Amendments To The Cabinet Of Ministers Of 20 April 2004, Regulations No 354 "provisions On Essential Requirements For Cosmetic Products And The Management Agenda"

Original Language Title: Grozījumi Ministru kabineta 2004.gada 20.aprīļa noteikumos Nr.354 "Noteikumi par būtiskajām prasībām kosmētikas līdzekļiem un to uzraudzības kārtību"

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Read the untranslated law here: https://www.vestnesis.lv/ta/id/137098

Cabinet of Ministers Regulations No. 420 Riga 2006 (23 May. No 28 34) amendments to the Cabinet of Ministers of 20 April 2004, regulations No 354 "provisions on essential requirements for cosmetic products and their supervisory order" Issued in accordance with the law "on conformity assessment" article 7, first subparagraph, and the consumer protection law, article 21 of the first part of the draw of the Cabinet of Ministers of 20 April 2004, regulations No 354 "provisions on essential requirements for cosmetic products and their supervisory arrangements" (Latvian journal , 2004, 68, no. 185; 2005, 8, 63, 157, no. 201) the following amendments: 1. Make a point 20 as follows: "20. chemical composition of the product shall be used for the determination of the methods set out in annex 8 of these rules." 2. To supplement the provisions and paragraph 78.79 by the following: "78. From august 22, 2006, banned the placing on the market of cosmetic products whose composition complies with this provision 3 of chapter I of Annex 17 and paragraph 29 and annex 15.267.682, 683, 684,..., 685, 686, 687., 688, 689, 690, 691., 692, 693, 694.., 695, 696, 697, 698.., 699, 700, 701, 702, 703.., 704. , 705, 706, 707.., 708, 709., 710, 711, 712.., 713, 714, 715..., 716, 717, 718.., 719, 720, 721.., 722, 723, 724..., 725, 726, 727..., 728, 729, 730..., 731, 732, 733..., 734, 735, 736.., 737, 738, 739, 740, 741.., 742, 743, 744..., 745, 746, 747, 748..., 749, 750, 751, 752, 753, 754.., 755 and 756. the requirements referred to in paragraph. 79. on 22 November 2006, forbidden to sell or realize the final consumers of cosmetic products which do not comply with this rule 3 of chapter I of Annex 17 and paragraph 29 and annex 15.267.682, 683, 684,..., 685, 686, 687., 688, 689, 690, 691., 692, 693, 694.., 695, 696, 697, 698.., 699, 700, 701, 702, 703.., 704, 705, 706..., 707, 708, 709.., 710, 711.. 712, 713, 714, 715, 716,..., 717, 718, 719., 720, 721, 722., 723, 724, 725.., 726, 727, 728..., 729, 730, 732, 733, 735, 734, 735, 736.., 737, 738, 739, 740, 741.., 742, 743, 744..., 745, 746, 747, 748..., 749, 750, 751, 752, 753, 754.., 755 and 756. the requirements in paragraph. " 3. To supplement the information in reference to European Union directives, paragraph 1 to 45, 46, 47, 48, 49, 50, 51, 52 and 53. subparagraph by the following: "45) Commission 22 December 1980 the first directive 80/1335/EEC on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products; the Commission's 46) 14 May 1982 a second Directive 82/434/EEC on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products; 47) Commission of 27 September 1983 on the third directive 83/514/EEC on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products; 48) Commission 11 October 1985 the Fourth Directive 85/490/EEC on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products; 49) Commission of 9 September 1993, the Fifth Directive 93/73/EEC on the methods of analysis necessary for checking the composition of cosmetic products; 50) Commission on July 7, 1995 in the Sixth Directive 95/32/EC as regards the methods of analysis necessary for checking the composition of cosmetic products; 51) Commission of 2 July 1996, the seventh Directive 96/45/EC relating to methods of analysis necessary for checking the composition of cosmetic products; 52) Commission of 4 April 1990 directive 90/207/EEC, amending the second Directive 82/434/EEC on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products; 53) Commission 21 November 2005 Directive 2005/80/EC, amending Council Directive 76/768/EEC, concerning cosmetic products, for the purpose of adapting Annexes II and III. " 4. Put 3. in chapter I of Annex 17, paragraph 2 and 3 by the following: column ' boric acid, borates and tetraborāt, other than substances referred to in annex 15 to the reference number 729 Boric acid, borat and-with the exception of tetraborat substance in annexe II "From 1184 5. Express 3. paragraph 29 of chapter I in the column 2 and 3 as follows:" p-Phenylenediamine, its nitrogen substituted derivatives and its salts; nitrogen-substituted derivatives of o-Phenylenediamine (5), except for derivatives listed elsewhere in this annex p-Phenylenediamin, N-substituted it for counterparties and it is cold; N-substituted for counterparties of o-Phenylenediamin (4), with the exception of those counterparties listed in this Annex "elsewher 6. Deletion of annex 3, chapter 31. 7. Replace annex 4, paragraph 3, the words "cannot come" with the words "not for going into." 8. Express 6. paragraph 23 of annex 3 of the box the following: "Titanium dioxid." 9. Express 6. paragraph 27 of the annex to the column 2 and 3 by the following: "benzoic acid, 2-[4-(diethylamino)-2-hydroxybenzoyl] hexylester (INCI name: Hydroxybenzoyl Hexyl-Diethylamin CAS no 302776-Benzoat 68-7) Benzoic acid, 2-{4-(diethylamin)-2-hydroxybenzoyl]-, hexylester (INCI name: Hydroxybenzoyl Hexyl Benzoat Diethylamin the case Of 302776-68-7)" 10. Express new version of Annex 8 (annex). 11. Deletion of annex 15 and paragraph 142.143. 12. Express 15.267. Annex paragraph by the following: "267.687. Dinitrotoluene, technical (CAS No 121-14-2) Dinitrotoluen, technical grade (CAS No 121-14-2)" 13. Supplement 15.682, 683 annex., 684, 685, 686.., 687, 688, 689.., 690, 691, 692., 693, 694, 695, 696, 697, 698.699.,., 700, 701, 702., 703, 704, 705, 706..., 707, 708, 709.., 710, 711, 712.., 713, 714, 715..., 716, 717. , 718, 719, 720.., 721, 722, 723.., 724, 725, 726..., 727, 728, 729..., 730, 731, 732., 733, 734, 735, 736.., 737, 738, 739, 740, 741.., 742, 743, 744..., 745, 746, 747, 748..., 749, 750, 751, 752, 753, 754.., 755 and 756 points. the following wording: "682.

1137. Izobutilnitrīt (CAS no 542-56-3) Isobutyl nitrit (CAS No 542-56-3) 683.

1138. Isoprene (stabilized) (2-methyl-1.3-butadiene) (CAS No. 78-79-5) Isopren (stabilized) (2-methyl-1.3-butadien) (CAS No 78-79-5) 684.

1139.1-bromopropane; n-propilbromīd (CAS No 106-94-5) 1-n-propyl bromopropan "(CAS No106-94-5) 685.

1140. Chloroprene (stabilized) (2-chloro-1.3-butadiene) (CAS No 126-99-8) Chloropren (stabilized) (2-chlor-1.3-butadien) (CAS No126-99-8) 686.

1141.1, 2, 3-Trichloropropane (CAS No 96-18-4), 1, 2, 3-trichloropropan (CAS No 96-18-4) 687.

1142. Etilēnglikoldimetilēter (EGHI) (CAS No 110-71-4) Ethylen glycol dimethyl ether of (EGHI) (CAS No 110-71-4) 688.

1143. Dinocap (ISO) (CAS no 39300-45-3) Dinocap (ISO) (CAS No 39300-45-3) 689.

1144. Diaminotoluol, technical-blend, consisting of [4-methyl-m-Phenylenediamine] (1) and [2-methyl-m-Phenylenediamine] (2) metilfenilēndiamīn (CAS no 25376-45-8) Diaminotoluen, technical product-mixtur of [4-methyl-m-phenylenediamin] (1) and [2-methyl-m-phenylen-diamin] (2) methyl-phenylenediamin (CAS No 25376-45-8) 690.

1145. p-hlorbenzotrihlorīd (CAS no 5216-25-1) p-chlorobenzotrichlorid (CAS No 5216-25-1) 691.

1146. Diphenylether; oktabrom derivative (CAS No. 32536-52-0) Diphenylether; the derivat octabrom (CAS No 32536-52-0) 692.

1147.1.2-bis (2-2) ethane, trietilēnglikoldimetilēter (TEGDM) (CAS No. 112-49-2), 1.2-bis (2-Methoxyethoxy) triethylen glycol dimethyl ether of the ethan (TEGDM) (CAS No 112-49-2) 693.

1148. Tetrahidrotiopirān-3-karbaldehīd (CAS no 61571-06-0) Tetrahydrothiopyran-3-carboxaldehyd (CAS No 61571-06-0) 694.

1149.4, 4 '-bis (dimethylamino) Benzophenone (Mihler-ketone) (CAS No 90-94-8), 4, 4 '-bis (dimethylamin) benzophenon (Michler's ketone) (CAS No 90-94-8) 695.

oxiranemethanol, 4-1150. metilbenzolsulfonāt, (S)-(CAS No. 70987-78-9) Oxiranemethanol, 4-methylbenzen-sulfonat, (S)-(CAS No 70987-78-9) 696.

