b,print", "workTypes": "http://publications.europa.eu/ontology/cdm#decision,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": "1983-09-27", "subjects": "Canada,cattle,health certificate,import (EU),swine,veterinary inspection", "workIds": "celex:31983D0494,oj:JOL_1983_273_R_0037_017", "eurovoc_concepts": ["Canada", "cattle", "health certificate", "import (EU)", "swine", "veterinary inspection"], "url": "http://publications.europa.eu/resource/cellar/41e332f3-8c1a-4a0f-ac74-5586c4a09018", "lang": "eng", "formats": ["html", "pdfa1b", "print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/27501948-3eb5-4fd5-a0ec-bb4dd2036d6f", "title": "Third Commission Directive 83/514/EEC of 27 September 1983 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": "1983-09-27", "subjects": "analytical chemistry,approximation of laws,cosmetic product,product quality", "workIds": "celex:31983L0514,oj:JOL_1983_291_R_0009_005", "eurovoc_concepts": ["analytical chemistry", "approximation of laws", "cosmetic product", "product quality"], "url": "http://publications.europa.eu/resource/cellar/27501948-3eb5-4fd5-a0ec-bb4dd2036d6f", "lang": "eng", "formats": ["fmx4", "html", "pdfa1b", "print", "xhtml"], "text": "L_1983291EN. 01000901. xml\n\n\n\n\n\n\n\n\n\n\n24. 10. 1983\u00a0\u00a0\u00a0\n\n\nEN\n\n\nOfficial Journal of the European Communities\n\n\nL 291/9\n\n\n\n\n\nTHIRD COMMISSION DIRECTIVE\nof 27 September 1983\non the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products\n(83/514/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 83/341/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 two steps towards the attainment of this objective having already been taken through the definition of certain methods in Commission Directives 80/1335/EEC\u00a0(3) and 82/434/EEC\u00a0(4), the third step is to consist in the definition of methods for the determination of dichloromethane and 1,1,1-trichloroethane, the identification and determination of quinolin-8-ol and bis(8-hydroxyquino-linium) sulphate, the determination of ammonia, the identification and determination of nitromethane, the identification and determination of mercaptoacetic acid in hair-waving, hair-straightening and depilatory products, the identification and determination of hexachlorophene (INN), the tion of tosylchloramide sodium (INN), the determination of total fluorine in dental creams, the identification and determination of organomercury compounds, the determination of alkali and alkaline earth sulphides;\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\ndetermination of dichloromethane and 1,1,1-trichloroethane,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of quinolin-8-ol and bis(8-hydroxyquinolinium) sulphate,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ndetermination of ammonia,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of nitro-methane,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of mercapto-acetic acid in hair-waving, hair-straightening and depilatory products,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of hexachlorophene (INN),\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ndetermination of tosylchloramide sodium (INN),\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ndetermination of total fluorine in dental creams,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nidentification and determination of organo-mercury compounds,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\ndetermination of alkali and alkaline earth sulphides,\n\n\n\n\nare performed in accordance with the methods described in the Annex hereto. 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 1984. They shall forthwith inform the Commission thereof. Article 3\nThis Directive is addressed to the Member States. Done at Brussels, 27 September 1983. For the Commission\n\nFrans ANDRIESSEN\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 188, 13. 7. 1983, p. 15. (3)\u00a0\u00a0OJ No L 383, 31. 12. 1980, p. 27. (4)\u00a0\u00a0OJ No L 185, 30. 6. 1982, p. 1. ANNEX\nDETERMINATION OF DICHLOROMETHANE AND 1,1,1-TRICHLOROETHANE\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes the determination of dichloromethane (methylene chloride) and 1,1,1-trichloroethane (methyl chloroform) in all cosmetic products likely to contain these solvents. 2. DEFINITION\nThe dichloromethane and 1,1,1-trichloroethane content of the sample determined according to this method are expressed in percentage by mass. 3. PRINCIPLE\nThe method uses gas chromatography with chloroform as internal standard. 4. REAGENTS\nAll reagents must be of analytical quality. 4. 1. Chloroform (CHCl3). 4. 2. Carbon tetrachloride (CCl4). 4. 3. Dichloromethane (CH2Cl2). 4. 4. 1,1,1-trichloroethane (CH3CCl3). 4. 5. Acetone. 4. 6. Nitrogen. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Usual laboratory apparatus. 5. 2. Gas chromatograph fitted with a thermal conductivity detector. 5. 3. Transfer bottle, 50 to 100 ml (see sampling method 5. 3)\u00a0(1). 5. 4. Pressure gas-syringe, 25 or 50 \u03bcl (see sampling method 5. 4. 2. 2)\u00a0(1). 6. PROCEDURE\n\n\n\n\n\n\n\n\n6. 1. Non-pressurized sample: weigh the sample accurately in a stoppered conical flask. Introduce an accurately weighed quantity of chloroform (4. 1) as internal standard equivalent to the presumed quantity of dichloromethane and 1,1,1-trichloroethane contained in the sample. Mix throroughly. 6. 2. Pressurized sample: use the sampling method described in the sampling chapter, but with the following refinements:\n\n\n\n\n\n\n6. 2. 1. After transferring a sample into a transfer bottle (5. 3), further introduce into the transfer bottle a volume of chloroform (4. 1) as internal standard equivalent to the presumed quantity of dichloromethane and/or 1,1,1-trichloroethane contained in the sample. Mix thoroughly. Rinse the dead volume of the valve with 0,5 ml of carbon tetrachloride (4. 2). After drying, determine accurately the added mass of the internal standard by difference. 6. 2. 2. After filling the syringe with the sample, the nozzle of the syringe should be purged with nitrogen (4. 6) so that no residue remains before injection into the chromatograph. 6. 2. 3. After each sample is taken, the surface of the valve and of the transfer piece should be rinsed several times with acetone (4. 5) (using as required a hypodermic syringe) and then dried thoroughly with nitrogen (4. 6). 6. 2. 4. For each analysis, take measurements using two different transfer bottles and five measurements per bottle. 7. CHROMATOGRAPHIC CONDITIONS\n\n\n\n\n\n\n\n\n7. 1. Precolumn\n\nTubing: stainless steel. Length: 300 mm\nDiameter: 3 or 6 mm. Packing: same material as used for the analytical column packing. 7. 2. Column\n\nThe stationary phase is made of Hallcomid M 18 on chromosorb. The column must yield a resolution \u2018R\u2019 equal to, or better than, 1,5, where:\n\n\n\nlet:\n\n\n\n\n\n\n\nr1 and r2\n\n\n\n=\n\n\nretention times (in minutes),\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). 7. 3. As examples the following columns yield the results sought:\n\n\n\n\n\n\n\n\nColumn\n\n\n\n\nI\n\n\n\n\nII\n\n\n\n\n\nMaterial:\n\n\nStainless steel tubing\n\n\nStainless steel tubing\n\n\n\n\nLength:\n\n\n350 cm\n\n\n400 cm\n\n\n\n\nDiameter:\n\n\n3 mm\n\n\n6 mm\n\n\n\n\nSupport:\n\n\n\u00a0\n\n\n\u00a0\n\n\n\n\nchromosorb:\n\n\nWAW\n\n\nWAW-DMCS-HP\n\n\n\n\nsieve analysis\n\n\n100 to 120 mesh\n\n\n60 to 80 mesh\n\n\n\n\nStationary phase:\n\n\nHallcomid M 18, 10%\n\n\nHallcomid M 18, 20%\n\n\n\n\nTemperature conditions may vary as a function of the apparatus. In the examples they have been set as follows:\n\n\n\n\n\n\n\n\nColumn\n\n\n\n\nI\n\n\n\n\nII\n\n\n\n\n\nTemperatures:\n\n\n\u00a0\n\n\n\u00a0\n\n\n\n\ncolumn:\n\n\n65 oC\n\n\n75 oC\n\n\n\n\ninjector:\n\n\n150 oC\n\n\n125 oC\n\n\n\n\ndetector:\n\n\n150 oC\n\n\n200 oC\n\n\n\n\nCarrier gas:\n\n\n\u00a0\n\n\n\u00a0\n\n\n\n\nhelium flow rate:\n\n\n45 ml/min\n\n\n60 ml/min\n\n\n\n\ninlet pressure\n\n\n2,5 bar\n\n\n2 bar\n\n\n\n\nInjection:\n\n\n15 \u03bcl\n\n\n15\u03bcl\n\n\n\n\n\n\n\n\n8. MIXTURE FOR ESTABLISHING THE RESPONSE FACTORS\nMake up the following accurately weighed mixture in a stoppered conical flask:\nDichloromethane (4. 3), 30 % (m/m). 1,1,1-trichloroethane (4. 4), 35 % (m/m). Chloroform (4. 1), 35 % (m/m). 9. CALCULATIONS\n9. 1. Calculating a response factor of a substance \u2018p\u2019 relative to a substance \u2018a\u2019 selected as an internal standard\n\n\nLet the first substance be \u2018p\u2019, where:\n\n\n\n\n\n\n\nkp\n\n\n\n=\n\n\nits response factor,\n\n\n\n\nmp\n\n\n\n=\n\n\nits mass in the mixture,\n\n\n\n\nAp\n\n\n\n=\n\n\nits peak area. Let the second substance be \u2018a\u2019, where:\n\n\n\n\n\n\n\nka\n\n\n\n=\n\n\nits response factor (made equal to unity),\n\n\n\n\nMa\n\n\n\n=\n\n\nits mass in the mixture,\n\n\n\n\nAa\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nthen:\n\n\n\nAs examples the following response factors have been obtained (for chloroform: k = l):\nDichloromethane: k1 = 0,78 \u00b1 0,03\n1,1,1-trichloroethane: k2 = 1,00 \u00b1 0,03\n9. 2\u00a0\u00a0\u00a0\nCalculate the % (m/m) of dichloromethane and 1,1,1-trichloroethane present in the sample to be analyzed\n\n\nLet:\n\n\n\n\n\n\n\nma\n\n\n\n=\n\n\nthe mass (in grams) of chloroform introduced,\n\n\n\n\nMs\n\n\n\n=\n\n\nthe mass (in grams) of the sample to be analyzed,\n\n\n\n\nAa\n\n\n\n=\n\n\nthe area of the chloroform peak,\n\n\n\n\nA1\n\n\n\n=\n\n\nthe area of the d ichloromethane peak,\n\n\n\n\nA2\n\n\n\n=\n\n\nthe area of the 1 1,1-trichloroethane peak,\n\n\n\n\nthen:\n\n\n\n\n\n\n10. REPEATABILITY\u00a0(2)\n\nFor a dichloromethane and/or 1,1,1-trichloroethane content of 25 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 2,5 % (m/m)\nIDENTIFICATION AND DETERMINATION OF QUINOLIN-8-OL AND BIS(8-HYDROXYQUINOLINIUM) SULPHATE\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes the identification and quantitative determination of quinolin-8-ol and its sulphate. 2. DEFINITION\nThe quinolin-8-ol and bis(8-hydroxyquinolinium) sulphate content of the sample as determined by this method is expressed in percentage by mass of quinolin-8-ol. 3. PRINCIPLE\n3. 1. Identification\n\n\nIdentification is by thin-layer chromatography. 3. 2. Determination\n\n\nThe determination is carried out by spectrophotometry at 410 nm of the complex obtained by reaction with Fehling's solution. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Quinolin-8-ol. 4. 2. Benzene. In view of its toxicity great care must be taken when working with benzene. 4. 3. Chloroform. 4. 4. Aqueous sodiun hydroxide, 50 % (m/m) solution. 4. 5. Copper sulphate pentahydrate. 4. 6. Potassium sodium tartrate. 4. 7. M hydrochloric acid. 4. 8. 0,5 M sulphuric acid. 4. 9. M sodium hydroxide solution. 4. 10. Ethanol. 4. 11. Butan-1-ol. 4. 12. Glacial acetic acid. 4. 13. 0,1 hydrochloric acid. 4. 14 \u2018Celite 545\u2019or equivalent. 4. 15. Standard solutions\n\n\n\n\n\n\n\n\n\n\n\n\n\n4. 15. 1. Weigh 100 mg of quinolin-8-ol (4. 1) into a 100 ml standard flask. Dissolve in a little sulphuric acid (4. 8) Make up to the mark with sulphuric acid (4. 8). 4. 15. 2. Weigh 100 mg of quinolin-8-ol into a 100 ml standard flask. Dissolve in ethanol (4. 10). Make up to the mark with ethanol (4. 10) and mix. 4. 16. Fehling's solution\n\n\nSolution A\n\nWeigh 7 g of copper sulphate pentahydrate (4. 5) into a 100 ml standard flask. Dissolve in a little water. Make up to the mark with water and mix. Solution B\n\nWeigh 35 g of potassium sodium tartrate (4. 6) into a 100 ml standard flask. Dissolve in 50 ml of water. Add 20 ml of sodium hydroxide (4. 4). Make up to the mark with water and mix. Immediately before use, pipette 10 ml of solution A and 10 ml of solution B into a 100 ml standard flask. Make up to the mark and mix. 4. 17. Eluting solvents for thin-layer chromatography\n\n\n\n\n\n\n\n\nI\n\n\n:\n\n\nButan-1-ol (4. 11) /acetic acid (4. 12) /water (80: 20: 20; v/v/v). II\n\n\n:\n\n\nChloroform (4. 13) /acetic acid (4. 12) (95: 5; v/v). 4. 18. 2,6-dichloro-4-(chloroin ino)cyclohexa-2,5-dienone, 1 % (m/v) solution in ethanol (4. 10). 4. 19. Sodium carbonate, 1 % (m/v) solution in water. 4. 20. Ethanol (4. 10), 30 % (v/v) solution in water. 4. 21. Disodium dihydrogen ethylenediaminetetraacetate, 5 % (m/v) solution in water. 4. 22. Buffer solution, pH 7\n\nWeigh 27 g of potassium dihydrogenorthophosphate anhydrous and 70 g of dipotassium hydrogenorthophosphate trihydrate into a one litre standard flask. Make up to the mark with water. 4. 23. Prepared thin-layer plates\n\nReady made thin-layer plates of a thickness of 0,25 mm (e. g. Merck Kieselgel 60 or equivalent). Before use, spray with 10 ml of reagent (4. 21) and dry at 80 oC. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. 100 ml round-bottom flask with ground-glass neck. 5. 2. Standard flasks. 5. 3. Graduated pipettes, 10 and 5 ml. 5. 4. Bulb pipettes, 20, 15, 10 and 5 ml. 5. 5. Separating funnels, 100, 50 and 25 ml. 5. 6. Pleated filter paper, diameter 90 mm. 5. 7. Rotary evaporator. 5. 8. Reflux condenser with ground-glass neck. 5. 9. Spectrophotometer. 5. 10. Optical cells of 10 mm path length. 5. 11. Stirrer hotplate. 5. 12. Glass chromatography column dimensions: 160 mm long with a diameter of 8 mm, a construction at the lower end containing a glass-wool plug, and an adaptor at the upper end for application of pressure. 6. PROCEDURE\n6. 1. Identification\n\n\n6. 1. 1. Liquid samples\n\n\n\n\n\n\n\n\n\n6. 1. 1. 