1151. dipentilester 1.2-benzoldikarbonskāb, with a branched or linear chain (CAS no 84777-06-0) n-pentilizopentilftalāt di-n-pentilftalāt (CAS No 131-18-0), diizopentilftalāt (CAS No. 605-50-5) 1.2-benzenedicarboxylic acid, dipentylester, branched and linear (CAS No 84777-06-0) n-pentyl-isopentylphthalat di-n-pentyl phthalat (CAS No 131-18-0), diisopentylphthalat (CAS No 605-50-5) 697.

1152. Benzyl butyl phthalate (BBP) (CAS No 85-68-7) Benzyl butyl phthalat (BBP) (CAS No 85-68-7) 698.

1153. benzoldikarbonskāb 1.2-di-C 7-11, alkilester, branched or linear chain (CAS No. 68515-42-4) 1.2-Benzenedicarboxylic acid di-C 7-11, branched and linear alkylester (CAS No 68515-42-4) 699.

1154. a Mixture of disodium 4-(3-etoksikarbonil-4-(4-(3-etoksikarbonil-5-hydroxy-1-(4-sulfonātfenil) pirazol-4-YL) Penta-2.4-dienilidēn)-4.5-dihydro-5-okspirazol-1-YL) benzolsulfonāt and trisodium 4-(3-etoksikarbonil-4-(4-(3-etoksikarbonil-5-oxide-1-(4-sulfonātfenil) pirazol-4-YL) Penta-2.4-dienilidēn)-4.5-dihydro-5-oksopirazol-1-YL) benzolsulfonāt (EC No 402-660-9) A mixtur of: disodi of 4-(3-ethoxycarbonyl-4-(4-(3-ethoxycarbonyl-5-hydroxy-1-(4-sulfonatophenyl) pyrazol-4-YLE) Penta-2.4-dienyliden)-4.5-dihydr-5-oxopyrazol-1-universal plug) of sulfonat and trisodi of benzen 4-(3-ethoxycarbonyl-4-(4-(3-ethoxycarbonyl-5-oxide-1-(4-sulfonatophenyl) pyrazol-4-YLE) Penta-2 4-dienyliden)-4.5-dihydr-5-oxopyrazol-1-YLE) benzenesulfonat (From ECU 402-660-9) 700.

1155. (methylene-bis (4,1-fenilēnaz (1-(3-(dimethylamino) propyl)-1.2-dihydro-6-hydroxy-4-methyl-2-oksopiridīn-5.3-2,4-diyl)))-1,1 '-dipiridīnij dichloride dihydrochloride of (EC No 401-500-5) (methyleneb (4,1-phenylen azo (1-(3-(dimethylamin) propyl)-1.2-dihydr-6-hydroxy-4-methyl-2-oxopyridin-5.3-diyl)))-1,1 '-dipyridini of dichlorid of dihydrochlorid (ECU From 401-500-5) 701.

1156.2-[2-hydroxy-3-(2-chlorophenyl)-1-naftilaz-karbamoil]-7-[2-hydroxy-3-(3-metilfenil)-karbamoil-1-naftilaz] Fluorene-9-one (EC No 420-580-2), 2-[2-hydroxy-3-(2-chlorophenyl)-1-naphthylaz carbamoyl]-7-[2-hydroxy-3-(4-methylphenyl)-carbamoyl-1-naphthylaz] fluoren-9-one (From 420-580-2) 702.

1157. Azafenidin (CAS no 68049-83-2) Azafenidin (CAS No 68049-83-2) 703.

1158.2,4,5-trimethylaniline (CAS No 137-17-7) 2,4,5-trimethylaniline hydrochloride (CAS No. 21436-97-5) 2, 4, 5-trimethylanilin (CAS No 137-17-7) 2, 4, 5-trimethylanilin-hydrochlorid (CAS From 21436-97-5) 704.

1159.4, 4 '-thiodianiline and its salts (CAS No. 139-65-1) 4, 4 '-thiodianilin and it is cold (CAS No 65-139-1) 705.

4, 4 '-oxydianiline 1160. (p-aminofenilēter) and its salts (CAS No 101-80-4) 4, 4 '-oxydianilin (p-aminophenyl ether) and it is cold (CAS No 101-80-4) 706.

1161. N, N, N ', N '-tetramethyl-4,4-methylenedianiline (CAS No 101-61-1) N, N, N ', N '-tetramethyl-4, 4 '-methylendianilin (CAS No 101-61-1) 707.

1162.6-methoxy-m-toluidine (p-cresidine) (CAS No. 120-71-8), 6-methoxy-m-toluidin (p-cresidin) (CAS No 120-71-8) 708.

1163.3-ethyl-2-methyl-2-(3-aka)-1.3-oxazolidine (CAS no 143860-04-2) 3-ethyl-2-methyl-2-(3-methylbutyl)-1.3-oxazolidin (CAS No 143860-04-2) 709.

1164. A mixture consisting of 1, 3, 5-TRIS (3-aminometilfenil)-5-(1 h, 3 h, 5 h)-triazine-.6 trion and 3.5-bis (3-aminometilfenil)-1-Paul [3,5-bis (3-aminometilfenil) -2,4, 6-trioks-1,3,5-(1 h, 3 h, 5 h)-triazine-1-YL]-5-(1 h, 3 h, 5 h)-triazine-trion-.6 oligomers (EC No. 421-550-1) A mixtur of: 1, 3, 5-TRIS (3-aminomethylphenyl)-5-(1 h, 3 h, 5 h)-triazin-2,4,6-trion and a mixtur of oligomer of 3.5-bis (3-aminomethylphenyl)-1-[3,5-bis poly (3-aminomethylphenyl) -2,4 .6-1-triox , 3.5-(1 h, 3 h, 5 h)-triazin-1-5-YLE]-(1 h, 3 h, 5 h)-triazin-2,4,6-trion (ECU From 421-550-1) 710.

1165.2-nitrotoluene (CAS No 88-72-27) 2-nitrotoluen (CAS No 88-72-2) 711.

1166. Tributyl phosphate (CAS No 126-73-8) Tributyl phosphate (CAS No 126-73-8) 712.

1167. Naphthalene (CAS No. 91-20-3) Naphthalen (CAS No 91-20-3) 713.

1168. Nonylphenol (CAS no 25154-52-3), 4-nonylphenol, branched-chain (CAS No. 84852-15-3) Nonylphenol (CAS No 25154-52-3), 4-nonylphenol, branched (CAS No. 84852-15-3) 714.

1169.1, 1-trichloroethane 2 (CAS No 79-00-5), 1-1, 2 trichloroethan (CAS No 79-00-5) 715.

1170. Pentahloretān (CAS No 76-01-7) Pentachloroethan (CAS No 76-01-7) 716.

1171. Vinylidene (1.1-dichloroethylene) (CAS No 75-35-4) Vinyliden-chloride (1.1-dichloroethylen) (CAS No 75-35-4) 717.

1172. Alilhlorīd (3-chloropropene) (CAS No 107-05-1) Allyl chloride (3-chloropropen) (CAS No 107-05-1) 718.

1173.1.4-dichlorobenzene (p-dichlorobenzene) (CAS No 106-46-7) 1.4-dichlorobenzen (p-dichlorobenzen) (CAS No 106-46-7) 719.

1174. bis (2-chloroethyl) ether (CAS No 111-43-4) bis (2-chloroethyl) ether (CAS No 111-43-4) 720.

1175. Phenol (CAS No 108-95-2) Phenol (CAS No 108-95-2) 721.

1176. Bifenol A (4, 4 '-isopropylidenediphenol) (CAS No. 80-05-7) Bisphenol A (4, 4 '-isopropylidenediphenol) (CAS No 80-05-7) 722.

1177. Trioksimetilēn (1,3,5-trioxane) (CAS No 110-88-3) Trioxymethylen (1,3,5-trioxan) (CAS No 110-88-3) 723.

1178. Propargīt (ISO) (CAS No. 2312-35-8) Propargit (ISO) (CAS No 2312-35-8) 724.

1179.1-chloro-4-nitrobenzene (CAS No 100-00-5) 1-chlor-4-nitrobenzen (CAS No 100-00-5) 725.

1180. Molinate (ISO) (CAS no 2212-67-1), Molinat (ISO) (CAS No 2212-67-1) 726.

1181. Fenpropimorph (CAS no 67564-91-4) Fenpropimorph (CAS No 67564-91-4) 727.

1182. Epoxiconazole (CAS no 133855-98-8) Epoxiconazol (CAS No 133855-98-89) 728.

1183. Metilizocianāt (CAS No. 624-83-9) Methyl (CAS No isocyanat 624-83-9) 729.

1184. N, N-dimethylaniline-tetrakis (pentafluorfenil) Borate (CAS No. 118612-00-3) N, N-tetrakis (pentafluorophenyl) dimethylanilini of borat (CAS No 118612-00-3) 730.

1185. O, o'-(etenilmetilsililēn) di [(4-metilpentān-2-one) oksīm] (EC No. 421-870-1) O, o'-(ethenylmethylsilylen) di [(4-methylpentan-2-one) oxim] (ECU From 421-870-1) 731.

1186. in relation 2:1 prepared mixture, consisting of 4-(4-hydroxy-2, 4-trimethyl-2-4 hromanil) rezorcinol-4-YL-TRIS (6-5.6-dihydro-diaz-5-oksonaftalīn-1-sulfonate) and 4-(2-hydroxy-2, 4-trimethyl-2-4 hromanil) rezorcinol-bis (5-5.6-dihydro-diaz-5-oksonaftalīn-1-sulfonate) (CAS no 140698-96-0) 2:1 A mixtur of: 4-(4-hydroxy-2, 4-trimethyl-2-4 chromanyl) resorcinol-4-YLE-TRIS (6-diaz-dihydr-5.6-5-oxonaphthalen-1-sulfonat) and 4-(2-hydroxy-2, 4-trimethyl-2-4 chromanyl), resorcinolb (6-diaz-dihydr-5.6-5-oxonaphthalen-1-sulfonat) (CAS No 140698-96-0) 732.

1187. A mixture consisting of 4, 4 '-methylene-bis [2-(4-hidroksibenzil)-3.6-dimetilfenol] and 6-5.6-dihydro-diaz-5-oksonaftalīnsulfonāt (1:2) reaction products and 4, 4 '-methylene-bis [2-(4-hidroksibenzil)-3.6-dimetilfenol] and 6-5.6-dihydro-diaz-5-oksonaftalīnsulfonāt (1:3) reaction products (EC No 417-980-4) A mixtur of: reaction product of 4, 4 '-methyleneb [2-(4-hydroxybenzyl) 3.6-dimethyl-phenol] and 6-diaz-dihydr-5.6-5-oxo-naphthalenesulfonat (1:2) and the reaction product of 4, 4 '-methyleneb [2-(4-hydroxy benzyl)-3.6-dimethylphenol] and 6-diaz-5 6-dihydr-5-oxonaphthalenesulfonat (1:3) (From ECU 417-980-4) 733.

1188. Malahītzaļ in hydrochloride (CAS Nr. 569-64-2) in the Malahītzaļ oxalate (CAS No. 18015-76-4) green hydrochlorid Malachit (CAS No 70987-78-9), Malachit green oxalat (CAS No 18015-76-4) 734.

1189.1-(4-chlorophenyl)-4.4-dimethyl-3-(1, 2, 4-triazole-1-ilmetil) pentane-3-ol (CAS no 107534-96-3), 1-(4-chlorophenyl)-4.4-dimethyl-3-(1, 2, 4-triazole-1-ylmethyl) pentan-3-ol (CAS No 107534-96-3) 735.

1190.5-(3-butiril-2, 4, 6-trimetilfenil)-2-[1-(etoksiimin) propyl]-3-hidroksiciklohek-2-Ene-1-one (CAS no 138164-12-2) 5-(3-4, 6-2, butyryl-trimethylphenyl)-2-[1-(ethoxyimin) propyl]-3-hydroxycyclohex-2-en-1-one (CAS No 138164-12-2) 736.

1191. TRANS-4-phenyl-L-PROLINE (CAS no 96314-26-07) TRANS-4-phenyl-L-prolin (CAS No 96314-26-0) 737.

1192. Bromoksinilheptanoāt (ISO) (CAS-Nr. 56634-95-8) heptanoat Bromoxynil (ISO) (CAS No 56634-95-8) 738.

1193. A mixture consisting of 5-[(4-[(4-amino-1-Hydroxy-3-2-naftil-sulfa) azo]-2.5-dietoksifenil) azo]-2-[(3-fosfonfenil) azo] benzoic acid and 5-[(4-[(4-amino-1-Hydroxy-3-2-naftil-sulfa) azo]-2.5-dietoksifenil) azo]-3-[(3-fosfonfenil) azo] benzoic acid (CAS no 163879-69-4) A mixtur of: 5-[(4-[(7-amino-1-hydroxy-3-2-naphthyl-sulfa) azo]-2.5-diethoxyphenyl) azo]-2-[(3-phosphonophenyl) azo] benzoic acid and 5-[(4-[(7-amino-1-hydroxy-3-2-naphthyl-sulfa) azo]-2.5-diethoxy phenyl) azo]-3-[(3-phosphonophenyl) azo] benzoic acid (CAS No 163879-69-4) 739.

1194.2-{4-(2-amonijpropilamin)-6-[4-hydroxy-3-(5-methyl-2-methoxy-4-sulfamoilfenilaz)-2-sulfonātnaf-7-ilamin]-5-triazin-2-ilamin a}-2-aminopropilformiāt (EC No 260-424-3) 2-{4-(2-ammoniopropylamin)-6-[4-hydroxy-3-(4-methyl-2-methoxy-4-Sulfamoylphenyl azo)-2-sulfonatonaphth-7-ylamin]-5-triazin-2-ylamin a}-2-aminopropyl formats (From ECU 424-260-3) 740.

1195.5-Nitro-o-toluidine (CAS No 99-55-8), 5-Nitro-o-toluidine hydrochloride (CAS no 51085-52-0) 5-Nitro-o-toluidin (CAS No 99-55-8), 5-Nitro-o-toluidin-hydrochlorid (CAS No 51085-52-0) 741.

1196.1-(1-naftilmetil) hinolīnij chloride (CAS no 65322-65-8) 1-(1-naphthylmethyl) of quinolini chloride (CAS No 65322-65-8) 742.

1197. (R)-5-bromo-3-(1-methyl-2-pirolidinilmetil)-1 h-indole (CAS no 143322-57-0) (R)-5-bromo-3-(1-methyl-2-pyrrolidinylmethyl)-1 h-indole (CAS No 143322-57-0) 743.

1198. Pymetrozine (ISO) (CAS no 123312-89-0) Pymetrozin (ISO) (CAS No 123312-89-0) 744.

1199. Oxadiargyl (ISO) (CAS no 39807-15-3) Oxadiargyl (ISO) (CAS No 39807-15-3) 745.

1200. Chlorotoluron (3-(3-chloro-p-tolil)-1.1-dimetilurīnviel) (CAS no 15545-48-9) Chlorotoluron (3-(3-p-tolyl-chlor)-1.1-dimethylure) (CAS From 15545-48-9) 746.

1201. N-[2-(5-nitrotiofēn-acetyl-3-2-ilaz)-5-dietilaminofenil] acetamide (EC No 416-860-9) N-[2-(3-acetyl-5-nitrothiophen-2-ylaz)-4-diethylaminophenyl] acetamid (EC No 416-860-9) 747.

1202.1.3-bis (vinilsulfonilacetamid)-propane (CAS no 93629-90-4) 1.3-bis (vinylsulfonylacetamid)-propan (CAS No 93629-90-4) 748.

1203. p-fenetidīn (4-etoksianilīn) (CAS No. 156-43-4) p-phenetidin (4-ethoxyanilin) (CAS No 156-43-4) 749.

1204. m-Phenylenediamine and its salts (CAS No 108-45-2) m-phenylenediamin and it is cold (CAS No 108-45-2) 750.

1205. Residues (coal tar), creosote for des., if content >% benzo 0.005 [a]-pyrene (CAS no 92061-93-3) Residu (coal tar), creosot oil distn., if it contains > 0.005% w/w benzo [a] pyren (CAS No 92061-93-3) 751.

1206. Creosote, acenaphthene fraction wash oil, if it contains > 0.005% by benzo [a] pyrene (CAS no 90640-84-9) Creosot, acenaphthen fraction of the oil, wash oil, if it contains > 0.005% w/w benzo [a] pyren (CAS No 90640-84-9) 752.

1207. Creosote if contains > 0.005% by benzo [a] pyrene (CAS no 61789-28-4) Creosot oil, if it contains > 0.005% w/w benzo [a] pyren (CAS No 61789-28-4) 753.

1208. Creosote, if containing 0.005% benzo > [a]-pyrene (CAS no 8001-58-9), if it contains Creosot > 0.005% w/w benzo [a] pyren (CAS No 8001-58-9) 754.

1209. Creosote, the distillate of high boiling point, wash oil, if it contains > 0.005% by benzo [a] pyrene (CAS no 70321-79-8) Creosot oil, high-boiling distillat, wash oil, if it contains > 0.005% w/w benzo [a] pyren (CAS No 70321-79-8) 755.

1210. extraction residues (coal), creosote oil acid washing of the extraction residues, 0.005% if content > benzo [a] pyrene (CAS no 122384-77-4) extract residu (coal), oil creosot acid, wash oil extract, if it contains residu > 0.005% w/w benzo [a] pyren (CAS No 122384-77-4) 756.