1. The pH of part of the test sample is adjusted to 7. 5 and 10 \u03bcl are spotted on the starting line of a pretreated silica gel thin-layer plate (4. 23). 6. 1. 1. 2. 10 and 30 \u03bcl of the standard solution (4. 15. 2) is spotted on two more points of the starting line after which the plate is developed in one of the two eluents (4. 17). 6. 1. 1. 3. When the solvent front has advanced 150 mm, the plate is dried at 110 oC (for 15 minutes). Under a UV lamp (366 nm) the quinolin-8-ol spots fluoresce yellow. 6. 1. 1. 4. Spray the plate with sodium carbonate solution (4. 19). Dry and spray with 2,6-dichloro-4-(chloroimino)cyclohexa-2,5-dienone solution (4. 18). The quinolin-8-ol becomes visible as a blue spot. 6. 1. 2. Solid samples or creams\n\n\n\n\n\n\n\n\n6. 1. 2. 1. Disperse 1 g of the sample in 5 ml of buffer solution (4. 22). Then transfer with 10 ml of chloroform (4. 3) into a separating funnel and shake. After separation of the chloroform ayer the aqueous layer is extracted twice more with 10 ml of chloroform (4. 3) Evaporate the combined and filtered chloroform extracts almost to dryness in a 100 ml round-bottom flask (5. 1) on the rotary evaporator (5. 7). Dissolve the res due in 2 ml of chloroform (4. 3) and spot 10 and 30\u03bcl of the solution obtained on a silica gel, thin-layer plate (4. 23) in accordance with the method described in 6. 1. 1. 1 onward. 6. 1. 2. 2. Apply 10 and 30 \u03bcl of the standard solution (4. 15. 2) to the plate and continue as described in 6. 1. 1. 2 to 6. 1. 1. 4. 6. 2. Determination\n\n\n6. 2. 1. Liquid samples\n\n\n\n\n\n\n\n\n\n6. 2. 1. 1. Weigh 5 g of the sample into a 100 ml round-bottom flask. Add 1 ml of a suphuric acid solution (4. 8) and evaporate the mixture almost to dryness under reduced pressure at 50 oC. 6. 2. 1. 2. Dissolve this residue in 20 ml of warm water. Transfer into a 100 ml standard flask. Rinse three times with 20 ml of water. Make up to 100 ml with water and mix. 6. 2. 1. 3. Pipette 5 ml of this solution into a 50 ml separating funnel (5. 5). Add 10 ml of Fehling's solution (4. 16). Extract the quinolin-8-ol copper complex [oxine copper (ISO)] obtained with three times 8 ml of chloroform (4. 3). 6. 2. 1. 4. Filter and collect the chloroform layers in a 25 ml standard flask (5. 2). Make up to the mark with chloroform (4. 3) and shake. Measure the optical density of the yellow solution against chloroform at 410 nm. 6. 2. 2. Solid samples or creams\n\n\n\n\n\n\n\n\n\n6. 2. 2. 1. Weigh 0,500 g of the sample into a 100 ml round-bottom flask (4. 1). Add 30 ml of benzene (4. 2) and 20 ml of hydrochloric acid (4. 7). Boil the contents of the flask under reflux, with stirring, for 30 minutes. 6. 2. 2. 2. Transfer the contents of the flask into a 100 ml separating funnel (5. 5). Rinse with 5 ml of 1 N HC1 (4. 7). Transfer the aqueous phase into a round-bottom flask (5. 1) and wash the benzene phase with 5 ml of hydrochloric acid (4. 7). 6. 2. 2. 3. In the case of emulsions that impede further treatment, mix 0,500 g of the sample with 2 g of Celite 545 (4. 14) to form a freely flowing powder. Transfer the mixture in small portions into a glass chromatography column (5. 12). After each addition, tarmp down the column packing. As soon as the whole of the mixture has been transferred into the column, elute with hydrochloric acid (4. 13) in such a way that 10 ml of eluate is obtained in approximately 10 minutes (if necessary, this elution can be performed under a slight nitrogen pressure). During the elution it must be ensured that there is always some hydrochloric acid above the column packing. The first 10 ml of eluate is further treated as described in 6. 2. 2. 4. 6. 2. 2. 4. Evaporate the collectec aqueous phases (6. 2. 2. 2) or the eluate (6. 2. 2. 3) almost to dryness in the rotary evaporator under reduced pressure. 6. 2. 2. 5. Dissolve the residue in 6 ml of the sodium hydroxide solution (4. 9). Add 20 ml of Fehling's solution (4. 16) and transfer the contents of the flask into a 50 ml separating funnel (5. 5) Rinse the flask with 8 ml of chloroform (4. 3). Shake and filter the chloroform phase into a 50 ml standard flask (5. 2). 6. 2. 2. 6. Repeat the extraction three times with 8 ml of chloroform (4. 3). Filter the chloroform phases and collect in the 50 ml flask. Make up to the mark with chloroform (4. 3) and shake. Measure the optical density of the yellow solution against chloroform (4. 3) at 410 nm. 7. STANDARD CURVE\nInto four 100 ml round-bottom flasks (5. 1), each containing 3 ml of 30 % aqueous ethanol (4. 20), pipette 5, 10, 15 and 20 ml portions of the standard solution (4. 15. 1) corresponding to 5, 10, 15 and 20 mg of quinolin-8-ol. Proceed as described in 6. 2. 1. 8. CALCULATION\n8. 1. Liquid samples\n\n\n\nwhere:\n\n\n\n\n\n\n\na\n\n\n=\n\n\nmilligrams of quinolin-8-ol on the standard curve (7),\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in milligrams) of the test portion (6. 2. 1. 1). 8. 2. Solid samples or creams\n\n\nQuinolin-8-ol content (in % (m/m)) \n\nwhere:\n\n\n\n\n\n\n\na\n\n\n=\n\n\nmilligrams of quinolin-8-ol on the standard curve (7),\n\n\n\n\nm\n\n\n=\n\n\nthe mass ( in milligrams) of test portion (6. 2. 2. 1). 9. REPEATABILITY\u00a0(3)\n\nFor a content of about 0,3 % quinolin-8-ol, the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,02 %. DETERMINATION OF AMMONIA\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes the determination of free ammonia in cosmetic products. 2. DEFINITION\nThe ammonia content of the sample determined in accordance with this method is expressed in percentage by mass of ammonia. 3. PRINCIPLE\nBarium chloride solution is added to a test portion of the cosmetic product diluted in an aqueous methanol medium. Any precipitate which may form is filtered or centrifuged off. This procedure avoids the loss of ammonia, during steam distillation, from certain ammonium salts such as the carbonate and hydrogencarbonate and those of the fatty acids, with the exception of ammonium acetate. The ammonia is steam distilled from the filtrate or supernatant and is determined by potentiometric or other titration. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Methanol. 4. 2. Barium chloride dihydrate, 25 % (m/v) solution. 4. 3. Orthoboric acid, 4 % (m/v) solution. 4. 4. Sulphuric acid, 0,25 M standard solution. 4. 5. Anti-foam liquid. 4. 6. Sodium hydroxide, 0,5 M standard solution. 4. 7. Indicator, if required: mix 5 ml of a 0,1 % (m/v) methyl red solution in ethanol with 2 ml of 0,1 % (m/v) methylene blue solution in water. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Usual laboratory apparatus. 5. 2. Centrifuge with stoppered 100 ml bottles. 5. 3. Steam distillation apparatus. 5. 4. Potentiometer. 5. 5. Indicating glass electrode and dimercury dichloride (calomel) reference electrode. 6. PROCEDURE\n\n\n\n\n\n\n\n\n6. 1. Weigh into a 100 ml standard flask a mass (m) of the sample corresponding to 150 mg maximum of ammonia. 6. 2. Add 10 ml of water, 10 ml of methanol (4. 1) and 10 ml of barium chloride solution (4. 2). Make up to 100 ml with methanol (4. 1). 6. 3. Mix and leave overnighs in the refrigerator (5 oC). 6. 4. Then filter, or centrifuge the still cold solution in closed tubes for 10 minutes, so as to obtain a clear filtrate or supernatant layer. 6. 5. Pipette 40 ml of this clear solution into the steam distillation apparatus (5. 3), followed by 0,5 ml of antifoam liquid (4. 5), where appropriate. 6. 6. Distil and collect 200 ml of distillate in a 250 ml beaker containing 10 ml of standard sulphuric acid (4. 4) and 0,1 ml of indicator (4. 7). 6. 7. Back titrate the excess acid with standard sodium hydroxide solution (4. 6). 6. 8. NB: For potentiometric determination, collect 200 ml of distillate in a 250 ml beaker containing 25 ml of orthoboric acid solution (4. 3) and titrate with standard sulphuric acid (4. 4), recording the neutralization curve. 7. CALCULATIONS\n7. 1. Calculation in the case of back titration\n\n\nLet:\n\n\n\n\n\n\n\nV1\n\n\n\n=\n\n\nthe volume (in inillilitres) of the sodium hydroxide solution (4. 6) used,\n\n\n\n\nM1\n\n\n\n=\n\n\nits actual molarity (4. 6),\n\n\n\n\nM2\n\n\n\n=\n\n\nthe actual molarity factor of the sulphuric acid solution (4. 4),\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in milligrams) of the test portion (6. 1) taken,\n\n\n\n\nthen:\n\n\n\n7. 2. Calculation in the case of direct potentiometric titration\n\n\nLet:\n\n\n\n\n\n\n\nV2\n\n\n\n=\n\n\nthe volume (in millilitres) of the sulphuric acid solution (4. 4) used,\n\n\n\n\nM2\n\n\n\n=\n\n\nits actual molarity (4. 4),\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in milligrams) of the test portion (6. 1) taken,\n\n\n\n\nthen:\n\n\n\n8. REPEATABILIT Y\u00a0(4)\n\nFor a content of about 6 % ammonia, the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,6 %. IDENTIFICATION AND DETERMINATION OF NITROMETHANE\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method is suitable for the identification and determination of nitromethane at up to about 0,3 % in cosmetic products packed in aerosol dispensers. 2. DEFINITION\nThe nitromethane content of the sample determined according to this method is expressed in percentage by mass of nitromethane, in the total aerosol dispenser content. 3. PRINCIPLE\nThe nitromethane is identified by colour reaction. Nitromethane is determined gas chromatographically after addition of an internal standard. 4. IDENTIFICATION\n4. 1. Reagents\n\n\nAll reagents should be of analytical purity. 4. 1. 1. Sodium hydroxide, 0,5 M solution. 4. 1. 2. Folin's reagent\nDissolve 0,1 g of sodium 3,4-dihydro-3,4-dioxonaphthalene-l-sulphonate in water and dilute to 100 ml. 4. 2. Procedure\n\n\nTo 1 ml of sample add 10 ml of 4. 1. 1 and 1 ml of 4. 1. 2. A violet coloration indicates the presence of nitromethane. 5. DETERMINATION\n5. 1. Reagents\n\nAll reagents must be of analytical quality. 5. 1. 1. Chloroform (internal standard 1). 5. 1. 2. 2,4-dimethylheptane (internal standard 2). 5. 1. 3. Ethanol, 95 %. 5. 1. 4. Nitromethane. 5. 1. 5. Chloroform reference solution\nInto a tared 25 ml volumetric flask, introduce about 650 mg of chloroform (5. 1. 1). Accurately reweigh the flask and contents. Make up to 25 ml with 95 % ethanol (5. 1. 3). Weigh and calculate the percentage by mass of chloroform in this solution. 5. 1. 6. 2,4-dimethylheptane reference solution\nMake up in a similar manner to the chloroform reference solution but weigh 270 mg of 2,4-dimethylheptane (5. 1. 2) into the 25 ml volumetric flask. 5. 2. Apparatus\n\n\n\n\n\n\n\n\n\n\n5. 2. 1. Gas chromatograph with flame ionization detector. 5. 2. 2. Apparatus for sampling of aerosols (transfer bottle, microsyringe connectors, etc. ) as described in Chapter II of the Annex to Commission Directive 80/1335/EEC of 22 December 1980\u00a0(5). 5. 2. 3. Usual laboratory apparatus. 5. 3. Procedure\n\n5. 3. 1. Preparation of the sample\n\nInto a 100 ml tared transfer bottle, purged or evacuated according to the procedure described in 5. 4 of Chapter II of the abovementioned Directive, introduce about 5 ml of either of the internal standard solutions (5. 1. 5 or 5. 1. 6). Use a 10 or 20 ml glass syringe, without needle, adapted to the transfer piece following the technique described in paragraph 5 of Chapter II of the above-mentioned Commission Directive. Reweigh to determine the quantity introduced. Using the same technique, transfer into this bottle about 50 g of the contents of the aerosol dispenser sample. Again reweigh to determine the quantity of sample transferred. Mix well. Inject about 10 \u03bcl using the specified microsyringe (5. 2. 2). Make five injections. 5. 3. 2. Preparation of the standard\n\nInto a 50 ml volumetric flask, accurately weigh about 500 mg of nitromethane (5. 1. 4) and either 500 mg of chloroform (5. 1. 1) or 210 mg of 2,4-dimethylheptane (5. 1. 2). Make up to volume with 95 % ethanol (5. 1. 3). Mix well. Place 5 ml of this solution into a 20 mg volumetric flask. Make up to volume with 95 % ethanol (5. 1. 3). Inject about 10 \u03bcl using the specified microsyringe (5. 2. 2). Make five injections. 5. 3. 3. Gas chromatographic conditions\n\n5. 3. 3. 1. Column\n\nThis is in two parts, the first containing didecyl phthalate on Gas Chrom Q as packing, the second having Ucon 50 HB 280X on Gas Chrom Q as packing. The prepared combined column must yield a resolution \u2018R\u2019 equal to, or better than, 1,5, where:\n\n\n\nlet:\n\n\n\n\n\n\n\nr1 and r2\n\n\n\n=\n\n\nretention times (in minutes),\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). As examples the following two parts yield the required resolution:\nColumn A:\nMaterial: stainless steel. Length: 1,5 m. Diameter: 3 mm. Packing: 20 % didecyl phthalate on Gas Chrom Q (100 to 120 mesh). Column B:\nMateria: stainless steel. Length: 1,5 m. Diameter: 3 mm. Packing: 20 % Ucon 50 HB 280X on Gas Chrom Q (100 to 120 mesh). 5. 3. 3. 2. Detector\n\nA suitable sensitivity setting for the electrometer of the flame ionization detector is 8 \u00d7 l0-10A. 5. 3. 3. 3. Temperature conditions\n\nThe following have been found suitable:\nInjection port: 150 oC,\nDetector: 150 oC,\nColumn: between 50 and 80 oC depending upon individual columns and apparatus. 5. 3. 3. 4. Suitable gas supplies\n\nCarrier gas: nitrogen. Pressure: 2,1 bar. Flow: 40 ml/min\nDetector supplies: as specified by the makers of the detector. 6. CALCULATIONS\n6. 