1211. Creosote, distillate with a low boiling point, wash oil, if it contains > 0.005% by benzo [a] pyrene (CAS no 70321-80-1) Creosot oil, low-boiling distillat, wash oil, if it contains > 0.005% w/w benzo [a] pyren (CAS No 70321-80-1) notes. (1) the reference number of This part 2 of annex 1 and 2 in column is 291. in box is 364. (2) the reference number of This part 2 of the annex 1 in box is the box and 2.290 is 413. "
Prime Minister a. Halloween Health Minister g. Smith attachment Cabinet of 23 May 2006 no. 420 "provisions of Annex 8 of the Cabinet of Ministers of 20 April 2004, regulations No 354 cosmetic sampling, sample preparation and cosmetic chemicals contained in methods 1. Cosmetic sampling 1. Cosmetic products total sample (the sample as a whole, some of which are one and the same batch number), having in their original containers and n't open sends a laboratory. 2. Cosmetic products (market offered bulk or small trade of sold in packaging that is different from the manufacturer's original packaging you) samples in laboratory containers (subjects, which placed in the product and which continuously faced with it) in view of the quantity necessary for analysis. 3. laboratory requires samples to be determined by the analytical method. 4. The samples are sealed (sealed) and add the labels in accordance with regulations, arrangements for market surveillance authorities to request and receive product samples, as well as those handled by the laboratory or other expertise. 5. sampling and certificate completed in accordance with the laws, regulations of the ERS, arrangements for market surveillance authorities to request and receive product samples, as well as those handled by the laboratory or other expertise. 6. individual samples (units taken from the lot offered for sale) must be stored in accordance with the manufacturer's instructions shown on the label. 7. laboratory samples (total sample representative of the faction to be analysed in separate laboratories), stored in the dark at 10-25 ° C, unless other conditions are specified. 8. open directly in individual samples prior to analysis. 2. preparation of the test portion in 9 laboratories. If possible, each of the individual samples are analysed separately. If the sample is too small, use a minimum number of samples. 10. before the test portion (representative of the laboratory sample quantity required per analysis) of sampling in certain samples of well mixed. 11. In accordance with the relevant method of analysis of the container that holds the sample, open the inert gas and, as soon as possible, the necessary number of test specimens are taken. The analysis shall be carried out as quickly as possible. If you want to save the model, close the container in inert gas. 12. If the original homogeneous cosmetic product distribution through the phases, the test portion before sampling it homogenize again. 13. If the cosmetic product on the market in a way that can not be handled in accordance with the methods laid down in this annex and in the case where the relevant analysis methods not provided for in this annex, an original procedure may be adopted, provided that it describes the analysis report. 14. Liquid cosmetic products (oil, alcohol solution or water, toilet water, aftershave, or Royal Jelly, which can be packed in flasks, bottles, ampoules or tubes) of the test portion in the following order: 14.1 the container shake vigorously before opening. 14.2. Open the container. 14.3. A few millilitres of the liquid is poured into a test tube to visually assess its characteristics in order to take the test portion. 14.4. If necessary, take the test portion. 14. close the container carefully. 15. the Slurry of cosmetic products (pastes, creams, emulsions and gels that can be packed in tubes, plastic bottles or jars) of the test portion in the following order: 15.1 Of the containers with a narrow neck to remove at least the first centimetre of the product. Squeezes the test portion and reseal the container immediately. 15.2. From the dishes with a wide neck evenly scraped away the surface, removing the top layer. Remove the test portion and reseal the container immediately. 16. Hard cosmetic (loose powders, compacted powders, pencils, which can be packed in different containers) of the test portion in the following order: 16.1. Loose powder before unpacking or shake vigorously to open, open and separate the test portion. 16.2. From pressed powder or pencil evenly scraped away the top layer. Withdrawal of the test portion of the exposed layer. 17. the Aerosol (any non-reusable container made of metal, glass or plastics and containing a gas compressed, liquefied or under pressure in liquid form with or without a liquid, paste or powder, and is equipped with a device which allows content to flow out as solid or liquid particles with gas, foam, powder or liquid) of the test portion as follows: spray the container shake vigorously the representative of the amount of content, with a suitable connector (for example, Figure 1; except for the method of analysis can predict the other connectors) into a glass bottle, covered with plastic (Figure 4) and applied to the aerosol valve but not siphon tubes. The transfer quantity, bottle with valve down there. It's moving, the content becomes clearly visible in one of the following four ways: 17.1. Spray in the form of a homogeneous solution for direct analysis. 17.2. Spray, which consist of two liquid phases. Each phase can be analyzed after the lower phase is transferred to another bottle, the first bottle holding the valve down. The lower phase is often watery, and there are no propellant (such as Bhutan and water mixture). 17.3. An Aerosol that contains suspended powder. The liquid phase can be analyzed after the powder separation. 17.4. the cosmetic foam or cream. First bottle weigh accurately 5 g of 2-Methoxyethanol to 10, thus preventing foam formation during degazācij and enables you to output the propellant gases without loss of liquid. 18. the quantitative sampling of Aerosol test uses the following accessories: 18.1. Connector (Figure 1), which is made of Duralumin or brass. It's designed so that with a polyethylene adaptor can be tailored for different valve systems. You can use other connectors (fig. 2 and 3). 18.2. Bottle, described in paragraph 17 of this annex. Its volume is 50 to 100 ml. 19. to transfer enough of the sample from the bottle blow air. To this end, the connector type about 10 ml of dichlorodifluoromethane or butane (depending on the test of the product) and, holding the bottle with valve to the highest position, Degas, to disappear completely in liquid phase. Remove the connector. Weigh the bottle (a grams). Shake vigorously spray from which the sample was taken. Attach the connector to the aerosol container to be valve (dish holding the valve upwards) bottle (neck down) at the connector. Filled about two-thirds of the bottle. If the transfer ends prematurely so that the pressure equalization, it can be renewed by chilling a bottle. The sample thus obtained can be used: 19.1. standard chemical analysis: 19.1.1. Degas, holding the transfer bottle valve upwards. If the degazēj occurs foam bottle, which uses the connector with the syringe above accurately weighed quantity entered (5-10 g) 2-methoxyethanol. 19.1.2. Complete separation of volatile constituents without loss by shaking in a water bath kept at 40 ° C temperature. Remove the connector. 19.1.3. Reweigh the bottle (c g) to determine the mass of the balance of m2 (m2 = c-a) (calculation of residual mass, subtract 2-Methoxyethanol was used). 19.1.4. Removing the valve, open the bottle. 19.1.5. dissolve the residue completely in a known quantity of an appropriate solvent. 19.1.6. Take aliquots of quantitative analysis. The calculation uses the following formula: and that m1 – the bottle entered aerosol mass; M2 – the mass of the residue after heating at 40 ° C; r – the percentage of the substance m2 (determined by the respective methods); R – the percentage of the substance for analysis received spray; Q – the total mass of the substance in the aerosol container; P-spray (individual samples) in a clean start. 19.2. the analysis of the volatile constituents by gas chromatography: 19.2.1. With gas chromatography syringe from the bottle takes the appropriate amount. The syringe contents enter the gas chromatograph. 19.2.2. using A2 series 25 l or 50 µ µ (Figure 5) or equivalent gas-chromatography syringe for accurate volume of the sample nomērīšan. This syringe is put in the tip of the needle valve. With the connector attached to the bottle and syringe to polyethylene tube (length 8 mm, internal diameter 2.5 mm) syringe connected to the bottle. 19.2.3. when the bottle filled the quantity of spray, the conical tip of the syringe attached to the bottles in accordance with 19.2.2. of this annex. Open the valve and pumped into the appropriate quantity of liquid. Output of gas bubbles, several times turning the piston (if necessary, cool the syringe). When the syringe is the quantity of fluid without bubbles, close the valve and disconnect the syringe from the bottle. Add a needle, syringe type gas chromatograph injector, open the valve and enters the syringe content. 19.2.4. If necessary, enter the internal standard bottle (with an ordinary glass syringe using a connector).