1. Response factor of nitromethane, calculated with reference to the internal standard used\n\n\nIf \u2018n\u2019 represents nitromethane:\nlet:\n\nkn\n= its response factor,\n\nm'n\n= its mass (in grams) in the mixture,\n\nS'n\n= its peak area. If \u2018c\u2019 represents the internal standard, chloroform or 2,4-dimathylheptane:\nlet:\n\n\n\n\n\n\n\nm'c\n\n\n\n=\n\n\nits mass (in grams) in the mixture,\n\n\n\n\nS'c\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nthen:\n\n\n\n(kn is a function o2 the apparatus). 6. 2. Concentration of nkromethane in the sample\n\n\nIf \u2018n\u2019 represents nitromethane:\nlet:\n\n\n\n\n\n\n\nkn\n\n\n\n=\n\n\nits response factor,\n\n\n\n\nSn\n\n\n\n=\n\n\nits peak area. If \u2018c\u2019 represents the internal standard, chloroform or 2,4-dimethylheptane:\nlet:\n\n\n\n\n\n\n\nmc\n\n\n\n=\n\n\nits mass (in grans) in the mixture,\n\n\n\n\nSc\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nM\n\n\n=\n\n\nthe mass (in grams) of the aerosol transferred,\n\n\n\n\nthen the % (m/m) nitromethane in the sample is:\n\n\n\n7. REPEATABILITY\u00a0(6)\n\nFor a nitromethane content of about 0,3 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,03 % (m/m). IDENTIFICATION AND DETERMINATION OF MERCAPTOACETIC ACID IN HAIR-WAVING, HAIR-STRAIGHTENING AND DEPILATORY PRODUCTS\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes he identification and determination of mercaptoacetic acid in hair-waving, hair-straightening and depilatory products in which other reducing agents may be present. 2. DEFINITION\nThe mercaptoacetic acid content of the sample determined according to this method is expressed in percentage by mass of mercaptoacetic acid. 3. PRINCIPLE\nMercaptoacetic acid is identified by spot tests and by thin-layer chromatography and is determined by iodometry or gas chromatography. 4. IDENTIFICATION\n4. 1. Identification by spot tests\n\n\n4. 1. 1. Reagents\n\nAll reagents should be of analytical purity. 4. 1. 1. 1. Lead di(acetate) papes. 4. 1. 1. 2. Hydrochloric acid solution (one volume of concentrated hydrochloric acid plus one volume of water)\n\n\n\n\n4. 1. 2. Procedure\n4. 1. 2. 1. Identification of mercaptoacetic acid by means of a colour reaction with lead di(acetate)\n\nPlace a drop of the sample to be analyzed on lead di(acetate) paper (4. 1. 1. 1). If an intense yellow colour appears, mercaptoacetic acid is probably present. Sensitivity: 0,5 %. 4. 1. 2. 2. Characterization of inorganic sulphides by the formulation of hydrogen sulphide on acidification\n\nIntroduce, into a test tube, a few milligrams of the sample to be studied. Add 2 ml of distilled water and 1 ml of hydrochloric acid (4. 1. 1. 2). Hydrogen sulphide, recognizable by its smell, is evolved and a black lead sulphide precipitate forms on the lead di(acetate) paper (4. 1. 1. 1). Sensitivity: 50 ppm. 4. 1. 2. 3. Characterization of sulphites by the formation of sulphur dioxide upon acidification\n\nProceed as described in 4. 1. 2. 2. Bring to the boil. The sulphur dioxide is recognizable by its smell and by its reducing properties in respect, for example, of permanganate ions. 4. 2. Identification by thin-layer chromatography\n4. 2. 1. Reagents\n\nAll reagents, except where otherwise stated, should be of analytical purity. 4. 2. 1. 1. Mercaptoacetic acid (thioglycollic acid), 98 % minimum purity assayed by iodometry. 4. 2. 1. 2. 2,2'-dithiodi(acetic acid), 99 % minimum purity assayed by iodometry. 4. 2. 1. 3. 2-mercaptopropionic acid (thiolactic acid), 95 % minimum purity assayed by iodometry. 4. 2. 1. 4. 3-mercaptopropionic acid, 98 % minimum purity assayed by iodometry. 4. 2. 1. 5. 3-mercaptopropane-l,2-diol (1-thioglycerol), 98 % minimum purity assayed by iodometry. 4. 2. 1. 6. Thin-layer plates, silica gel, ready prepared, 0,25 mm thickness. 4. 2. 1. 7. Thin-layer plates, aluminium oxide, Merck F 254 E or equivalent. 4. 2. 1. 8. Hydrochloric acid, concentrated, d4\n20 = 1,19 g/ml. 4. 2. 1. 9. Ethyl acetate. 4. 2. 1. 10. Chloroform. 4. 2. 1. 11. Diisopropyl ether\n\n\n\n\n\n\n\n\n\n\n\n\n4. 2. 1. 12. Carbon tetrachloride. 4. 2. 1. 13. Acetic acid, glacial. 4. 2. 1. 14. Potassium iodide, 1 % (m/v) solution in water. 4. 2. 1. 15. Platinum tetrachloride, 0,1 % (m/v) solution in water. 4. 2. 1. 16. Eluting solvents\n\n\n\n\n\n\n\n\n\n4. 2. 1. 16. 1. Ethyl acetate (4. 2. 1. 9), chloroform (4. 2. 1. 10), diisopropyl ether (4. 2. 1. 11), acetic acid (4. 2. 1. 13) (20: 20: 10: 10, by volume). 4. 2. 1. 16. 2. Chloroform (4. 2. 1. 10), acetic acid (4. 2. 1. 13) (90: 20, by volume). 4. 2. 1. 17. Detection reagents\n\n\n\n\n\n\n\n\n\n4. 2. 1. 17. 1. Mix, immediately before use, equal volumes of solution (4. 2. 1. 14) and solution (4. 2. 1. 15). 4. 2. 1. 17. 2. Bromine solution 5 % (m/v):\nDissolve 5 g of bromine in 100 ml of carbon tetrachloride (4. 2. 1. 12). 4. 2. 1. 17. 3. Fluorescein solution, 0,1 % (m/v):\nDissolve 100 mg of fluorescein in 100 ml of ethanol. 4. 2. 1. 17. 4. Hexaammonium heptamolybdate, 10 % (m/v) solution in water. 4. 2. 1. 18. Reference solutions\n\n\n\n\n\n\n\n\n\n4. 2. 1. 18. 1. Mercaptoacetic acid (4. 2. 1. 1), 0,4 % (m/v) solution in water. 4. 2. 1. 18. 2. 2,2'-dithiodi(acetic) acid (4. 2. 1. 2), 0,4 % (m/v) solution in water. 4. 2. 1. 18. 3. 2-mercaptopropionic acid (4. 2. 1. 3), 0,4 % (m/v) solution in water. 4. 2. 1. 18. 4. 3-mercaptopropionic acid (4. 2. 1. 4), 0,4 % (m/v) solution in water. 4. 2. 1. 18. 5. 3-mercaptopropane-l,2-diol (4. 2. 1. 5), 0,4 % (m/v) solution in water. 4. 2. 2. Apparatus\n\nUsual apparatus for thin-layer chromatography. 4. 2. 3. Procedure\n\n4. 2. 3. 1. Treatment of samples\n\nAcidify to pH 1 with a few drops of hydrochloric acid (4. 2. 1. 8) and filter if necessary. In certain cases it may be advisable to dilute the sample. If so acidify it with hydrochloric acid before dilution. 4. 2. 3. 2. Elution\n\nPlace on the plate 1 \u03bcl of sample solution (4. 2. 3. 1) and one litre of each of the five reference solutions (4. 2. 1. 18). Dry carefully in a gentle current of nitrogen and elute the plate with solvents (4. 2. 1. 16. 1 or 4. 2. 1. 16. 2). Dry the plate as quickly as possible to minimize oxidation of the thiols. 4. 2. 3. 3. Detection\n\nSpray the plate with one of the three reagents (4. 2. 1. 17. 1, 4. 2. 1. 17. 3 or 4. 2. 1. 17. 4). If the plate is sprayed with reagent (4. 2. 1. 17. 3), further treat it with bromine vapour (e. g. in a tank containing a small beaker of the reagent (4. 2. 1. 17. 2)) until the spots are visible. Detection with the spray reagent (4. 2. 1. 17. 4) will be satisfactory only if the drying time for the thin layer has not exceeded 30 minutes. 4. 2. 3. 4. Interpretation\n\nCompare the Rf values and the colour of the reference solutions with those of the standards. The mean Rf values given below as a rough guide have only a comparative value. They depend upon:\n\n\n\n\n\n\n\u2014\n\n\nthe state of activation of the thin layer at the time of chromatographing,\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\nthe temperature of the chromatography tank. Examples of Rf values obtained on a silica gel layer\n\n\n\n\n\n\n\n\n\n\u00a0\n\n\nEluting solvents\n\n\n\n\n4. 2. 1. 16. 1\n\n\n4. 2. 1. 16. 2\n\n\n\n\nMercaptoacetic acid\n\n\n0,25\n\n\n0,80\n\n\n\n\n2-mercaptopropionic acid\n\n\n0,40\n\n\n0,95\n\n\n\n\n2,2'-dithiodi(acetic) acid\n\n\n0,00\n\n\n0,35\n\n\n\n\n3-mercaptopropionic acid\n\n\n0,45\n\n\n0,95\n\n\n\n\n3-mercaptopropane-1,2 diol\n\n\n0,45\n\n\n0,35\n\n\n\n\n5. DETERMINATION (see NB)\nThe determination should always start with the iodometric procedure. 5. 1. lodometry\n\n\n5. 1. 1. Principle\n\nThe determination is performed by oxidation of the \u2018-SH\u2019 group with iodine in an acid medium according to the equation:\n2 HOOC-CH2SH + I2 \u2192 (HOOC-CH2-S)2 + 2 I- + 2 H+\n\n5. 1. 2. Reagents\n\nIodine, 0,05 M standard solution. NB: The determination of mercaptoacetic acid must be carried out on unused product from freshly opened containers in order to prevent oxidation. 5. 1. 3. Apparatus\n\nUsual laboratory equipment. 5. 1. 4. Procedure\n\nAccurately weigh out a quantity of between 0,5 and 1 g of the sample into a 150 ml stoppered conical flask containing 50 ml of distilled water. Add 5 ml of hydrochloric acid (4. 1. 1. 2) (pH of solution about 0) and titrate with iodine solution (5. 1. 2) until a yellow colour appears. Use an indicator (e. g. starch solution or carbon tetrachloride) if desired. 5. 1. 5. Calculation\n\nThe mercaptoaceric acid content is calculated according to the formula:\n\n\n\nwhere:\n\n\n\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in grams) of the test portion,\n\n\n\n\nn\n\n\n=\n\n\nthe volume of iodine solution (5. 1. 2) used. 5. 1. 6. Remarks\n\nIf the result, calculated as mercaptoacetic acid, is 0,1 % or more below the authorized maximum concentration, there is no point in carrying out further determinations. If the result is equal to or above the permitted maximum concentration, and the identification has revealed the presence of several reducing agents, it is necessary to carry out a gas chromatographic determination. 5. 2. Gas chromatograyhy\n\n\n5. 2. 1. Principle\nMercaptoacetic acid is separated from the excipient by precipitation with cadmium di(acetate) solution. After methylation with diazomethane, prepared either in situ or in advance in a diethyl ether solution, the methyl derivative of the mercaptoacetic acid is measured by gas/liquid chromatography, methyl octanoate being used as the internal standard. 5. 2. 2. Reagents\n\nAll the reagents must be of analytical quality. 5. 2. 2. 1. Mercaptoacetic acid, 98 %. 5. 2. 2. 2. Hydrochloric acid, d4\n10 = 1,19 g/ml. 5. 2. 2. 3. Methanol. 5. 2. 2. 4. Cadmium di(acetate) dihydrate, 10 % (m/v) solution in water. 5. 2. 2. 5. Methyl octanoate, 2 % (m/v) solution in methanol. 5. 2. 2. 6. Acetate buffer solution (pH 5):\nSodium acetate trihydrate, 77 g. Acetic acid (glacial), 27,5 g. Demineralized water to give a final volume of one litre. 5. 2. 2. 7. Hydrochloric acid, 3 M solution in methanol (5. 2. 2. 3), freshly prepared. 5. 2. 2. 8. 1-methyl-3-nitro 1 -nitrosoguanidine. 5. 2. 2. 9. Sodium hydroxide, 5 M solution. 5. 2. 2. 10. Iodine, 0,05 M standard solution. 5. 2. 2. 11. Diethyl ether. 5. 2. 2. 12. Diazomethane solution prepared from iV-methyl-AT-nitrosotoluen-4-sulfonamide (Fieser, Reagents for Organic Synthesis (Wiley), 1967)\nThe solution obtained contains about 1,5 g of diazomethane in 100 ml of diethyl ether. As diazomethane is a toxic and very unstable gas, all experiments must be carried out under a powerful hood and the use of ground-glass apparatus must be avoided (there are special kits for this purpose). 5. 2. 3. Apparatus\n\n\n\n\n\n\n\n\n\n5. 2. 3. 1. Usual laboratory equipment. 5. 2. 3. 2. Apparatus for the preparation of diazomethane for in situ methylation (see Fales, H. M. , Jaouni, T. M. and Babashak, J. F. , Analyt. Chem. 1973, 45, 2302). 5. 2. 3. 3. Apparatus for the advance preparation of diazomethane (Fieser). 5. 2. 4. Preparation of the sample\n\nWeigh accurately into a 50 ml centrifuge tube enough of the sample to give a presumed quantity of 50 to 70 mg of mercaptoacetic acid. Acidify with a few drops of hydrochloric acid (5. 2. 2. 2) to obtain a pH of about 3. Add 5 ml of demineralized water and 10 ml of acetate buffer solution (5. 2. 2. 6). Check with pH paper that the pH value is about 5. Then add 5 ml of cadmium di(acetate) solution (5. 2. 2. 4). Wait 10 minutes and then centrifuge for at least 15 minutes at 4\u00a0000 g. Remove the supernatant liquid which may contain an insoluble fat (in the case of cream products). This fat cannot be confused with the thiols which collects in a compact mass at the bottom of the tube. Check that no precipitation occurs when a few drops of cadmium di(acetate) solution (5. 2. 2. 4) are added to the supernatant. Where earlier identification revealed no reducing agents other than the thiols, check by iodometry that the thiol present in the supernatant liquid does not exceed 6 to 8 % of the initial quantity. Introduce 10 ml of methanol (5. 2. 2. 3) into the centrifuge tube containing the precipitate and finely disperse the precipitate with a stirring rod. Centrifuge again for at least 15 minutes at 4\u00a0000 g. Pour off the supernatant and check for the absence of thiols. Wash the precipitate a second time by the same procedure. Still using the same centrifuge tube, add:\n\n\n\n\n\n\n\u2014\n\n\n2 ml of methyl octanoate solution (5. 2. 2. 5),\n\n\n\n\n\n\n\n\n\n\n\u2014\n\n\n5 ml of hydrochloric acid in methanol (5. 2. 2. 7). Completely dissolve the thiols (a little insoluble matter may persist from the excipient). This is solution \u2018S\u2019. With an aliquot of this solution, check iodometrically that the thiols content is at least 90 % of that obtained in 5. 1. 5. 2. 5. Methylation\n\nThe methylation is carried out either by in situ preparation (5. 2. 5. 1) or with previously prepared diazomethane solution (5. 2. 5. 2). 5. 2. 5. 1. Methylation in situ\n\n\nInto the methylation apparatus (5. 2. 3. 2) containing 1 ml of ether (5. 2. 2. 11) introduce 50 \u03bcl of solution \u2018S\u2019 and methylate by the method (5. 2. 3. 2) with about 300 mg of l-methyl-3 nitro-1-nitrosoguanidine (5. 2. 2. 8). After 15 minutes (the ether solution should be yellow to indicate excess diazomethane) transfer the sample solution to a 2 ml bottle having an airtight stopper. Place in the refrigerator overnight. Methylate two samples simultaneously. 5. 2. 5. 2. Methylation with the previously prepared diazomethane solution\n\nIntroduce, into a 5 ml stoppered flask, 1 ml of diazomethane solution (5. 