Figure 1 figure 2 P1 connector connector M2 transition between deep and comprehensive the valves Figure 3 connector M1 transition between the two valves of the enormous figure 4 bottle. Capacity 50-100 ml syringe Figure 5 gas sample 3. Free sodium and potassium hydroxides quantitative and qualitative determination of free sodium and potassium hydroxides quantitative and qualitative method of determining the procedure for quality large amounts of free sodium or potassium hydroxides in cosmetic products and the determination of free sodium or potassium hydroxides in hair styling products and solvents intended for the rope to slide the nail. 21. Free sodium and potassium hydroxide is determined by the volume of standard acid required to neutralize the product, get the quantity expressed in free sodium hydroxide by mass. 22. Laboratory sample is dissolved or disperse water and titrated with standard acid. Adding acid, recorded pH value: plain sodium or potassium hydroxide solution end point is the sharp rise in the pH value. The simple titration curve may change: 22.1. Ammonia and other weak organic bases, which the titration curve is without sharp jumps. This method of ammonia distillation separates the vacuum at room temperature. 22.2. The weak acid salts, titration curve can lead to several leaps. In such a case, only the first part of the curve to match the first leap free of sodium or potassium hydroxide neutralization of hydroxyl ion coming from. If weak inorganic acid salts substantially interfering effects of alternative titration in alcohol. It is theoretically possible that the high pH levels other soluble strong bases (for example, Lithium hydroxide, quaternary ammonium hydroxide), however, the probability of the presence of this type of cosmetic products is very small. 3.1. Identification 23. use alkaline Reagent standard buffer pH 9.18 at 25 ° C: 0.05 M sodium tetraborāt a dekahidrāt. 24. quality determination requires the following equipment: 24.1. Usual laboratory glassware. 24.2. a pH meter. 24.3. glass membrane electrode. 15.2. Calomel reference electrode. 25. a pH meter is calibrated with the electrodes using a standard buffer solution. Prepare the test product 10% solution or dispersion in water and filter. Measure the pH. If the pH is 12 or more, the determination shall be made. 3.2. Identification 26. Titration in the aquatic environment carried out in the following order: 26.1. Agent uses the standard 0.1 n hydrochloric acid. 26.2. For titration of water environment using equipment: 26.2.1. Usual laboratory glassware. 26.2.2. pH meter preferably with recorder. 26.2.3. glass membrane electrode. 26.2.4. Standard calomel reference electrode. 26.3.150 ml beaker weigh accurately a test portion of 0.5-1.0 g. If the quantity of ammonia is present add a few vārķer body, place the beaker in a vaccum Desiccator, evacuate using a water pump until the odour of ammonia is no longer detectable (about three hours). 26.4. Add 100 ml water, dissolve or disperse the residue and Titrate with the 0.1 n hydrochloric acid solution of pH changes are recorded. 26.5. determine the titration curve of growth points. If the first point is the low growth in pH 7 level, the sample does sodium or potassium hydroxide. 16.5. If the curve has two or more points, a significant increase is only the first paragraph. 16.6. the volume of titrant first growth point. 16.7. the volume of Titrant is denoted by V, expressed in millilitres, the test mass, in grams, of the quantity denoted by m. 26.9. Sodium or potassium hydroxide content of the sample expressed in% and calculated according to the formula:. 26.10. If, contrary to the claims of sodium or potassium hydroxide in the presence of a large quantity of titration curve does not appear clear growth point, the determination is repeated in isopropanol. 27. Titration in isopropanol performed in the following order: 27.1. For titration in isopropanol reagents used are: 27.1.1. Isopropanol. 27.1.2.1.0 n hydrochloric acid solution. 27.1.3. By diluting the 1.0 n hydrochloric acid with isopropanol prepared immediately before use 0.1 n hydrochloric acid in isopropanol. 27.2. For titration in isopropanol used equipment: 27.2.1. Usual laboratory glassware. 27.2.2. pH meter preferably with recorder. 27.2.3. glass membrane electrode. 27.2.4. Standard calomel reference electrode. 27.3.150 ml beaker weigh accurately a test portion of the 0.5-1.0 g. If ammonia is present add some boiling granules, place the beaker in a vaccum Desiccator, evacuate using a water pump until the odour of ammonia is no longer detectable (about three hours). Add 100 ml isopropanol, dissolve or disperse the residue and Titrate with the 0.1 n hydrochloric acid solution of pH changes are recorded. 27.4. calculation carried out in accordance with this annex, paragraph 26, assuming the first inflection point is about 9 pH level. 28. If the sodium or potassium hydroxide content in sodium hydroxide 5% mass expression, from a single sample, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.25%. 4 4. Oxalic Acid and its alkaline salts in quantitative and qualitative determination of hair care products 29. Oxalic Acid and its alkaline salts in quantitative and qualitative determination of hair care products method determines the procedure of its oxalic acid and alkali salts, quantitatively and qualitatively, the determination of hair care products. You can use the colorless water/alcohol solutions and lotions which contain about 5% oxalic acid or an equivalent quantity of alkali metal oxalates. 30. in paragraph 29 of the annex to the method referred to in the quantification of the Sorrel acids or salts of the alkali content of the sample expressed as oxalic acid percentage by mass of the free. 31. After all the active anionic surface agent, which is a removal with p-toluidine hydrochloride, oxalic acid or oxalates are precipitated as calcium oxalate. Then filter the solution, dissolve the precipitate in sulphuric acid and titrated with potassium permanganate. 32. Oxalic Acid and its alkaline salts in quantitative and qualitative determination of hair care products to be used in the method reaģenti1:32.1. Ammonium acetate solution, 5% mass. 32.2. calcium chloride solution, 10% of the mass. 32.3. Ethanol, 95% (by volume). 32.4. Carbon tetrachloride. 32.5. diethyl ether. 32.6. p-toluidine dihydrochloride solution, 6.8%. 32.7.0.1 N potassium permanganate solution. 20.4. sulphuric acid, 20% by mass. 32.9. Hydrochloric acid, 10% of the mass. 32.10. sodium acetate trihydrate. 32.11. Glacial acetic acid. 32.12. sulphuric acid (1:1). 32.13. Saturated barium hydroxide solution. 33. Oxalic Acid and its alkaline salts in quantitative and qualitative determination of hair care products, equipment used in the method: 33.1. Separating funnels, 500 ml. 33.2. Beakers, 50 ml. and glass 600 33.3. G-4 filter crucible. 20.8. Measuring cylinders, 25 and 100 ml. Pipette 10 ml 20.8.20.9.500 ml flasks, Bunsen. 20.9. Water pump. 33.8. Thermometer graduated from 0 to 100 ° C. 21.1. magnetic stirrer with heating element. 33.10. Magnetic rods with a teflon coating. 33.11. Burette, 25 ml. 33.12. Conical flasks, 250 ml. 4.1 determination 34. Weigh 6-7 g of the sample into a 50 ml beaker with dilute hydrochloric acid (32.9. bottom) to pH 3 and with 100 ml of distilled water into a separating funnel. In turn add 25 ml of ethanol, 25 ml p-toluidine dihydrochloride solution and 25-30 ml of carbon tetrachloride and the mixture is shaken vigorously. 35. when the phases are separated, separates the lower (organic) phase repeat the extraction with this annex referred to in paragraph 34 of the reagents and again separate the organic phase. 35. Water solution into a 600 ml beaker and boil the solution, all the carbon tetrachloride that are not separated. 36. Add 50 ml of ammonium acetate solution, heat the solution to the boil and stir in the boiling solution 10 ml of hot calcium chloride solution, allows the sediment to settle. 37. adding a few drops of calcium chloride solution, check that precipitation is complete, allow to cool to room temperature, then stir in 200 ml of ethanol and leave for 30 minutes. 38. Filter the liquid through a glass filter Crucible, with a small quantity of hot water (50-60 ° C) the precipitate on the filter Crucible and wash with cold water. 39. The precipitate five times with small amounts of ethanol and then five times with a little diethyl ether, and dissolve the precipitate in 50 ml of hot sulphuric acid, sulfuric acid under reduced pressure at filtering out through the filter crucible. 40. The solution without loss into a conical flask and titrated with a solution of potassium permanganate, until the solution becomes pale pink. 41. the percentage of the mass of oxalic acid content of the sample, is given by the formula:% oxalic acid =, where A-0.1 N potassium permanganate consumption, measured in accordance with paragraph 40 of this annex; E – the quantity of test sample (g) (paragraph 34); 4.50179-the conversion factor for oxalic acid. 42. If the oxalic acid content of about 5%, from the same sample, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.15%. 4 4.2. Identification 43. Oxalic Acid or oxalates are precipitated as calcium oxalate and dissolved in sulphuric acid. The solution adds a little potassium permanganate solution that turns colourless and causes the formation of carbon dioxide. This carbon dioxide through barium hydroxide solution, a white precipitate of barium carbonate (turbidity). 44. a quantity of test sample treated in accordance with this annex, 34, 35 and 36, thus separating the room detergents. 45. Approximately 10 ml solution obtained in accordance with this annex, 44, adds blade tip of sodium acetate and acidify the solution with a few drops of glacial acetic acid. 46. Add 10% calcium chloride solution and filter. The calcium oxalate precipitate is dissolved in 2 ml of sulphuric acid (1:1). 47. The solution into a test tube and drop by drop, add about 0.5 ml of 0.1 N potassium permanganate solution. If the solution contains oxalate solution loses color – at first gradually, then rapidly. 48. immediately after adding the potassium permanganate, the tube with the stopper stopper, which is suitable for glass tube a little tube content slightly and collect the carbon dioxide formed in a saturated barium hydroxide solution. If after three to five minutes of visible white turbidity of barium carbonate, oxalic acid in the solution. 