2. 2. 12) then 50 \u03bcl of solution \u2018S\u2019. Leave in the refrigerator overnight. 5. 2. 6. Preparation of the standard\n\nPrepare a standard solution of mercaptoacetic acid (5. 2. 2. 1) of known strength containing about 60 mg of pure mercaptoacetic acid (5. 2. 2. 1) in 2 ml. This is solution \u2018E\u2019. Precipitate, assay and methylate as described in 5. 2. 4 and 5. 2. 5. 5. 2. 7. Gas chromatographic conditions\n\n\n\n\n\n\n\n\n\n5. 2. 7. 1. Column\nType: stainless steel. Length: 2 m. Diameter: 3 mm. 5. 2. 7. 2. Packing\n20 % didecyl phthalate/chromosorb, WAW 80 to 100 mesh. 5. 2. 7. 3. Detector\nFlame ionization. A suitable sensitivity setting for the electrometer of the flame ionization detector is 8 \u00d7 10-10 A. 5. 2. 7. 4. Gas supplies\nCarrier gas: nitrogen. pressure: 2,2 bar,\nflow: 35 ml/min. Auxiliary gas: hydrogen. pressure: 1,8 bar,\nflow: 15 ml/min. Detector supplies: as specified by the makers of the apparatus. 5. 2. 7. 5. Temperature conditions\nInjector: 200 oC\nDetector: 200 oC\nColumn: 90 oC\n\n\n\n\n\n\n\n\n\n\n\n\n5. 2. 7. 6. Recorder chart speed\n5 mm/min. 5. 2. 7. 7. Quantity injected\n3 \u03bcl Carry out five injections. 5. 2. 7. 8. The conditions of chromatography are given as a guide. They permit the achievement of a resolution \u2018R\u2019 equal to, or better than, 1,5, where:\n\n\n\nlet:\n\n\n\n\n\n\n\nr1 and r2\n\n\n\n=\n\n\nretention times (in minutes),\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). It is recommended that chromatography be terminated by regulating the tempera-ture from 90 to 150 oC at a rate of 10 oC per minute so as to eliminate substances liable to interfere with subsequent measurements. 5. 2. 8. Calculations\n\n5. 2. 8. 1. Coefficient of proportionality for mercaptoacetic acid\n\nThis is calculated with respect to methyl octanoate on the basis of a standard mixture. If \u2018t\u2019 represents mercaptoacetic acid:\nlet:\n\n\n\n\n\n\n\nkt\n\n\n\n=\n\n\nits response factor,\n\n\n\n\nm't\n\n\n\n=\n\n\nits mass (in milligrams) in the mixture,\n\n\n\n\nS't\n\n\n\n=\n\n\nits peak area. If \u2018c\u2019 represents methyl octanoate:\nlet:\n\n\n\n\n\n\n\nm'c\n\n\n\n=\n\n\nits mass (in millegrams) in the mixture,\n\n\n\n\nS'c\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nthen: \n\nThis coefficient varies according to the apparatus used. 5. 2. 8. 2. Concentration of mercaptoacetic acid present in the sample\n\nIf \u2018t\u2019 represents mercaptoacetic acid:\nlet:\n\n\n\n\n\n\nkt\n\n\n\nits response factor,\n\n\n\n\n\n\n\n\n\n\n\nSt\n\n\n\n=\n\n\nits peak area. If \u2018c\u2019 represents methyl octanoate:\nlet:\n\n\n\n\n\n\n\nmc\n\n\n\n=\n\n\nits mass (in mill grams) in the mixture,\n\n\n\n\nSc\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nM\n\n\n=\n\n\nthe mass (in milligrams) of the initial test portion,\n\n\n\n\nthen the % (m/m) mercaptoacetic acid present in the sample is:\n\n\n\n6. REPEATABILITY\u00a0(7)\n\nFor a mercaptoacetic acid content of 8 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,8 % (m/m). IDENTIFICATION AND DETERMINATION OF HEXACHLOROPHENE\n\nA. IDENTIFICATION\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method is suitable for all cosmetic products. 2. PRINCIPLE\nHexachlorophene in the sample is extracted with ethyl acetate and identified by thin-layer chromatography. 3. REAGENTS\nAll reagents should be of analytical purity. 3. 1. Sulphuric acid, 4 M solution. 3. 2. Celite AW. 3. 3. Ethyl acetate. 3. 4. Eluting solvent: Benzene containing 1 % (v/v) of glacial acetic acid. 3. 5. Visualizing agent I:\nRhodamine B solution: dissolve 100 mg of Rhodamine B in a mixture of 150 ml of diethyl ether, 70 ml of absolute ethanol and 16 ml of water. 3. 6. Visualizing agent II:\n2,6-dibromo-4-(cMoroimino)cyclohexa-2,5-dienone solution: dissolve 400 mg of 2,6(dibromo-4-(chloroimino)cyclohexa-2,5-dienone in 100 ml of methanol (prepare fresh daily). Sodium carbonate solution: dissolve 10 g of sodium carbonate in 100 ml of demineralized water. 3. 7. Reference solution:\nHexachlorophene, 0,05 % (m/v) solution in ethyl acetate. 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Kiesel gel 254 TLC plates, 200 x 200 mm (or equivalent). 4. 2. Usual TLC equipment. 4. 3. Bath thermostatted at 26 oC to hold the chromatography tank. 5. PREPARATION OF THE TEST SAMPLE\n\n\n\n\n\n\n\n\n5. 1. Thoroughly mix 1 g of homogenized sample with 1 g of Celite AW (3. 2) and 1 ml of sulphuric acid (3. 1). 5. 2. Dry at 100 oC for two hours. 5. 3. Cool and finely powder the dried residue. 5. 4. Extract twice with 10 ml of ethyl acetate (3. 3) each time, centrifuge after each extraction and combine the ethyl acetate layers. 5. 5. Evaporate at 60 oC. 5. 6. Dissolve the residue in 2 ml of ethyl acetate (3. 3). 6. PROCEDURE\n\n\n\n\n\n\n\n\n6. 1. Place 2 \u00b5l of the test sample solution (5. 6) and 2 \u00b5l of the reference solution (3. 7) on a TLC plate (4. 1). 6. 2. Saturate the tank (4. 3) with the eluting solvent (3. 4). 6. 3. Place the TLC plate in the tank and elute up to 150 mm. 6. 4. Remove the TLC plate and dry in a ventilated oven at a temperature of about 105 oC. 6. 5. Visualization\nHexachlorophene spots on the thin-layer plate are visualized as indicated under 6. 5. 1 or 6. 5. 2. 6. 5. 1. Spray the visualizing agent I (3. 5) evenly on the plate. After 30 minutes examine the plate under UV light at 254 nm. 6. 5. 2. Spray the 2,6-dibromo-4-(chloroimino)cyclohexa-2,5-dienone solution of visualizing agent II (3. 6) evenly on the plate. Subsequently spray the plate with sodium carbonate solution (3. 6). Examine the plate in daylight after 10 minutes drying at room temperature. 7. INTERPRETATION\n\n\n\n\n\n\n\n\n7. 1. Visualizing agent I (3. 5):\nHexachlorophene is revealed as a bluish spot on a yellow-orange fluorescent background and has an Rf of approximately 0,5. 7. 2. Visualizing agent II (3. 6):\nHexachlorophene is revealed as a sky-blue to turquoise coloured spot on a white background and has an Rf of approximately 0,5. B. DETERMINATION\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method applies to all cosmetic products. 2. DEFINITION\nThe hexachlorophene content of the sample determined according to this method is expressed in percentage by mass of hexachlorophene. 3. PRINCIPLE\nHexachlorophene is determined, after conversion to the methyl derivative, gas chromatographically with an electron capture detector. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Ethyl acetate. 4. 2. N -methyl- N -nitroso-p toluenesulphonamide (diazald). 4. 3. Diethyl ether. 4. 4. Methanol. 4. 5. 2-(2-ethoxyethoxy)ethanol (carbitol). 4. 6. Formic acid. 4. 7. Potassium hydroxide, 50 % (m/m) aqueous solution (prepare fresh daily). 4. 8. Hexane for spectroscopy. 4. 9. Bromochlorophene (standard No 1). 4. 10. 4,4',6,6'-tetrachloro-2,2'-thiodiphenol (standard No 2). 4. 11. 2,4,4'-trichloro- 2-hydroxy-diphenyl ether (standard No 3). 4. 12. Acetone. 4. 13. 4 M sulphuric acid. 4. 14. Celite AW. 4. 15. Formic acid/ethyl acetate, 10 % (v/v) solution. 4. 16. Hexachlorophene. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Usual laboratory glassware. 5. 2. Mini-apparatus for the preparation of diazomethane (Analyt. Chem. , 1973, 45, 2302-2). 5. 3. Gas chromatograph equipped with a 63 Ni source electron capture detector. 6. PROCEDURE\n6. 1. Preparation of the standard solution\n\n\nThe standard is chosen so that it does not interfere with any substance contained in the excipient of the product being analyzed. Usually standard No 1 is most suitable (4. 9). 6. 1. 1. Accurately weigh about 50 mg of standard No 1, 2 or 3 (4. 9, 4. 10 or 4. 11) and 50 mg of hexachlorophene (4. 16) into a 100 ml volumetric flask. Make up to volume with ethyl acetate (4. 1) (solution A). Dilute 10 ml of solution A to 100 ml with ethyl acetate (4. 1) (solution B). 6. 1. 2. Accurately weigh about 50 mg of standard No 1, 2 or 3 (4. 9, 4. 10 or 4. 11) into a 100 ml volumetric flask. Make up to volume with ethyl acetate (4. 1) (solution C ). 6. 2. Preparation of the sample\n\n\u00a0(8)\n\nAccurately weigh 1 g of homogenized sample and mix thoroughly with 1 ml of sulphuric acid (4. 13), 15 ml of acetone (4. 12) and 8 g of Celite AW (4. 14). Air dry the mixture for 30 minutes on a steam bath, then dry for one-and-a-half hours in a ventilated oven. Cool, finely powder the residue and transfer to a glass column. Elute with ethyl acetate (4. 1) and collect 100 ml. Add 2 ml of internal standard solution (solution C) (6. 1. 2). 6. 3. Methylation of the sample\n\n\nCool all reagents and apparatus to between 0 and 4 oC for two hours. Into the external compartment of the diazomethane apparatus place 1,2 ml of the solution obtained in 6. 2 and 0,1 ml of methanol (4. 4). Place about 200 mg of diazald (4. 2) in the central reservoir, add 1 ml of carbitol (4. 5) and 1 ml of diethyl ether (4. 3) and dissolve. Assemble the apparatus, half immerse the apparatus in a bath at 0 oC and introduce by syringe about 1 ml of cooled potassium hydroxide solution (4. 7) into the central reservoir. Ensure that the yellow colour formed from the formation of diazomethane persists. If the yellow colour does not persist, repeat the methylation with a further 200 mg of diazald (4. 2)\u00a0(9). The apparatus is removed from the bath after 15 minutes then left closed at ambient temperature for 12 hours. Open the apparatus, react the excess diazomethane by adding a few drops of a 10 % (v/v) solution of formic acid in ethyl acetate (4. 15) and transfer the organic solution to a 25 ml volumetric flask. Make up to volume with hexane (4. 8). Inject 1,5 \u03bcl of this solution into the chromatograph. 6. 4. Methylation of the standard\n\n\nCool all reagents and apparatus to between 0 and 4 oC for two hours. Into the external compartment of the diazomethane apparatus introduce:\n0,2 ml of solution B (6. 1. 1),\n1 ml of ethyl acetate (4 1),\n0,1 ml of methanol (4. 4). Continue the methylation as described in 6. 3. Inject 1,5 \u00b5l of the resultant solution into the chromatograph. 7. GAS CHROMATOGRAPHY\n\nThe column must yield a resolution \u2018R\u2019 equal to, or better than, 1,5, where:\nlet: \n\n\n\n\n\n\n\n\nr1 and r2\n\n\n\n=\n\n\nretention times (in minutes),\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). The following gas chromatographic conditions have been found suitable:\n\nColumn: stainless steel. Length: 1,7 m. Diameter: 3 mm. Support:\n\nchromosorb: WAW\n\nsieve analysis: 80 to 100 mesh. Stationary phase: 10 % OV 17. Temperatures:\n\n\n\n\n\n\n\ncolumn\n\n\n:\n\n\n280 oC,\n\n\n\n\ninjector\n\n\n:\n\n\n280 oC,\n\n\n\n\ndetector\n\n\n:\n\n\n280 oC. Carrier gas: oxygen-free nitrogen. Pressure\n\n\n:\n\n\n2,3 bar. Flow\n\n\n:\n\n\n30 ml/min. 8. CALCULATION\n8. 1. Proportionality coefficient of hexachlorophene\n\n\nThis is calculated with respect to the chosen standard in relation to the standard mixture. Let:\n\n\n\n\n\n\n\nh\n\n\n=\n\n\nthe hexachlorophene,\n\n\n\n\nkh\n\n\n\n=\n\n\nits proportionality coefficient,\n\n\n\n\nm'h\n\n\n\n=\n\n\nits mas (in grams) in the mixture,\n\n\n\n\nA'h\n\n\n\n=\n\n\nits peak area,\n\n\n\n\ns\n\n\n=\n\n\nthe chosen standard,\n\n\n\n\nm's\n\n\n\n=\n\n\nits mass (in grams) in the mixture,\n\n\n\n\nA's\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nthen: \n\n8. 2. The amount of hexachlorophene in the sample\n\n\nLet:\n\n\n\n\n\n\n\nh\n\n\n=\n\n\nthe hexachlorophene,\n\n\n\n\nkh\n\n\n\n=\n\n\nits proportionality coefficient,\n\n\n\n\nAh\n\n\n\n=\n\n\nits peak area,\n\n\n\n\ns\n\n\n=\n\n\nthe chosen standard,\n\n\n\n\nms\n\n\n\n=\n\n\nits mass (in grams) in the mixture,\n\n\n\n\nAs\n\n\n\n=\n\n\nits peak area,\n\n\n\n\nM\n\n\n=\n\n\nthe mass (in grams) of the sample taken,\n\n\n\n\nthen % (m/m) of hexachlorophene in the sample is:\n\n\n\n9\u00a0\u00a0\u00a0REPEATABILITY\u00a0(10)\n\nFor a content of hexachlorophene of 0,1 % (m/m), the difference between the results of two determinations carried out in parallel on the sample should not exceed an absolute value of 0,005 % (m/m). QUANTITATIVE DETERMINATION OF TOSYLCHLORAMIDE SODIUM (INN)\n(CHLORAMINE-T)\n1. SCOPE AND FIELD OF APPLICATION\nThis method relates to the quantitative thin-layer chromatographic determination of tosylchloramide sodium (chloramine-T) in cosmetic products. 2. DEFINITION\nThe chloramine-T content of the sample, as determined by this method, is expressed as a percentage by mass (m/m). 3. PRINCIPLE\nChloramine-T is completely hydrolyzed to 4-toluenesulphonamide by boiling with hydrochloric acid. The amount of 4-toluenesulphonamide formed is determined photo-densitometrically by thin-layer chromatography. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Tosylchloramide sodium (chloramine-T). 4. 2. Standard solution of 4-toluenesulphonamide: 50 mg of 4-toluenesulphonamide in 100 ml of ethanol (4. 5). 4. 3. Hydrochloric acid, 37 % (m/m), d4\n20 = 1,18 g/ml. 4. 4. Diethyl ether. 4. 5. Ethanol, 96 % (v/v). 4. 6. Development solvent\n\n\n\n\n\n\n\n\n\n\n4. 6. 1. 1-butanol /ethanol (4. 5) /water (40: 4: 9; v/v/v), or\n\n\n\n\n\n\n\n\n\n\n\n\n4. 6. 2. Chloroform /acetone (6: 4; v/v). 4. 7. Ready prepared thin-layer chromatography plates, silica gel 60, without fluorescent indicator. 4. 8. Potassium permanganace. 4. 9. Hydrochloric acid, 15 % (m/m). 4. 10\u00a0\u00a0\u00a0Spray reagent: 2-toluidine, 1 % (m/v) solution in ethanol (4. 5). 5. APPARATUS\n\n\n\n\n\n\n\n\n\n5. 1. Normal laboratory apparatus. 5. 2. Usual thin-layer chromatography equipment. 5. 3. Photodensitometer. 6. PROCEDURE\n6. 1. Hydrolysis\n\n\nWeigh accurate y into a 50 ml round-bottom flask approximately 1 g of the sample (m). Add 5 ml of water and 5 ml of hydrochloric acid (4. 3) and boil for one hour, using a reflux condenser. Immediately transfer the hot suspension with water into a 50 ml graduated flask. Allow to cool and make up to the mark with water. Centrifuge at at least 3000 rpm for five minutes and pass the supernatant liquid through a filter. 6. 2. Extraction\n\n\n\n\n\n\n\n\n\n\n6. 2. 1. Take 30 ml of the filtrate and extract three times with 15 ml of diethyl ether (4. 4). If necessary dry the ethereal phases and collect them in a 50 ml graduated flask. Make up with diethyl ether (4. 4). 6. 2. 2. Take 25 ml of the dried ethereal extract and evaporate to dryness in a nitrogen stream. Redissolve the residue with 1 ml of ethanol (4. 5). 6. 3. Thin-layer chromatography\n\n\n\n\n\n\n\n\n\n\n6. 3. 1. Spot 20 \u03bcl of the ethanolic residue (6. 2) on to a thin-layer chromatography plate (4. 7). At the same time and in the same manner, apply 8, 12, 16 and 20 \u03bcl of the standard solution of 4-toluenesulphonamide (4. 2). 6. 3. 2. Then allow to develop approximately 150 mm in the development solvent (4. 6. 1 or 4. 6. 2). 6. 3. 3. After completely evaporating the development solvent, place the plate for two to three minutes in an atmosphere of chlorine vapour, which is produced by pouring about 100 ml of hydrochloric acid (4. 9) over about 2 g of potassium permanganate (4. 8) in a closed vessel. Remove the excess chlorine by heating the plate to 100 oC for five minutes. Then spray the plate with the reagent (4. 10). 6. 4. Measurement\n\n\nAfter approximately one hour, measure the violet spots by means of a photodensitometer at 525 nm. 6. 5. Plotting the calibration curves\n\n\nPlot the maximum peak height values ascertained for the four 4-toluenesulphonamide spots against the corresponding quantities of 4-toluenesulphonamide (i. e. 4, 6, 8, 10 \u03bcg of 4-toluenesulphonamide per spot). 7. NOTE\nThe method may be controlled by using a solution of 0,1 or 0,2 % (m/v) of chloramine-T (4. 1) treated in the same way as the sample (6). 8. CALCULATION\nThe chloramine-T content of the sample, expressed as a percentage by mass, is calculated as follows:\n\n\n\nwhere:\n\n\n\n\n\n\n\n1,33\n\n\n=\n\n\nthe 4-toluenesulphonamide-chloramine-T conversion factor,\n\n\n\n\na\n\n\n=\n\n\nthe quantity (in \u03bcg) of 4-toluenesulphonamide in the sample as read from the calibration curves,\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in grams) of the sample taken. 9. REPEATABILITY\u00a0(11)\n\nFor a chloramine-T content of about 0,2 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,03 % (m/m). DETERMINATION OF TOTAL FLUORINE IN DENTAL CREAMS\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method is designed for the determination of total fluorine in dental creams. It is suitable for levels not in excess of 0,25 %. 2. DEFINITION\nThe fluorine content of the sample determined according to this method is expressed as a percentage by mass. 3. PRINCIPLE\nThe determination is carried out by gas chromatography. The fluorine from the fluorine containing compounds is converted to triethylfluorosilane (TEFS) by direct reaction with chlorotriethylsilane (TECS) in acid solution and simultaneously extracted with xylene containing cyclohexane as internal standard. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Sodium fluoride, dried at 120 oC to constant mass. 4. 2. Water, double distilled or equivalent quality. 4. 3. Hydrochloric acid, d4\n20 = 1,19 g/ml. 4. 4. Cyclohexane (CH). 4. 5. Xylene with no peaks in the chromatogram prior to the solvent peak when chromatographed under the same conditions as the sample (6. 1). If necessary purify by distillation (5. 8). 4. 6. Chlorotriethylsilane (TECS Merck or an equivalent). 4. 7. Fluorine standard solutions\n\n\n\n\n\n\n\n\n\n\n4. 7. 1. Stock solution, 0,250 mg F-/ml. Weigh accurately 138,1 mg of sodium fluoride (4. 1) and dissolve in water (4. 2). Quantitatively transfer the solution into a 250 ml volumetric flask (5. 5). Dilute to the mark with water (4. 2) and mix. 4. 7. 2. Diluted stock solution, 0,050 mg F-/ml. Transfer by pipette 20 ml of the stock solution (4. 7. 1) into a 100 ml volumetric flask (5. 5). Dilute to the mark with water and mix. 4. 8. Internal standard solution\n\n\nMix 1 ml of cyclohexane (4. 4) and 5 ml of xylene (4. 5). 4. 9. Chlorotriethylsilane/internal standard solution\n\n\nTransfer, by pipette (5. 7), 0,6 ml of TECS (4. 6) and 0,12 ml of the internal standard solution (4. 8) into a 10 ml volumetric flask. Dilute with xylene (4. 5) to the mark and mix. Prepare fresh daily. 4. 10. Perchloric acid, 70 % (m/v). 4. 11. Perchloric acid, 20 % (m/v) in water (4. 2). 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Standard laboratory equipment. 5. 2. Gas chromatograph fitted with a flame ionization detector. 5. 3. Vortex swirl mixer or equivalent. 5. 4. B\u00fchler, shaker, type SMB1 or equivalent. 5. 5. Volumetric flasks, 100 and 250 ml, made of polypropylene. 5. 6. Centrifuge tubes (glass); 20 ml with teflon lined screw-caps, Sovirel type 611-56 or equivalent. Clean tubes and screw-caps by leaching several hours in perchloric acid (4. 11), followed by five subsequent rinsings with water (4. 2), and finally dry at 100 oC. 5. 7. Pipettes, adjustable to deliver volumes of 50 to 200 \u03bcl, with disposable plastics tips. 5. 8. Distillation apparatus, fitted with a three-ball Schneider column or an equivalent Vigreux column. 6. PROCEDURE\n6. 1. Sample analysis\n\n\n\n\n\n\n\n\n\n\n6. 1. 1. Select a dental-cream tube not previously opened, cut open the tube and remove the whole contents. Transfer to a plastics container, mix thoroughly and store under conditions avoiding deterioration. 6. 1. 2. Weigh accurately 150 mg (m) of sample into a centrifuge tube (5. 6), add 5 ml of water (4. 2) and homogenize (5. 3);\n\n\n\n\n\n\n\n\n\n\n\n\n6. 1. 3. Add 1 ml of xylene (4. 5). 6. 1. 4. Add dropwise 5 ml of hydrochloric acid (4. 3) and homogenize (5. 3). 6. 1. 5. Add, by pipette, 0,5 ml of chlorotriethylsilane/internal standard solution (4. 9) into the centrifuge tube (5. 6). 6. 1. 6. Close the tube with the screw-cap (5. 6) and mix for 45 minutes thoroughly on a shaker (5. 4) set at 150 strokes per minute. 6. 1. 7. Centrifuge 10 minutes at such a speed as to produce a clear separation of the phases, uncap the tube, withdraw the organic layer and inject 3 \u03bcl of the organic phase on to the column of the gas chromatograph (5. 2). Remark:\n\nIt takes about 20 minutes before all components are eluted. 6. 1. 8. Repeat the injection, calculate the average peak area ratio (ATEFS/ACH) and read the corresponding amount of fluorine (in milligrams (m1)) from the calibration graph (6. 3). 6. 1. 9. Calculate the total fluorine content of the sample (in per cent by mass of fluorine) as indicated in paragraph 7. 6. 2. Chromatographic conditions\n\n\n\n\n\n\n\n\n\n\n6. 2. 1. Column: stainless steel. Length: 1,8 m. Diameter: 3 mm. Support: Gaschrom Q 80 to 100 mesh. Stationary phase: silicon oil DC 200 or equivalent, 20 %. Condition the column overnight at 100 oC (carrier gas flow at 25 ml nitrogen per minute) and repeat every night. After each fourth or fifth injection recondition the column by heating for 30 minutes at 100 oC. Temperatures:\n\n\n\n\n\n\n\ncolumn\n\n\n:\n\n\n70 oC,\n\n\n\n\ninjector\n\n\n:\n\n\n150 oC,\n\n\n\n\ndetector\n\n\n:\n\n\n250 oC. Gas flow carrier: 35 ml of nitrogen per minute. 6. 3. Calibration graph\n\n\n\n\n\n\n\n\n\n\n6. 3. 1. Place, by pipette, into a series of six centrifuge tubes (5. 6), 0, 1, 2, 3, 4 and 5 ml of the diluted fluoride standard solution (4. 7. 2). Make up the volume in each tube to 5 ml with water (4. 2). 6. 3. 2. Proceed as described under 6. 1. 3 to 6. 1. 6 inclusive. 6. 3. 3. Inject 3 \u03bcl of the organic phase on to the column of the gas chromatograph (5. 2). 6. 3. 4. Repeat the injection and calculate the average peak ratio (ATEFS/ACH). 6. 3. 5. Plot a calibration graph correlating the mass of fluorine (in milligrams) in the standard solutions (6. 3. 1) and the peak area ratio (ATEFS/ACH) measured under 6. 3. 4. Connect the points of the graph with the best fitting straight line calculated by regression analysis. 7. CALCULATION\nThe concentration of the total fluorine content of the sample (in per cent by mass of fluorine) (% (m/m) F) is given by:\n\n\n\nwhere:\n\n\n\n\n\n\n\nm\n\n\n=\n\n\nthe test portion (in milligrams) (6. 1. 2),\n\n\n\n\nm1\n\n\n\n=\n\n\nthe amount of F (in milligrams) read from the calibration graph (6. 1. 8). 8. REPEATABILITY\u00a0(12)\n\nFor a fluorine content of about 0,15 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,012 % (m/m). IDENTIFICATION AND DETERMINATION OF ORGANOMERCURY COMPOUNDS\n\nSCOPE AND FIELD OF APPLICATION\nThe method described below can be used to identify and determine organo-mercury derivatives employed as preservatives in cosmetic products for the eyes. It is applicable to thiomersal (INN) (sodium 2-(ethylmercuriothio)benzoate) and phenylmercury and its salts. A. IDENTIFICATION\n\n1. PRINCIPLE\nThe organomercury compounds are complexed with l,5-diphenyl-3-thiocarba-zone. After extraction of the dithizonate with carbon tetrachloride, silica gel, thin-layer chromatography is carried out. The spots of the dithizonates appear as an orange colour. 2. REAGENTS\nAll the reagents should be of analytical purity. 2. 1. Sulphuric acid, 25 % (v/v). 2. 2. l,5-diphenyl-3-thiocarbazone (dithizone): 0,8 mg in 100 ml carbon tetrachloride (2. 4). 2. 3. Nitrogen. 2. 4. Carbon tetrachloride. 2. 5. Development solvent: hexane /acetone, 90:10 (v/v). 2. 6. Standard solution, 0,001 % in water of:\nsodium 2-(ethylmercuriothio)benzoate,\nethylmercury chloride or methylmercury chloride,\nphenylmercury nitrate or phenylmercury acetate,\nmercury dichloride or mercury di(acetate). 2. 7. Ready prepared silica gel plates (e. g. Merck 5721 or equivalent). 2. 8. Sodium chloride. 3. APPARATUS\n\n\n\n\n\n\n\n\n3. 1. Normal laboratory equipment. 3. 2. Normal TLC apparatus. 3. 3. Phase-separating filter. 4. PROCEDURE\n4. 1. Extraction\n\n\n\n\n\n\n\n\n\n\n4. 1. 1. Dilute 1 g of sample in a centrifuge tube by titration with 20 ml of distilled water. Obtain the maximum dispersion and warm to 60 oC in a water bath. Add 4 g of sodium chloride (2. 8). Shake. Allow to cool. 4. 1. 2. Centrifuge for at least 20 minutes at 4\u00a0500 rev/min in order to separate the greater part of the solid from the liquid. Filter into a separating funnel and add 0,25 ml of sulphuric acid solution (2. 1). 4. 1. 3. Extract several times with 2 or 3 ml of dithizone solution (2. 2) until the last organic phase remains green. 4. 1. 4. Filter each organic phase sequentially through a phase-separating filter (3. 3). 4. 1. 5. Evaporate to dryness in a stream of nitrogen (2. 3). 4. 1. 6. Dissolve with 0,5 ml of carbon tetrachloride (2. 4). Apply this solution immediately as indicated in 4. 2. 1. 4. 2. Separatum and identification\n\n\n\n\n\n\n\n\n\n\n4. 2. 1. Apply immediately 50 \u03bcl of the carbon tetrachloride solution obtained in 4. 1. 6 on to a silica gel plate (2. 7). Treat simultaneously 10 ml of standard solution (2. 6) as in 4. 1 and apply 50 \u03bcl of the solution obtained in 4. 1. 6 on the same plate. 4. 2. 2. Place the plate in the solvent (2. 5) and allow the latter to rise 150 mm. The organomercury compounds appear as coloured spots whose colour is stable, provided the plate is covered by a glass plate immediately the solvent evaporates. For example, the following Rf values are obtained:\n\n\n\n\n\n\n\n\u00a0\n\n\nRf\n\n\nColour\n\n\n\n\nThiomersal\n\n\n0,33\n\n\nOrange\n\n\n\n\nEthylmercury chloride\n\n\n0,29\n\n\nOrange\n\n\n\n\nMethylmercury chloride\n\n\n0,29\n\n\nOrange\n\n\n\n\nPhenylmercury salts\n\n\n0,21\n\n\nOrange\n\n\n\n\nMercury (II) salts\n\n\n0,10\n\n\nOrange\n\n\n\n\nMercury di(acetate)\n\n\n0,10\n\n\nOrange\n\n\n\n\n1,5-diphenyl-3-thiocarbazone\n\n\n0,09\n\n\nPink\n\n\n\n\n\n\n\n\nB. DETERMINATION\n\n1. DEFINITION\nThe content of organomercurial compounds determined by this method is expressed as the percentage by mass (m/m) as mercury in the sample. 2. PRINCIPLE\nThe method consists in measuring the quantity of total mercury present. It is thus necessary to have first made sure that no mercury in an inorganic state is present and to have identified the organomercurial derivative contained in the sample. After mineralization, the mercury liberated is measured by flameless atomic absorption. 3. REAGENTS\nAll the reagents should be of analytical purity. 3. 1. Concentrated nitric acid, d4\n20 = 1,41 g/ml. 3. 2. Concentrated sulphuric acid, d4\n20 = 1,84 g/ml. 3. 3. Redistilled water. 3. 4. Potassium permanganate, 7 % (m/v) solution. 3. 5. Hydroxylammonium chloride, 1,5 % (m/v) solution. 3. 6. Dipotassium peroxodisulphate, 5 % (m/v) solution. 3. 7. Tin dichloride, 10 % (m/v) solution. 3. 8. Concentrated hydrochloric acid, d4\n20 = 1,18 g/ml. 3. 9. Palladium dichloride impregnated glass wool, 1 % (m/m). 4. APPARATUS\n\n\n\n\n\n\n\n\n4. 1. Normal laboratory equipment. 4. 2. Apparatus for flameless atomic absorption mercury determination (cold vapour technique), including the necessary glassware. Path length of the cell at least 100 mm. 5. PROCEDURE\nTake all normal precautions for trace mercury analysis. 5. 