5. the determination of chloroform in toothpastes in 49. quantitative determination of chloroform in toothpaste in the method used for gas chromatography determination of the quantity of chloroform in toothpaste. This method is suitable for the quantitative determination of chloroform at levels of 5% or less. The chloroform content determined is expressed as percentage by mass of the product. 50. Toothpaste is suspended in methanol and dimethylformamide, a mixture which Add a known amount of Acetonitrile as internal standard. By centrif gēšan part of the liquid phase gas chromatography and take the chloroform content calculated. 51. quantitative determination of chloroform in toothpaste method uses the following reaģentus1:51.1. Porapak Q, Chromosorb 101 or equivalent, which the particle size is 80 – 100.51.2. Acetonitrile. 51.3. the chloroform. 51.4. Dimethylformamide. 51.5. Methanol. 51.6. Internal standard solution, which prepare, pipette 50 ml standard flask, pipette 5 ml of dimethylformamide and adding about 300 mg (M mg) of Acetonitrile, accurately weighed. Make up to the mark with dimethylformamide and mix. 32.1. The solution is required to determine the relative response factor, prepare, pipette 10 ml standard flask, pipette 5 ml of the internal standard solution and add about 300 mg (M1 mg) accurately weighted chloroform. Make up to the mark with dimethylformamide and mix. 52. the quantitative determination of chloroform in toothpaste method uses the following machinery and equipment: 52.1. Analytical balance. 52.2. Gas Chromatograph with a flame ionization detector. 52.3. Microsyringe with a capacity of 5 to 10 l and 0.1 µ µ l section. 52.4. Graduated pipettes of 1, 4 and 5 ml capacity. 52.5. volumetric flasks, 10 and 50 ml. Tubes, 52.6. approximately 20 ml, with screw caps, Sovirel type of France No 20 or equivalent. Screw cover plate sealing inside are, on one side coated with teflon. 52.7. Centrifuge. 53. appropriate conditions for gas chromatography are: 53.1. column (materials-glass, length 150 cm, internal diameter 4 mm, external diameter 6 mm), using a vibrator with Porapak Q, Chromosorb 101 or equivalent material with a particle size of 80 – 100.53.2. Flame ionization detector sensitivity adjusted so that, when you enter 3 µ l of the solution (51.7), acetonitrile peak height would be approximately three quarters of the full deflection. 53.3. Carrier gas: nitrogen, flow rate 65 ml/min gas flow detector shall be adjusted so that the flow of air or oxygen 5-10 times than the hydrogen flow. 53.4. Temperature: 210 ° C in 53.4.1. injector. 53.4.2.210 ° C detector. 53.4.3. column oven at 175 ° c. 13. A chart speed of about 100 cm per hour. 54. The test sample taken from an open tube. Remove one-third of the content of the tube screws the back cover, thoroughly mix the tube and take the test portion. 55. Screw tube up to the nearest 10 mg, 6 to 7 g (Mo g) toothpaste, treated in accordance with this annex, paragraph 54, and add three small glass beads. 56. With the pipette tube pipette exactly 5 ml of the internal standard solution, 4 ml of dimethylformamide and 1 ml of methanol into the tube and mix. 57. shake for half an hour with a mechanical Shaker and 15 minutes the screwed tube centrifuge at the speed to phase fully delimited. If the liquid phase remains cloudy after centrifuging, it also can change the liquid phase, adding 1 to 2 g of sodium chloride, allowing you to settle and again by centrifugation. 58. According to paragraph 53 of this annex 3 of this supplement 57 µ l referred to in solution. Repeat the above step. According to the above conditions the retention time can be expressed with the following indicative values: 58.1. methanol for about one minute 58.2. acetonitrile approximately 2.5 minutes 58.3. chloroform about six minutes 58.4. dimethylformamide > 15 minutes 59. to determine the relative response factor, enter 3 ¶l of the solution (51.7). Repeat this operation. The relative response factor is determined each day. 60. The relative response factor is calculated as follows: 60.1. Size of Acetonitrile and chloroform peaks of height and width at half peak and calculates both the peak area by using the formula: height × width at half. 60.2. acetonitrile and chloroform determined peak areas in the chromatograms obtained in accordance with this annex, paragraph 59, and calculate the relative response fs with the following formula: fs-chloroform which relative response factor; Axis-of the chloroform peak area (paragraph 59); A1-acetonitrile peak area (paragraph 59); Ms – the quantity of chloroform (in milligrams) in 10 ml of the solution specified in this annex, paragraph 59 (= M1); MI-acetonitrile (in milligrams) in 10 ml of the solution specified in this annex, paragraph 59 (1/10 M). Calculates the average of the readings obtained. 61. The chloroform content calculated as follows: 61.1. in accordance with this annex, section 60.1. calculation of the chloroform and acetonitrile peaks of the chromatograms obtained in accordance with paragraph 58 of this annex describes the procedure. 61.2. Chloroform content in the toothpaste is given by the following formula: where% X-content of chloroform in toothpaste, expressed as percentage by weight; Axis-of the chloroform peak area (paragraph 58); AI-acetonitrile peak area (paragraph 58); MSX-55 of this annex shows the mass of mg (= 1000 Mo); MI-acetonitrile (in milligrams) in 10 ml of the solution obtained in accordance with this annex 56 (1/10 M). Calculate average levels and expresses with 0.1% accuracy. 62. If the chloroform content of about 3%, from the same sample, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.3%. 4 6. quantitative determination of zinc in zinc 63. quantification method apply to the chloride, sulphate or 4-hydroxybenzenesulphonate, or more of these zinc salts in the determination of zinc in cosmetic products. 64. The zinc content of the sample in the laboratory of bis (2-methyl-8-hinolīnoksīd) in the form of determination of gravimetric and expressed in the sample as a percentage by mass of zinc. 65. the zinc acid Solution environment precipitated zinc bis (2-methyl-8-hinolīnoksīd) form. After filtering, the precipitate is dried and weighed. 66. Zinc quantification method uses the following reaģentus1:66.1. concentrated ammonia, 25%; = 0.91.66.2. Glacial acetic acid. 66.3. ammonium acetate. 66.4.2-methylquinolin-8-ol. 41.3. Ammonia solution, 6% by mass. Transfer 240 g of concentrated ammonia to 1000 ml volumetric flask, make up to the mark with distilled water and mix. 66.6.0.2 M ammonium acetate solution obtained by dissolving 15.4 g of ammonium acetate in distilled water, make up to 1000 ml volumetric flask and mix well. 66.7.2-methylquinolin-8-ol solution obtained by dissolving 5 g 2-methylquinolin-8-ol in 12 ml of glacial acetic acid and transfer with distilled water to 100 ml volumetric flask. Make up with distilled water and mix. 67. Zinc determination method using such apparatus and equipment: 67.1. volumetric flasks, 100 and 1000 ml beakers, 400 ml 67.2.. Measuring cylinders, 50 and 67.3.150 ml. Graduated pipettes, 10 ml 41.9. Glass filter crucibles G 67.5.-4. 67.6. Suction flasks, 500 ml. Water pump 67.7. mm. Thermometer graduated from 0 to 100 ° C. 67.9. Desiccator with a suitable desiccant and humidity indicator, e.g. Silicagel or equivalent. 67.10. Drying oven set at 150 ± 2 ºc. 67.11. pH meter. 67.12. Hot plate. 68. Weigh 400-ml beaker, 5 to 10 g (M gram) of the test sample containing about 50-100 mg of zinc, add 50 ml of distilled water and mix. 69. For every 10 mg of zinc, which is a solution (68), add 2 ml of the 2-methylquinolin-8-ol solution and mix. 70. the solution is diluted with 150 ml of distilled water, bring the temperature up to 60 ° C and, stirring constantly, add 45 ml 0.2 M ammonium acetate solution. 71. Stirring constantly, with 6% ammonia solution solution pH adjusted ranging from 5.7 to 5.9. The pH of the solution is measured by a pH meter. 72. The solution allow to stand 30 minutes. With the water pump filter through a G-4 filter Crucible, previously dried (150 ° C) and weighed after cooling (M0 grams), and wash the precipitate with 150 ml of distilled water at 95 ºc. 73. The Crucible causes the oven 150 ° C and dried for one hour. 74. Remove the Crucible from the drying Cabinet and in the desiccator, makes when it has cooled to room temperature, determine its mass (M1 grams). 75. the zinc content of the sample, as percentage by mass is calculated by the following formula:% zinc = M – which, in accordance with this annex 68 take the mass (in grams); M0 = empty and dry wash (72) mass (in grams); M1 – wash and sediment mass (in grams) (74). 76. One sample with approximately 1% of the mass of zinc content, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.1%. 4.4-hidroksibenzosulfoskāb-7 quantitative and qualitative determination of 77.4-hidroksibenzosulfoskāb quantitative and qualitative method of determining the procedure 4-hydroxybenzenesulphonic acid kvantit of the independent quality and determination of aerosols and face lotions. 78. The quantification of 4-hydroxybenzenesulphonic acid content of zinc 4-hydroxybenzenesulphonate in percentage by mass of the product. 79. The test portion is concentrated under reduced pressure, dissolved in water and purified by extraction with chloroform. Filtered water solution in aliquots of determination determination of 4-hidroksibenzolsulfoskāb. 80.4-hidroksibenzosulfoskāb-quantitative and qualitative method uses the following reaģentus1:80.1. concentrated hydrochloric acid, 36% (= 1,18). 80.2. Chloroform. 49.9. Butan-1-ol. 80.4. Glacial acetic acid. 80.5. potassium iodide. 50.1. potassium bromide. 80.7. sodium carbonate. 80.8. Sulphanilic acid. 80.9. Sodium nitrate. 80.10.0.1 n potassium bromate. 80.11.0.1 n Sodium Thiosulphate solution. 