1. Breakdown\n\n\n\n\n\n\n\n\n\n\n5. 1. 1. Weigh accurately 150 mg of the sample (m). Add 10 ml of nitric acid (3. 1) and leave to digest for three hours in an airtight flask in a water bath at 55 oC, shaking at regular intervals. At the same time, carry out a blank test on the reagents. 5. 1. 2. After cooling, add 10 ml of sulphuric acid (3. 2) and return to the water bath at 55 oC for 30 minutes. 5. 1. 3. Place the flask in an ice bath and add carefully 20 ml of water (3. 3). 5. 1. 4. Adding 2 ml aliquots of 7 % potassium permanganate solution (3. 4) until the solution remains coloured. Return to the water bath at 55 oC for a further 15 minutes. 5. 1. 5. Add 4 ml of dipotassium peroxodisulphate solution (3. 6). Continue to warm in the water bath at 55 oC for 30 minutes. 5. 1. 6. Allow to cool and transfer the contents of the flask into a 100 ml standard flask. Rinse the flask with 5 ml of hydroxylammonium chloride (3. 5) and then rinse four times with 10 ml of water (3. 3). The solution should be completely decolorized. Make up to the mark with water (3. 3). 5. 2. Determination\n\n\n\n\n\n\n\n\n\n\n5. 2. 1. Place 10 ml of the test solution (5. 1. 6) in the glass vessel for the cold vapour mercury determination (4. 2). Dilute with 100 ml of water (3. 3) and subsequently 5 ml of sulphuric acid (3. 2) and 5 ml of tin dichloride solution (3. 7). Mix after each addition. Wait 30 seconds to reduce all ionic mercury to the metallic state and take a reading (n). 5. 2. 2. Place some palladium dichloride impregnated glass wool (3. 9) between the mercury reduction vessel and the flow cell of the instrument (4. 2). Repeat 5. 2. 1 and record the reading. If the reading is not zero mineralization was incomplete and analysis must be repeated. 6. CALCULATION\nLet:\n\n\n\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in milligrams) of the test sample. n\n\n\n=\n\n\nthe quantity of mercury (in \u03bcg) read on the instrument. The quantity of mercury, expressed as mercury, as percentage by mass, is calculated by the formula:\n\n\n\n7. NOTES\n\n\n\n\n\n\n\n\n7. 1. To improve mineralization it might be necessary to start by diluting the sample. 7. 2. If absorption of the mercury by the substrate is suspected, a quantitative determination by the method of standard additions should be done. 8. REPEATIBILITY\u00a0(13)\n\nIn the case of mercury concentrations of 0,007 %, the difference between the results of two determinations carried out in parallel on the sample should not exceed an absolute value of 0,00035 %. DETERMINATION OF ALKALI AND ALKALINE EARTH SULPHIDES\n\n1. SCOPE AND FIELD OF APPLICATION\nThis method describes the determination of sulphides present in cosmetic products. The presence of thiols or other reducing agents (including sulphites) does not interfere. 2. DEFINITION\nThe concentration of sulphides determined by this method is expressed as a percentage of sulphur by mass. 3. PRINCIPLE\nAfter acidification of the medium, hydrogen sulphide is entrained by a stream of nitrogen and then fixed in the form of cadmium sulphide. The latter is filtered and rinsed and then determined by iodometry. 4. REAGENTS\nAll reagents should be of analytical purity. 4. 1. Concentrated hydrochloric acid, d4\n20 = 1,19 g/ml. 4. 2. Sodium thiosulphate, 0,1 M standard solution. 4. 3. Iodine, 0,05 M standard solution. 4. 4. Disodium sulphide. 4. 5. Cadmium di(acetate). 4. 6. Concentrated ammonia, d4>20 = 0,90 g/ml. 4. 7. Ammoniacal solution of cadmium di(acetate): dissolve 10 g of cadmium di(acetate) (4. 5) in approximately 50 ml of water. Add ammonia (4. 6) until the precipitate redissolves (i. e. approximately 20 ml). Make up to the 100 ml mark with water. 4. 8. Nitrogen. 4. 9. Solution of ammonia M. 5. APPARATUS\n\n\n\n\n\n\n\n\n5. 1. Usual laboratory equipment. 5. 2. 100 ml round-bottom flask with three standard ground-glass necks. 5. 3. Two 150 ml conical flasks with ground-glass necks, fitted with a device comprising a dip tube and a side outlet tube for releasing the entraining gas. 5. 4. One long-stem tunnel. 6. PROCEDURE\n6. 1. Entrainment of the sulphides\n\n\n\n\n\n\n\n\n6. 1. 1. Take a package which has not been previously opened. Weigh accurately a mass (m) (expressed in grams) of the product corresponding to not more than 30 mg of sulphide ions in the round-bottom flask (5. 2). Add 60 ml of water and two drops of an anti-foaming liquid. 6. 1. 2. Transfer 50 ml of solution (4. 7) to each of the two conical flasks (5. 3). 6. 1. 3. Fit a dropping funnel, the dip tube and the outlet tube on to the round-bottom flask (5. 2). Connect the outlet tube to the conical flasks (5. 3) set up in series by means of PVC tubing. NB: The entraining apparatus must pass the following leak-tightness test: simulating the test conditions, replace the product to be determined by 10 ml of a sulphide solution (prepared from 4. 4) containing \u2018X mg\u2019 of sulphide (iodometrically determined). Let \u2018Y\u2019 be the number of milligrams of sulphide found at the end of this operation. The difference between quantity \u2018X\u2019 and quantity \u2018Y\u2019 must not exceed 3 %. 6. 1. 4. Pass nitrogen (4. 8) through for 15 minutes, at a rate of two bubbles per second, in order to expel the air contained in the round-bottom flask (5. 2). 6. 1. 5. Heat the round-bottom flask to 85 \u00b1 5 oC. 6. 1. 6. Stop the nitrogen (4. 8) stream and add 40 ml of hydrochloric acid (4. 1) drop by drop. 6. 1. 7. Turn the nitrogen (4. 8) stream on again when nearly all the acid has been transferred, leaving a minimum liquid seal to prevent leakage of hydrogen sulphide. 6. 1. 8. Cease heating after 30 minutes. Allow the flask (5. 2) to cool and continue to pass the nitrogen (4. 8) stream through for at least one-and-a-half hours. 6. 2. Titration\n\n\n\n\n\n\n\n\n6. 2. 1. Filter the cadmium sulphide through a long-stem funnel (5. 4). 6. 2. 2. Rinse the conical flasks (5. 3) first with the ammonia solution (4. 9) and pour on the filter. Then rinse with distilled water and use the water to wash the precipitate retained by the filter. 6. 2. 3. Complete the washing of the precipitate with 100 ml of water. 6. 2. 4. Place the paper filter in the first conical flask that contained the precipitate. Add 25 ml (n1) of the iodine solution (4. 3), approximately 20 ml of hydrochloric acid (4. 1) and 50 ml of distilled water. 6. 2. 5. Determine the excess iodine using the sodium thiosulphate solution (n2) (4. 2). 7. CALCULATON\nThe sulphide content of the sample, expressed as sulphur, as percentage by mass, is calculated by the following formula:\n\n\n\nwhere:\n\n\n\n\n\n\n\nn1\n\n\n\n=\n\n\nthe number (in millilitres) of iodine standard solution (4. 3) used,\n\n\n\n\nx1\n\n\n\n=\n\n\nthe molarity of this solution,\n\n\n\n\nn2\n\n\n\n=\n\n\nthe number (in millilitres) of the sodium thiosulphate standard solution (4. 2),\n\n\n\n\nx2\n\n\n\n=\n\n\nthe molarity of this solution,\n\n\n\n\nm\n\n\n=\n\n\nthe mass (in grams) of the test sample. 8. REPEATABILITY\u00a0(14)\n\nFor a sulphide content of about 2 % (m/m), the difference between the results of two determinations carried out in parallel on the same sample should not exceed an absolute value of 0,2 % (m/m). (1)\u00a0\u00a0OJ No L 383, 31. 12. 1980, p. 27. (2)\u00a0\u00a0Norm ISO 5725. (3)\u00a0\u00a0Norm ISO 5725. (4)\u00a0\u00a0Norm ISO 5725. (5)\u00a0\u00a0OJ No L383, 31. 12. 1980, p. 27. (6)\u00a0\u00a0Norm ISO 5725. (7)\u00a0\u00a0Norm ISO 5725. (8)\u00a0\u00a0Because of the wide range of product types in which hexachlorophene could be present, it is important to first check recovery of hexachlorophene from the sample by this procedure before recording results. If recoveries are low, modifications, such as change of solvent (benzene instead of ethyl acetate) etc. , could be introduced with agreement of the parties concerned. (9)\u00a0\u00a0The persistence of this yellow coloration indicates an excess of diazomethane, which is necessary to ensure a complete methylation of the sample. (10)\u00a0\u00a0Norm ISO 5725. (11)\u00a0\u00a0Norm ISO 5725. (12)\u00a0\u00a0Norm ISO 5725. (13)\u00a0\u00a0Norm ISO 5725. (14)\u00a0\u00a0Norm ISO 5725"}
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/f4c92f2e-2945-4a94-b5dc-946ac04bb500", "title": "QUESTION NO 53 BY MR GAUTHIER (H-225/83) TO THE COMMISSION: EEC' S NUCLEAR PROGRAMME", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,GAUTHIER", "date": "1983-09-14", "subjects": "EU Member State,European Community,France,communications policy,energy policy,energy supply,nuclear energy,nuclear reactor,public safety,research programme", "workIds": "celex:91983H000225", "eurovoc_concepts": ["EU Member State", "European Community", "France", "communications policy", "energy policy", "energy supply", "nuclear energy", "nuclear reactor", "public safety", "research programme"], "url": "http://publications.europa.eu/resource/cellar/f4c92f2e-2945-4a94-b5dc-946ac04bb500", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/757c3498-6703-49d0-bc0c-d74140819a9b", "title": "QUESTION NO 67 BY MR CLINTON (H-246/83) TO THE COMMISSION: LIBERALISATION OF INTRA-COMMUNITY TRADE IN MINCED MEAT PRODUCTS", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "CLINTON,European Parliament", "date": "1983-09-14", "subjects": "Ireland,foodstuff,free movement of goods,health control,meat,power of decision,proposal (EU),trade policy,trading operation", "workIds": "celex:91983H000246", "eurovoc_concepts": ["Ireland", "foodstuff", "free movement of goods", "health control", "meat", "power of decision", "proposal (EU)", "trade policy", "trading operation"], "url": "http://publications.europa.eu/resource/cellar/757c3498-6703-49d0-bc0c-d74140819a9b", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/f5898f68-716d-4241-aabc-f7a3ab1cbb1b", "title": "QUESTION NO 55 BY MR WELSH (H-233/83) TO THE COMMISSION: NATIONAL ASSISTANCE LEADING TO AN INCREASE IN NYLON MANUFACTURING CAPACITY IN BELGIUM", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,WELSH", "date": "1983-09-14", "subjects": "Belgium,France,Ireland,Netherlands,State aid,United Kingdom,competition,man-made fibre,private sector,textile industry", "workIds": "celex:91983H000233", "eurovoc_concepts": ["Belgium", "France", "Ireland", "Netherlands", "State aid", "United Kingdom", "competition", "man-made fibre", "private sector", "textile industry"], "url": "http://publications.europa.eu/resource/cellar/f5898f68-716d-4241-aabc-f7a3ab1cbb1b", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/d5c97369-f7ef-4534-aa33-e4349970c531", "title": "QUESTION NO 52 BY MR BORD (H-212/83) TO THE COMMISSION: LACK OF QUALIFIED ENGINEERS IN THE ELECTRONICS INDUSTRY", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "BORD,European Parliament", "date": "1983-09-14", "subjects": "EU employment policy,European Social Fund,Japan,United States,computer,computer systems,electronics industry,engineer,exchange of information,industrial policy,information policy,labour mobility,professional qualifications,scientific education,small and medium-sized enterprises,social policy,technology,unemployment,vocational training,young person", "workIds": "celex:91983H000212", "eurovoc_concepts": ["EU employment policy", "European Social Fund", "Japan", "United States", "computer", "computer systems", "electronics industry", "engineer", "exchange of information", "industrial policy", "information policy", "labour mobility", "professional qualifications", "scientific education", "small and medium-sized enterprises", "social policy", "technology", "unemployment", "vocational training", "young person"], "url": "http://publications.europa.eu/resource/cellar/d5c97369-f7ef-4534-aa33-e4349970c531", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/43b874f0-c82c-4a78-abe6-3b073b8f3d0d", "title": "WRITTEN QUESTION NO 1030/83 BY MR PAUL SCHNITKER TO THE COMMISSION: INTRODUCTION OF A EUROPEAN VOCATIONAL TRAINING PASS", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_written,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,SCHNITKER", "date": "1983-09-14", "subjects": "diploma,education policy,free movement of workers,passport,professional qualifications,recognition of diplomas,unemployment,vocational training,young person", "workIds": "celex:91983E001030", "eurovoc_concepts": ["diploma", "education policy", "free movement of workers", "passport", "professional qualifications", "recognition of diplomas", "unemployment", "vocational training", "young person"], "url": "http://publications.europa.eu/resource/cellar/43b874f0-c82c-4a78-abe6-3b073b8f3d0d", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/b6900dfe-b65a-4dcf-b61a-4caf78ca6f20", "title": "QUESTION NO 61 BY MR GEROKOSTOPOULOS (H-279/83) TO THE COMMISSION: INCOMPLETE REPORTING TO GREEK PUBLIC OPINION OF THE RESULTS OF THE COUNTRY' S MEMBERSHIP OF THE EEC", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,GEROKOSTOPOULOS", "date": "1983-09-14", "subjects": "Denmark,EU aid,European Community,European Parliament,Greece,accession to the European Union,broadcasting,budget policy,financial aid,freedom of expression,information,information policy,press,public opinion,television", "workIds": "celex:91983H000279", "eurovoc_concepts": ["Denmark", "EU aid", "European Community", "European Parliament", "Greece", "accession to the European Union", "broadcasting", "budget policy", "financial aid", "freedom of expression", "information", "information policy", "press", "public opinion", "television"], "url": "http://publications.europa.eu/resource/cellar/b6900dfe-b65a-4dcf-b61a-4caf78ca6f20", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/c6cb72e0-76f8-4b50-916c-77dde18c65d4", "title": "WRITTEN QUESTION NO 1016/83 BY MR DIETER ROGALLA TO THE COMMISSION: ARTICLE 235 OF THE EEC TREATY", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_written,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,ROGALLA", "date": "1983-09-14", "subjects": "Council of the European Union,EEC Treaty,European Commission,consumer protection,environmental protection,frontier,parliamentary question,proposal (EU),resolution,social policy,supervisory power", "workIds": "celex:91983E001016", "eurovoc_concepts": ["Council of the European Union", "EEC Treaty", "European Commission", "consumer protection", "environmental protection", "frontier", "parliamentary question", "proposal (EU)", "resolution", "social policy", "supervisory power"], "url": "http://publications.europa.eu/resource/cellar/c6cb72e0-76f8-4b50-916c-77dde18c65d4", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/7eda1eda-2fef-4ef5-b169-e3ff2ec2ace8", "title": "QUESTION NO 35 BY MRS HAMMERICH (H-184/83) TO THE FOREIGN MINISTERS OF THE TEN MEMBER STATES OF THE EUROPEAN COMMUNITIES MEETING IN POLITICAL COOPERATION: ECONOMIC ASPECTS OF SECURITY POLICY", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,HAMMERICH", "date": "1983-09-13", "subjects": "EU competence,Ireland,Israel,NATO,armed forces,disarmament,foreign policy,military equipment,neutrality,non-proliferation of arms,nuclear weapon,political cooperation,public safety,public statement,sale", "workIds": "celex:91983H000184", "eurovoc_concepts": ["EU competence", "Ireland", "Israel", "NATO", "armed forces", "disarmament", "foreign policy", "military equipment", "neutrality", "non-proliferation of arms", "nuclear weapon", "political cooperation", "public safety", "public statement", "sale"], "url": "http://publications.europa.eu/resource/cellar/7eda1eda-2fef-4ef5-b169-e3ff2ec2ace8", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/76cbc47b-5d22-44d5-80ed-4bfaecac9376", "title": "QUESTION NO 1 BY MR MARSHALL (H-837/82) TO THE COUNCIL: FULL DIPLOMATIC RECOGNITION OF ISRAEL BY GREECE", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,MARSHALL", "date": "1983-09-13", "subjects": "Greece,Israel,Middle East,association agreement,diplomatic relations,foreign policy", "workIds": "celex:91982H000837", "eurovoc_concepts": ["Greece", "Israel", "Middle East", "association agreement", "diplomatic relations", "foreign policy"], "url": "http://publications.europa.eu/resource/cellar/76cbc47b-5d22-44d5-80ed-4bfaecac9376", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/15b36e11-41a6-43fa-9dcf-f78f0c292c28", "title": "QUESTION NO 4 BY MR MORELAND (H-86/83) TO THE COUNCIL: DRAFT DIRECTIVE OF LORRY WEIGHTS AND DIMENSIONS", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,MORELAND", "date": "1983-09-13", "subjects": "Ireland,United Kingdom,approximation of laws,commercial vehicle,derogation from EU law,directive,road transport,transport policy,weights and measures", "workIds": "celex:91983H000086", "eurovoc_concepts": ["Ireland", "United Kingdom", "approximation of laws", "commercial vehicle", "derogation from EU law", "directive", "road transport", "transport policy", "weights and measures"], "url": "http://publications.europa.eu/resource/cellar/15b36e11-41a6-43fa-9dcf-f78f0c292c28", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/e8bbf516-fc2f-4b7b-aaa2-28fe2d77ca3b", "title": "QUESTION NO 2 BY MR GERONIMI (H-328/83) TO THE COUNCIL: RECOGNITION OF THE STATE OF ISRAEL BY GREECE", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,GERONIMI", "date": "1983-09-13", "subjects": "Greece,Israel,Middle East,association agreement,diplomatic relations,foreign policy", "workIds": "celex:91983H000328", "eurovoc_concepts": ["Greece", "Israel", "Middle East", "association agreement", "diplomatic relations", "foreign policy"], "url": "http://publications.europa.eu/resource/cellar/e8bbf516-fc2f-4b7b-aaa2-28fe2d77ca3b", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/66a29e06-dc78-4f6f-8c5f-fdc8a0993aa0", "title": "QUESTION NO 6 BY MR ROGALLA (H-127/83) TO THE COUNCIL: CHECKS AT INTERNAL FRONTIERS", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "European Parliament,ROGALLA", "date": "1983-09-13", "subjects": "free movement of persons,frontier,intra-EU transport,proposal (EU),supervisory power", "workIds": "celex:91983H000227", "eurovoc_concepts": ["free movement of persons", "frontier", "intra-EU transport", "proposal (EU)", "supervisory power"], "url": "http://publications.europa.eu/resource/cellar/66a29e06-dc78-4f6f-8c5f-fdc8a0993aa0", "lang": "eng", "formats": ["print"]}
+{"cellarURIs": "http://publications.europa.eu/resource/cellar/01d17ee3-010d-4a10-b9c6-2764d252918d", "title": "Agreement for cooperation in dealing with pollution of the North Sea by oil and other harmful substances (Bonn Agreement)", "langIdentifier": "ENG", "mtypes": "fmx4,html,pdfa1b,print,xhtml", "workTypes": "http://publications.europa.eu/ontology/cdm#agreement_international,http://publications.europa.eu/ontology/cdm#agreement_non-member-states,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "Belgium,Denmark,European Economic Community,France,Germany,Netherlands,Norway,Sweden,United Kingdom", "date": "1983-09-13", "subjects": "North Sea,cooperation agreement (EU),environmental cooperation,marine pollution,multilateral agreement,oil pollution,toxic substance", "workIds": "celex:21984A0716(02),oj:JOL_1984_188_R_0009_01", "eurovoc_concepts": ["North Sea", "cooperation agreement (EU)", "environmental cooperation", "marine pollution", "multilateral agreement", "oil pollution", "toxic substance"], "url": "http://publications.europa.eu/resource/cellar/01d17ee3-010d-4a10-b9c6-2764d252918d", "lang": "eng", "formats": ["fmx4", "html", "pdfa1b", "print", "xhtml"], "text": "L_1984188EN. 01000901. xml\n\n\n\n\n\n\n\n\n\n\n16. 7. 1984\u00a0\u00a0\u00a0\n\n\nEN\n\n\nOfficial Journal of the European Communities\n\n\nL 188/9\n\n\n\n\n\nAGREEMENT\nfor cooperation in dealing with pollution of the North Sea by oil and other harmful substances\n(Bonn Agreement)\nTHE GOVERNMENTS OF THE KINGDOM OF BELGIUM, THE KINGDOM OF DENMARK, THE FRENCH REPUBLIC, THE FEDERAL REPUBLIC OF GERMANY, THE KINGDOM OF THE NETHERLANDS, THE KINGDOM OF NORWAY, THE KINGDOM OF SWEDEN, THE UNITED KINGDOM OF GREAT BRITAIN AND NORTHERN IRELAND AND THE EUROPEAN ECONOMIC COMMUNITY,\nRECOGNIZING that pollution of the sea by oil and other harmful substances in the North Sea area may threaten the marine environment and the interests of coastal States,\nNOTING that such pollution has many sources and that casualties and other incidents at sea are of great concern,\nCONVINCED that an ability to combat such pollution as well as active cooperation and mutual assistance among States are necessary for the protection of their coasts and related interests,\nWELCOMING the progress that has already been achieved within the framework of the Agreement for cooperation in dealing with pollution of the North Sea by oil, signed at Bonn on 9 June 1969,\nWISHING to develop further mutual assistance and cooperation in combating pollution,\nHAVE AGREED AS FOLLOWS:\nArticle 1\nThis Agreement shall apply whenever the presence or the prospective presence of oil or other harmful substances polluting or threatening to pollute the sea within the North Sea area, as defined in Article 2 of this Agreement, presents a grave and imminent danger to the coast or related interests of one or more Contracting Parties. Article 2\nFor the purpose of this Agreement the North Sea area means the North Sea proper southwards of latitude 61oN, together with:\n\n\n\n\n\n\n(a)\n\n\nthe Skagerrak, the southern limit of which is determined east of the Skaw by the latitude 57o44'00'',8N;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nthe English Channel and its approaches eastwards of a line drawn SO nautical miles to the west of a line joining the Scilly Isles and Ushant. Article 3\n1. The Contracting Parties consider that protection against pollution of the kind referred to in Article 1 of this Agreement is a matter which calls for active cooperation between them. 2. The Contracting Parties shall jointly develop and establish guidelines for the practical, operational and technical aspects of joint action. Article 4\nContracting Parties undertake to inform the other Contracting Parties about:\n\n\n\n\n\n\n(a)\n\n\ntheir national organization for dealing with pollution of the kind referred to in Article 1 of this Agreement;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nthe competent authority responsible for receiving and dispatching reports of such pollution and for dealing with questions concerning measures of mutual assistance between Contracting Parties:\n\n\n\n\n\n\n\n\n\n\n(c)\n\n\ntheir national means for avoiding or dealing with such pollution, which might be made available for international assistance;\n\n\n\n\n\n\n\n\n\n\n(d)\n\n\nnew ways in which such pollution may be avoided and about new effective measures to deal with it;\n\n\n\n\n\n\n\n\n\n\n(e)\n\n\nmajor pollution incidents of this kind dealt with. Article 5\n1. Whenever a Contracting Party is aware of a casualty or the presence of oil or other harmful substances in the North Sea area likely to constitute a serious threat to the coast or related interests of any other Contracting Party, it shall inform that Party without delay through its competent authority. 2. The Contracting Parties undertake to request the masters of all ships flying their flags and pilots of aircraft registered in their countries to report without delay through the channels which may be most practicable and adequate in the circumstances:\n\n\n\n\n\n\n(a)\n\n\nall casualties causing or likely to cause pollution of the sea;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nthe presence, nature and extent of oil or other harmful substances likely to constitute a serious threat to the coast or relating interests of one or more Contracting Parties. 3. The Contracting Parties shall establish a standard form for the reporting of pollution as required under paragraph 1 of this Article. Article 6\n1. For the sole purpose of this Agreement the North Sea area is divided into the zones described in the Annex to this Agreement. 2. The Contracting Party within whose zone a situation of the kind described in Article 1 of this Agreement occurs, shall make the necessary assessments of the nature and extent of any casualty or, as the case may be, of the type and approximate quantity of oil or other harmful substances and the direction and speed of movement thereof. 3. The Contracting Party concerned shall immediately inform all the other Contracting Parties through their competent authorities of its assessments and of any action which it has taken to deal with the oil or other harmful substances and shall keep these substances under observation as long as they are present in its zone. 4. The obligations of the Contracting Parties under the provisions of this Article with respect to the zones of joint responsibility shall be the subject of special technical arrangements to be concluded between the Parties concerned. These arrangements shall be communicated to the other Contracting Parties. Article 7\nA Contracting Party requiring assistance to deal with pollution or the prospective presence of pollution at sea or on its coast may call on the help of the other Contracting Parties. Contracting Parties requesting assistance shall specify the kind of assistance they require. The Contracting Parties called upon for help in accordance with this Article shall use their best endeavours to bring such assistance as is within their power taking into account, particularly in the case of pollution by harmful substances other than oil, the technological means available to them. Article 8\n1. The provisions of this Agreement shall not be interpreted as in any way prejudicing the rights and obligations of the Contracting Parties under international law, especially in the field of the prevention and combating of marine pollution. 2. In no case shall the division into zones referred to in Article 6 of this Agreement be invoked as a precedent or argument in any matter concerning sovereignty or jurisdiction. Article 9\n1. In the absence of an agreement concerning the financial arrangements governing actions of Contracting Parties to deal with pollution which might be concluded on a bilateral or multilateral basis or on the occasion of a joint combating operation, Contracting Parties shall bear the costs of their respective actions in dealing with pollution in accordance with subparagraphs (a) or (b) below:\n\n\n\n\n\n\n(a)\n\n\nif the action was taken by one Contracting Party at the express request of another Contracting Party, the Contracting Party requesting such assistance shall reimburse to the assisting Contracting Party the costs of its action;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nif the action was taken by a Contracting Party on its own initiative, this Contracting Party shall bear the costs of its action. 