80.12. starch solution in water, 1% by mass. 80.13. sodium carbonate aqueous solution of 2% by mass. 80.14. aqueous solution of sodium nitrite, 4.5% by mass. 80.15. Dithizone in chloroform solution, 0.05% of the mass. 80.16. Developing solvent: Butan-1-ol/glacial acetic acid/water (4:1 volume: 5). Mix a separating funnel and discard the lower phase. 80.17. Pauly reagent, which is obtained as follows: dissolve 4.5 g sulfanil heating acid, 45 ml of concentrated hydrochloric acid and dilute the solution with water to 500 ml. Container with ice water to cool 10 ml of the solution and add 10 ml of cold sodium nitrite solution. Allow the solution to stand for 15 minutes at 0 ° C (in tempera in the solution is stable for tours from one day to three days) and immediately before spraying (87) add 20 ml of sodium carbonate solution. 80.18. Ready with cellulose coated plate (size 20 × 20 cm, thickness of the adsorbent layer 0.25 mm) thin layer chromatography. 81.4-hidroksibenzosulfoskāb-quantitative and qualitative method makes use of the following facilities and equipment: 81.1. Round-bottomed flask with ground glass stopper, 100 ml. 81.2. Separating funnel, 100 ml. 81.3. Conical flask with ground glass stopper, 250 ml. 81.4. Burette, 25 ml. 81.5. Graduated pipettes, 1, 2 and 10 ml. Graduated pipette, 5 ml 81.6.81.7. Microsyringe, 10 µl 0.1 µL with titles. 81.8. Thermometer graduated from 0 to 100 ° C. 81.9. Water bath, with a heating element. 81.10. Well ventilated drying oven set at 80 ° C temp is ratūr. 81.11. Standard equipment for thin layer chromatography. 82. Hydroxybenzenesulphonic acid for qualitative and quantitative determination of aerosols used balance resulting from aerosol containers of solvents and propellants by omitting the normal pressure evaporates. 7.1. Identification with a microsyringe makes 83.5 µ l (82) or the sample within six points on the starting line 1 cm from the lower edge of the thin-layer plate. 84. developing tank plate in Excess, which is already developing solvent, and develop until the solvent front has 15 cm from the starting line. 85. Remove the plate from the bath and dry at 80 ºc until no acetic acid vapour is perceptible. Spray the plate with sodium carbonate solution and dry in the air. 86. Half a plate covered with glass and covered part with 0.05% dithizone spray solution. Purple spots in the chromatogram indicates the presence of zinc ion. 87. Sprinkled the plate side covered with glass, and the other half sprayed with Pauly reagent. Chromatogram of 4-hydroxybenzenesulphonic acid the presence of Tan spot with shows about the Rf value turn on 3-0.26 hydroxybenzenesulphonic acid presence shows yellow spots with an Rf value of about 0.45.7.2. Determination 88. Weigh out 10 g of the sample or residue (82) 100 ml round-bottom flask on the Rotary evaporator and vacuum evaporate almost to dryness over a water bath kept at 40 ° C. 89. Pipette 10.0 ml pipette (V1 ml) water and dissolve by heating evaporation residue (88). 90. Quantitatively transfer the solution into a separating funnel and extract two times with 20 ml of aqueous solution of chloroform dose. After each extraction discard the form of chlorine. 91. Filter the aqueous solution through a fluted filter. Depending on the expected hydroxybenzenesulphonic acid content pipette 1.0 or 2.0 ml (V2) of filtrate 50 ml conical flask and dilute with water to the 75 ml. 92. Add 2.5 ml of hydrochloric acid 36% and 2.5 g of potassium bromide, mix and bring the temperature up to a water bath 50 ° C. 93. burette, add 0.1 n potassium bromate, solution, which is still 50 ° C temperature, turns yellow. 94. Add a further 3.0 ml of potassium bromate solution, stopper the flask and allow to stand for 10 minutes in a water bath. If after 10 minutes the solution loses its colour, add another 2.0 ml of potassium bromate solution, stopper the flask and heat for 10 minutes over a water bath kept at 50 ° c. Record the total potassium bromate solution added (a). 95. Cool the solution to room temperature, add 2 g of potassium iodide and mix. 96. The resulting iodine is titrated with 0.1 n Sodium Thiosulphate solution. The titration end stage, add a few drops of starch solution, which is the indicator. Record the quantity of Sodium Thiosulphate used (b). calculate the zinc hydroxybenzenesulphonate 97. content of the sample or residue (82) as a percentage by mass using the following formula:% zinc hydroxybenzenesulphonate = where (a) the overall added potassium bromate solution 0.1 n (94) quantity (ML); b – used for the back titration of Sodium Thiosulphate 0.1 n (96) quantity (ML); m-test or the balance of the product (paragraph 88) quantity (ML); V1 in accordance with this annex 89 for solution volume (ML); V2-analysis in the dissolved evaporation residue used (91) volume (ML). 98. as regards the results of the measurement of aerosols, indicate the balance (82) weight% of the initial quantity of the product. This calculation is based on aerosol sampling provisions. 99. One sample containing about 5% of the mass of zinc sulfonates hidroksibenzol, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.5% 4 100. Interpretation of results: in accordance with the provisions of annex 3, paragraph 19 of part I of zinc 4-hydroxybenzenesulphonate maximum level face lotions and deodorants is 6% by mass, and in addition the hidroksibenzolsulf acid content shall also determine the zinc content. Multiplying the calculated contents of zinc hidroksiben zolsulfonāt (97) by a factor of 0.1588, obtained the minimum zinc content in% mass, which, taking into account the specific hydroxybenzenesulphonic acid content, theoretically, should be the product. Zinc content that actually determines the risks gravime may be higher because of the cosmetic products you can also use the zinc chloride and zinc sulfate. 8. Oxidising agent identification and quantitative determination of hydrogen peroxide in hair-care preparations * persulphates, bromates 8.1 and hydrogen peroxide identification 101. sodium persulphate, potassium persulphate and ammonium persulphate, potassium bromate, sodium bromate and hydrogen peroxide, whether or not originating from barium peroxide, qualitatively detects the paper downward chromatography with two developing solvents. 102. Persulphates, bromates and hydrogen peroxide for qualitative detection uses the following reaģentus1:102.1. the connection of the mass by volume solution 0.75 for water: 102.1.1. Sodium persulphate. 102.1.2. potassium persulphate. ammonium persulphate. 102.1.3. 102.1.4. Potassium bromate. 102.1.5. sodium bromate. 102.1.6. Hydrogen peroxide. 102.2. Developing solvent A: 80% volume ethanol. 102.3. Developing solvent: benzene (B)/methanol/3-metilbutān-1-ol/water 34:38:18:10 (v/v/v/v). 102.4. Developing reagent A: 10 mass% potassium iodide solution. 102.5. Developing reagent B: 1 mass% starch solution in water. 102.6. Developing reagent C: 10% hydrochloric acid. 102.7.4 n hydrochloric acid. 103. Persulphates, bromates and hydrogen peroxide for qualitative determination of the use of such facilities and equipment: 103.1. Chromatography paper (vatmaņpapīr No 3 and no 4 or equivalent). 103.2. Micropipette, 1 µ l. Volumetric flasks, 100 ml 103.3.. 103.4. Fluted filter. 103.5. equipment of paper chromatography for top down. 104. Water-soluble cosmetics samples prepared from each sample prepare two solutions by dissolving 1 g and 5 g in 100 ml of the product water. Paper chromatography (107) uses 1 µ l of each solution. 105. The water partially soluble cosmetic sample shall be prepared as follows: 105.1. Weigh 1 g and 5 g of the sample and disperse in 50 ml of water, make up to 100 ml with water and mix. Both variances filter through a pleated filter and 1 µ l of each of the filtrate using paper chromatography (107). 105.2. Prepare two variances from each sample, dispersing 1 g and 5 g in 50 ml of water, acidify with dilute hydrochloric acid, make up with water to 100 ml and mix. Both variances filter through a pleated filter and 1 µ l of each of the filtrate using paper chromatography (107). 106. the sample is prepared, the Cream of each cosmetic product 5 g and 20 g 100 ml water, dispersing and variance using paper chromatography (107). 107. the paper chromatography of persulphates, bromates and hydrogen peroxide for qualitative determination shall be carried out in the following order: 107.1. appropriate solvent A (102.2) and B (102.3) into two separate chromatography tank to make the paper downward chromatography. Chromatographic tank for at least 24 hours with solvent vapour to saturate. 107.2 the starting point each on chromatography paper (vatmaņpapīr No 3 or equivalent) (103.1) bar, which is 40 cm long and 20 cm wide, or other appropriate size, makes 1 µ l of one sample solution and of one reference solution prepared according to this annex, 104, 106 and 105 102.1., and evaporate the solution in air. 107.3. Chromatography Strip (107.2) causes the chromatography tank filled with developing solvent A (107.1) and develop until the solvent front has advanced 35 cm for (about 15 hours). 107.4. Repeats of this annex and paragraph 107.2.107.3. the proc is described with chromatography paper fist (vatmaņpapīr No 4 or equivalent) and developing solvent b. Perform chromatography until the solvent front has moved about 35 cm (about five hours). 107.5. After development remove the chromatograms and dry in the air. 107.6. Spots develop the chromatogram by spraying it successively: 107.6.1. Developing the reagent A (102.4) and after a short while with developing the reagent B (102.5). First appears in the chromatogram persulphates spots, then hydrogen peroxide spots. The spots marked with a pencil. 107.6.2. Developing the reagent C (102.6) obtained in accordance with this 107.6.1. of the annex. On the presence of bromates show greyish blue spots in the chromatogram. 