2. The Contracting Party requesting assistance may cancel its request at any time, but in that case it shall bear the costs already incurred or committed by the assisting Contracting Party. Article 10\nUnless otherwise agreed the costs of action taken by a Contracting Party at the request of another Contracting Party shall be calculated according to the law and current practice in the assisting country concerning the reimbursement of such costs by a person or entity liable. Article 11\nArticle 9 of this Agreement shall not be interpreted as in any way prejudicing the rights of Contracting Parties to recover from third parties the costs of action to deal with pollution or the threat of pollution under other applicable provisions and rules of national and international law. Article 12\n1. Meetings of the Contracting Parties shall be held at regular intervals and at any time when, due to special circumstances, it is so decided in accordance with the Rules of Procedure. 2. The Contracting Parties at their first meeting shall draw up Rules of Procedure and Financial Rules, which shall be adopted by unanimous vote. 3. The Depositary Government shall convene the first meeting of Contracting Parties as soon as possible after the entry into force of this Agreement. Article 13\nWithin the areas of its competence, the European Economic Community is entitled to a number of votes equal to the number of its Member States which are Contracting Parties to the present Agreement. The European Economic Community shall not exercise its right to vote in cases where its Member States exercise theirs and conversely. Article 14\nIt shall be the duty of meetings of the Contracting Parties:\n\n\n\n\n\n\n(a)\n\n\nto exercise overall supervision over the implementation of this Agreement;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nto review the effectiveness of the measures taken under this Agreement;\n\n\n\n\n\n\n\n\n\n\n(c)\n\n\nto carry out such other functions as may be necessary under the terms of this Agreement. Article 15\n1. The Contracting Parties shall make provision for the performance of secretariat duties in relation to this Agreement, taking into account existing arrangements in the framework of other international agreements on the prevention of marine pollution in force for the same region as this Agreement. 2. Each Contracting Party shall contribute 2,5% towards the annual expenditure of the Agreement. The ballance of the Agreement's expenditure shall be divided among Contracting Parties other than the European Economic Community in proportion to their gross national product in accordance with the scale of assessment adopted regularly by the United Nations General Assembly. In no case shall the contribution of a Contracting Party to this balance exceed 20 % of the balance. Article 16\n1. Without prejudice to Article 17 of this Agreement, a proposal by a Contracting Party for the amendment of this Agreement or its Annex shall be considered at a meeting of the Contracting Parties. Following adoption of the proposal by unanimous vote the amendment shall be communicated by the Depositary Government to the Contracting Parties. 2. Such an amendment shall enter into force on the first day of the second month following the date on which the Depositary Government has received notifications of approval from all Contracting Parties. Article 17\n1. Two or more Contracting Parties may modify the common boundaries of their zones described in the Annex to this Agreement. 2. Such a modification shall enter into force for all Contracting Parties on the first day of the sixth month following the date of its communication by the Depositary Government unless, within a period of three months following that communication, a Contracting Party has expressed an objection or has requested consultation on the matter. Article 18\n1. This Agreement shall be open for signature by the Governments of the States invited to participate in the Conference on the Agreement for cooperation in dealing with pollution of the North Sea by oil and other harmful substances, held at Bonn on 13 September 1983, and by the European Economic Community. 2. These States and the European Economic Community may become Parties to this Agreement either by signature without reservation as to ratification, acceptance or approval or by signature subject to ratification, acceptance or approval followed by ratification, acceptance or approval. 3. Instruments of ratification, acceptance or approval shall be deposited with the Government of the Federal Republic of Germany. Article 19\n1. This Agreement shall enter into force on the frist day of the second month following the date on which the Governments of all the States mentioned in Article 18 of this Agreement and the European Economic Community have signed the Agreement without reservation as to ratification, acceptance or approval. 2. Upon the entry into force of this Agreement the Agreement for cooperation in dealing with pollution of the North Sea by oil, done at Bonn on 9 June 1969, shall cease to be in force. Article 20\n1. The Contracting Parties may unanimously invite any other coastal State of the north-east Atlantic area to accede to this Agreement. 2. In such a case Article 2 of this Agreement and its Annex shall be amended as necessary. The amendments shall be adopted by unanimous vote at a meeting of the Contracting Parties and shall take effect upon the entry into force of this Agreement for the acceding State. Article 21\n1. For each State acceding to this Agreement, the Agreement shall enter into force on the first day of the second month following the date of deposit by such State of its instrument of accession. 2. Instruments of accession shall be deposited with the Government of the Federal Republic of Germany. Article 22\n1. After this Agreement has been in force for five years it may be denounced by any Contracting Party. 2. Denunciation shall be effected by a notification in writing addressed to the Depositary Government which shall notify all the other Contracting Parties of any denunciation received and of the date of its receipt. 3. A denunciation shall take effect one year after its receipt by the Depositary Government. Article 23\nThe Depositary Government shall inform the Contracting Parties and those referred to in Article 18 of this Agreement of:\n\n\n\n\n\n\n(a)\n\n\nany signature of this Agreement;\n\n\n\n\n\n\n\n\n\n\n(b)\n\n\nthe deposit of any instrument of ratification, acceptance, approval or accession and of the receipt of any notice of denunciation;\n\n\n\n\n\n\n\n\n\n\n(c)\n\n\nthe date of entry into force of this Agreement;\n\n\n\n\n\n\n\n\n\n\n(d)\n\n\nthe receipt of any notification of approval relating to amendments to this Agreement or its Annex and of the date of entry into force of such amendments. Article 24\nThe original of this Agreement, of which the English, French and German texts are equally authentic, shall be deposited with the Government of the Federal Republic of Germany, which shall send certified copies thereof to the Contracting Parties and which shall transmit a certified copy to the Secretary-General of the United Nations for registration and publication in accordance with Article 102 of the Charter of the United Nations. In witness whereof the undersigned, being duly authorized there to by their respective Governments, have signed this Agreement. Done at Bonn, this 13th day of September 1983. F\u00dcR DIE REGIERUNG DES K\u00d6NIGREICHS BELGIEN,\nFOR THE GOVERNMENT OF THE KINGDOM OF BELGIUM,\nPOUR LE GOUVERNEMENT DU ROYAUME DE BELGIQUE:\n\n\nVorbehaltlich der Ratifikation,\nSubject to ratification,\nSous r\u00e9serve de ratification. F\u00dcR DIE REGIERUNG DES K\u00d6NIGREICHS D\u00c4NEMARK,\nFOR THE GOVERNMENT OF THE KINGDOM OF DENMARK,\nPOUR LE GOUVERNEMENT DU ROYAUME DE DANEMARK:\n\n\nVorbehaltlich der Genehmigung,\nSubject to approval,\nSous r\u00e9serve d'approbation. F\u00dcR DIE REGIERUNG DER FRANZ\u00d6SISCHEN REPUBLIK,\nFOR THE GOVERNMENT OF THE FRENCH REPUBLIC,\nPOUR LE GOUVERNEMENT DE LA R\u00c9PUBLIQUE FRANCAISE:\n\n\nF\u00dcR DIE REGIERUNG DER BUNDESREPUBLIK DEUTSCHLAND,\nFOR THE GOVERNMENT OF THE FEDERAL REPUBLIC OF GERMANY,\nPOUR LE GOUVERNEMENT DE LA R\u00c9PUBLIQUE FRAN\u00c7AISE:\n\n\nF\u00dcR DIE REGIERUNG DES K\u00d6NIGREICHS DER NIEDERLANDE,\nFOR THE GOVERNMENT OF THE KINGDOM OF THE NETHERLANDS,\nPOUR LE GOUVERNEMENT DU ROYAUME DES PAYS-BAS:\n\n\nVorbehaltlich der Annahme,\nSubject to acceptance,\nSous r\u00e9serve d'acceptation. F\u00dcR DIE REGIERUNG DES K\u00d6NIGREICHS NORWEGEN,\nFOR THE GOVERNMENT OF THE KINGDOM OF NORWAY,\nPOUR LE GOUVERNEMENT DU ROYAUME DE NORV\u00c8GE:\n\n\nVorbehaltlich der Ratifikation,\nSubject to ratification,\nSous r\u00e9serve de ratification. F\u00dcR DIE REGIERUNG DES K\u00d6NIGREICHS SCHWEDEN,\nFOR THE GOVERNMENT OF THE KINGDOM OF SWEDEN,\nPOUR LE GOUVERNEMENT DU ROYAUME DE SU\u00c8DE:\n\n\nF\u00dcR DIE REGIERUNG DES VEREINIGTEN K\u00d6NIGREICHS GROSSBRITANNIEN UND NORDIRLAND,\nFOR THE GOVERNMENT OF THE UNITED KINGDOM OF GREAT BRITAIN AND NORTHERN IRELAND,\nPOUR LE GOUVERNEMENT DU ROYAUME-UNI DE GRANDE-BRETAGNE ET D'IRLANDE DU NORD:\n\n\nVorbehaltlich der Ratifikation,\nSubject to ratification,\nSous r\u00e9serve de ratification. F\u00dcR DIE EUROP\u00c4ISCHE WIRTSCHAFTSGEMEINSCHAFT\nFOR THE EUROPEAN ECONOMIC COMMUNITY,\nPOUR LA COMMUNAUT\u00c9 \u00c9CONOMIQUE EUROP\u00c9ENNE:\n\n\nVorbehaltlich der Annahme,\nSubject to acceptance,\nSous r\u00e9serve d'acceptation. ANNEX\nDescription of the zones referred to in Article 6 of this Agreement\nThe zones, with the exception of the zones of joint responsibility, are limited by lines joining the following points:\n\nDenmark\n\n\n\n\n\n\n\n55o03'00'',0 N\n\n\n8o22'00'',0 E\n\n\n\n\n55o10'00'',0 N\n\n\n7o30'00'',0 E\n\n\n\n\n55o10'00'',0 N\n\n\n2o13'30'',0 E\n\n\n\n\n57o00'00'',0 N\n\n\nlo30'00'',0 E\n\n\n\n\n57o00'00'',0 N\n\n\n2o25'04'',6 E\n\n\n\n\n56o35'42'',0 N\n\n\n2o36'48'',0 E\n\n\n\n\n56o05'12'',0 N\n\n\n3o15'00'',0 E\n\n\n\n\n56o35'30'',0 N\n\n\n5o02'00'',0 E\n\n\n\n\n57o10'30'',0 N\n\n\n6o56'12'',0 E\n\n\n\n\n57o29'54'',0 N\n\n\n7o59'00'',0 E\n\n\n\n\n57o37'06'',0 N\n\n\n8o27'30'',0 E\n\n\n\n\n57o4l'48'',0 N\n\n\n8o53'18'',0 E\n\n\n\n\n57o59'18'',0 N\n\n\n9o23'00'',0 E\n\n\n\n\n58o15'41'',2 N\n\n\n10o01'48'',1 E\n\n\n\n\n58o10'00'',0 N\n\n\n10o00'00'',0 E\n\n\n\n\n57o48'00'',0 N\n\n\n10o57'00'',0 E\n\n\n\n\n57o44'48'',0 N\n\n\n10o38'00'',0 E\n\n\n\n\n\n\n\nFederal Republic of Germany\n\n\n\n\n\n\n53o34'N\n\n\n6o38'E\n\n\n\n\n54o00'N\n\n\n5o30'E\n\n\n\n\n54o00'N\n\n\n2o 39',1E\n\n\n\n\n55o10'N\n\n\n2o13',5E\n\n\n\n\n55o10'N\n\n\n7o30'E\n\n\n\n\n55o03'N\n\n\n8o22'E\n\n\n\n\n\n\n\n\nNetherlands\n\n\n\n\n\n\n\n51o32'N\n\n\n3o18'E\n\n\n\n\n5lo32'N\n\n\n2o06'E\n\n\n\n\n52o30'N\n\n\n3o10'E\n\n\n\n\n54o00'N\n\n\n2o39',1E\n\n\n\n\n54o00'N\n\n\n5o30'E\n\n\n\n\n53o34'N\n\n\n6o38'E\n\n\n\n\n\n\n\n\nNorway\n\n\n\n\n\n\n\n61o00'00'',0 N\n\n\n4o30'00'',0 E\n\n\n\n\n61o00'00'',0 N\n\n\n2o00'00'',0 E\n\n\n\n\n57o00'00'',0 N\n\n\n1o30'00'',0 E\n\n\n\n\n57o00'00'',0 N\n\n\n2o25'04'',6 E\n\n\n\n\n56o35'42'',0 N\n\n\n2o36'48'',0 E\n\n\n\n\n56o05'12'',0 N\n\n\n3o15'00'',0 E\n\n\n\n\n56o35'30'',0 N\n\n\n5o02'00'',0 E\n\n\n\n\n57o10'30'',0 N\n\n\n6o56'12'',0 E\n\n\n\n\n57o29'54'',0 N\n\n\n7o59'00'',0 E\n\n\n\n\n57o37'06'',0 N\n\n\n8o27'30'',0 E\n\n\n\n\n57o41'48'',0 N\n\n\n8o53'18'',0 E\n\n\n\n\n57o59'18'',0 N\n\n\n9o23'00'',0 E\n\n\n\n\n58o15'41'',2 N\n\n\n10o0l'48'',1 E\n\n\n\n\n58o10'00'',0 N\n\n\n10o00'00'',0 E\n\n\n\n\n58o53'34'',0 N\n\n\n10o38'25'',0 E\n\n\n\n\nTo be continued along the Norwegian-Swedish border\n\n\n\n\n\n\n\n\nSweden\n\n\n\n\n\n\n\n57o54'N\n\n\n11o28'E\n\n\n\n\n57o48'N\n\n\n10o57'E\n\n\n\n\n58o10'N\n\n\n10o00'E\n\n\n\n\n58o53'34'',0 N\n\n\n10o38'25'',0E\n\n\n\n\nTo be continued along the Norwegian-Swedish border\n\n\n\n\n\n\n\n\nUnited Kingdom\n\n\n\n\n\n\n\n61o00'N\n\n\n0o50'0\n\n\n\n\n61o00'N\n\n\n2o00'E\n\n\n\n\n57o00'N\n\n\n1o30'E\n\n\n\n\n52o30'N\n\n\n3o10'E\n\n\n\n\n51o32'N\n\n\n2o06'E\n\n\n\n\nThe zones of joint responsibility are as follows:\n1. Belgium, France and United Kingdom\n\nSea area between parallels 51o32'N and 51o06'N. 2. France and United Kingdom\n\nThe English Channel south-west of parallel 51o06'N to in line drawn between the points 49o52'N 07o44'W and 48o27'N 06o25'W. 3. Denmark and Sweden\n\nSea area between the lines in Skagerrak joining the points:\n\n\n\n\n\n\n57o54'N\n\n\n11o28'E\n\n\n\n\n57o44',8N\n\n\n10o38'E\n\n\n\n\n57o44',8N\n\n\n11o28'E"}
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+{"cellarURIs": "http://publications.europa.eu/resource/cellar/70a5bee5-28a7-4d57-b699-d2afea940d5d", "title": "QUESTION NO 33 BY MR BONDE (H-180/83) TO THE FOREIGN MINISTERS OF THE TEN MEMBER STATES OF THE EUROPEAN COMMUNITIES MEETING IN POLITICAL COOPERATION: THE COMMISSION' S ROLE IN EPC", "langIdentifier": "ENG", "mtypes": "print", "workTypes": "http://publications.europa.eu/ontology/cdm#question_parliamentary,http://publications.europa.eu/ontology/cdm#question_parliamentary_question_time,http://publications.europa.eu/ontology/cdm#resource_legal,http://publications.europa.eu/ontology/cdm#work", "authors": "BONDE,European Parliament", "date": "1983-09-13", "subjects": "Community budget,EU Member State,EU competence,European Commission,foreign policy,political cooperation,public safety,public statement", "workIds": "celex:91983H000180", "eurovoc_concepts": ["Community budget", "EU Member State", "EU competence", "European Commission", "foreign policy", "political cooperation", "public safety", "public statement"], "url": "http://publications.europa.eu/resource/cellar/70a5bee5-28a7-4d57-b699-d2afea940d5d", "lang": "eng", "formats": ["print"]}
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