107.7. With the above conditions relating to developing solvents A (102.2) and B (102.3), reference (102.1) Rf values are approximately as follows: developing solvent A (102.2) developing solvent B (102.3) sodium persulphate, potassium persulphate 0.40 0.02 + 0.40 0.10 0.05 a 0.50 0.10 0.20 ammonium persulphate + Sodium bromate Potassium bromate + 0.40 0.20 0.40 0.10 0.20 hydrogen peroxide of barium peroxide 0.80 0.80 8.2. identification 108. when the sample (105) in skābināt After the hydrogen peroxide form the fucking and the presence of barium ions high-quality barium peroxide is determined in the following order: 108.1. If not the persulphates (8.1. subchapter), then adding dilute sulphuric acid in the acid sample solution dose (111.1), a white precipitate of barium sulphate. The presence of barium ions in the sample (111.1) again confirms the paper chromatography in accordance with this annex, paragraph 112. 108.2. If you have both barium peroxide and persulphates (111.2), then the remainder of the solution (111.2) cracking in alkali. After the dissolution in hydrochloric acid to melt in the presence of barium ions in solution (111.2.3) confirms the paper chromatography and (or) deposition of barium sulphate. 109. Barium peroxide for qualitative detection uses the following reaģentus1:109.1. Methanol. 109.2. concentrated hydrochloric acid, 36% (m/m). 109.3.6 n hydrochloric acid. 109.4.4 n sulphuric acid. 109.5. of 109.6. Rhodizonic acid disodium barium chloride (BaCl2 · 2H2O). 109.7. Anhydrous sodium carbonate. 109.8. Barium chloride 1% solution in water. 109.9. Developing solvent: methanol/hydrochloric acid (36%) of concentrate/water 80:10:10 (v/v/v). 109.10. Developing reagent: 0.71% (m/v) solution of rhodizonic acid disodium, prepared just before use. 110. Barium peroxide qualitative determination of the use of such facilities and equipment: 110.1. Micropipette, 5 µ l. 110.2. Platinum crucibles. 110.3.100 ml volumetric flask. 110.4. Chromatography paper (Schleicher and Schüll Ashless 2,133 b or equivalent). Clear the paper, developing chromatography tank (103.5), which contains the developing solvent (109.9), and dry. 110.5. Fluted filter. 110.6. Normal apparatus for ascending paper chromatography. 111. the quality of barium peroxide determination prepare the following: 111.1. Cosmetic products do not contain: 111.1.1 persulphate. Disperse 2 g of the product in 50 ml of water and with hydrochloric acid (109.3) adjust the pH of the variance around to 1.111.1.2. Transfer the variance to 100 ml volumetric flask, make up to the mark with water and mix. Variance using paper chromatography analysis (112) and qualitative determination of barium by precipitation of the sulphate. 111.2. Cosmetic products containing persulphates: 111.2.1. Disperse 2 g of the product 100 ml water and filter. 111.2.2. the Dried residue is added to sodium carbonate (109.7. bottom) whose mass is 7-10 times less than that of the mass balance, mixed and the mixture an hour melt Platinum crucible. 111.2.3. Cool to room temperature, dissolve in 50 ml of water and the melt filter (110.5). 111.2.4. Melt the residue dissolved in hydrochloric acid (109.3) and make up with water to 100 ml. Solution using a paper chromatographic analysis (112) and qualitative determination of barium by precipitation of the sulphate. 112. qualitative determination of barium peroxide is carried out in the following order: 112.1. The quantity of developing solvent (109.9) transfer to paper chromatography tank upward and saturates the camera at least 15 hours. 112.2. chromatographic paper, previously treated in accordance with this annex, 110.4. three starting points makes 5 µ l of each solution, drawn up in accordance with this annex, 111.1.2., 111.2.4. and and stan dartšķīdum (109.8). air dry the sample 112.3. and standard solution spots. Develop the chromatogram until the solvent front has ascended 30 cm. 112.4. removed from the chromatogram and air-dried. Spray the paper with 112.5. developing reagents (109.10), develops spots in the chromatogram. The presence of barium in the chromatogram appears red spots with an Rf value of about 0.10.8.3. determination of hydrogen peroxide by iodometry 113. Hydrogen peroxide quantification is based on the following reaction: H2O2 + 2 h + + 2I-I2 + 2H2O. The reaction is slow, but can be accelerated by adding ammonium molybdate. Put down the titrimetrisk iodine with Sodium Thiosulphate, and it is the hydrogen peroxide content measured. 114. The hydrogen peroxide content measured in accordance with this annex, 115, 116, 117, 118 and 119 of the product expressed as a percentage by mass (% m/m). 115. The hydrogen peroxide quantification using reaģentus1:115.1.2 n sulfuric acid. 115.2. potassium iodide. 115.3. Ammonium molybdate. 115.4.0.1 n Sodium Thiosulphate. 115.5.10% (m/v) potassium iodide solution prepared immediately before use. 115.6. Ammonium molybdate solution, 20% (m/v). 115.7. starch solution, 1% (m/v). 116. The hydrogen peroxide quantification using such facilities and equipment: 116.1.100 ml beakers, 116.2. Burette, 50 ml. 250 ml 116.3. volumetric flasks, measuring cylinders, 25 116.4.. and 100 ml. 116.5. one mark pipettes, 10 ml. 116.6. Conical flasks, 250 ml. 117. Hydrogen peroxide quantification is performed in the following order: 117.1.100 ml beaker weigh out 10 g (m gram) of the product containing 0.6 g of hydrogen peroxide. Transfer the contents of the beaker to a 250 ml volumetric flask, make up to the mark with water and mix. 117.2. Pipette 10 ml of the sample solution (117.1) 250 ml conical flask (116.6) and add successively 100 ml of 2n sulphuric acid (115.1), 20 ml of potassium iodide solution (115.5) and three drops of ammonium molybdate solution (115.6). 117.3. Iodine formed immediately Titrate with the 0.1 n Sodium Thiosulphate solution (115.4) and just before the end point as indicator adds a few millilitres of starch solution (115.7). Registers the 0.1 n Sodium Thiosulphate (115.4) consumption in millilitres (V). 117.4. in accordance with this annex and paragraph 117.2.117.3. blank test, carried out in 10 ml sample solution instead of using 10 ml of water. 0.1 n sodium recorded Thiosulphate in the blank in the analysis of consumption (Vo ml). 118. Calculate the hydrogen peroxide content of the product as a percentage by mass (% m/m), using the formula:% hydrogen peroxide = (((V-Vo) × 1.7008 × 250 × 100)/(w × 10 × 1000)) or% hydrogen peroxide = (((V-Vo) × 4,252)/(m)), where m-test cosmetics (117.1) quantity (in grams); Vo-consumption of Thiosulphate solution 0.1 n (ML) in the blank analysis (117.4); V – consumption of Thiosulphate solution 0.1 n (ML) sample solution titration (117.3). 119. If the hydrogen peroxide content of the product is approximately 6%, from the same sample, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.2%. 4 * note. Hydrogen peroxide in cosmetic products by iodometry can be determined only if they contain no other oxidizing agents that form iodine from iodides. So before the quantitative determination of hydrogen peroxide by iodometry, qualitatively and quantitatively all other existing product oksidējošo agents. Identification takes place in two stages-first down, bromate and persulphates hydrogen peroxide and the second defines the barium peroxide. 9. the quality of some oxidizing colouring and semi-quantitative determination of hair dyes of Oxidizing colouring quality 120. and semi-quantitative determination of hair dyes are applied to the qualitative and semi-quantitative determination of creamy or liquid hair color: symbol of the substance in the substance o-Phenylenediamine (OPD) m-Phenylenediamine (CPA) p-Phenylenediamine (PPD) metilfenilēndiamīn 4-methyl-1.2-Phenylenediamine (toluene-3.4-diamine) (OTD) 4-methyl-1.3-Phenylenediamine (toluene-2.4-diamine) (MTD) 2-methyl-1.4-Phenylenediamine (toluene-2 5-diamine (RTD) diaminofenol of 2.4)-diaminofenol (DAP) 1.4-hydroquinone (H) benzēndiol α-naphthol (a-N) pyrogallol 1, 2, 3 – hidroksibenzol (P) resorcinol 1.3-dihidroksibenzol (R) 121. Oxidation colorants pH 10 level with 96% ethanol extracted from a creamy or liquid hair colors and high quality down cream or two-dimensional thin-layer chromatography. This substance detection, semi-quantitative sample chromatogram in four developing systems compared with simultaneous and similar circumstances obtain reference chromatograms. 122. Oxidising colouring agents for qualitative and semi-quantitative determination of hair colors, use the following reaģentus1:122.1. Ethanol, anhydrous. 122.2. Acetone. 122.3. Ethanol, 96% (v/v). 122.4. Ammonia solution, 25% (d204 = 0,91). 122.5. L (+)-Ascorbic acid. 122.6. Chloroform. 122. Cyclohexane. 122.8. Nitrogen, technical. 122.9. Toluene. 122.10. Benzene. 122.11. n-butanol. 122.12.2-butanol. 122.13. Fosforpaskāb, 50% (v/v) solution. diazo reagent 122.14.: 3-Nitro-1-benzenediazonium hlorbenzolsulf the extended (stabilized salt form) as in Red 2 JN-Francolor or 2-chloro-4-Nitro-1-benzene diazonium naphthalenebenzoate (stabilized salt form) as in NNCD reagent No 74 150 Fluka, or equivalent. 122.15. Silver nitrate. 122.16. p-dimethylaminobenzaldehyde. 122.17.2.5-dimetilfenol. 122.18. iron (iii) chloride hexahydrate. 122.19. Hydrochloric acid, 10% (m/v) solution. 122.20. Reference substances referred to in paragraph 120 of this annex. Amine compound reference standard is the hydrochloride (mono-or di-) or free base. 122.21. Reference solutions 0.5% (m/v): 122.21.1. Prepare all of this annex referred to 122.20. Standart substance 0.5% (m/v) solution. 122.21.2. Weigh 50 ± 1 mg standard 10-ml volumetric flask. 122.21.3. Add 5 ml of 96% ethanol (122.3) and 250 mg Ascorbic acid (122.5). 122.21.4. to the solution should be alkaline, add ammonia solution (122.4) providing pH 10 (test with indicator paper). 122.21.5. Make up to 10 ml with 96% ethanol (122.3) and mix well. 122.21.6. Solution can be stored for a week in a dark, cool place. 122.21.7. In some cases, after the Ascorbic acid and the ammonia will add my precipitate the nas can be formed. Before analysis, sediment allow to stand. 122.22. Developing solvents. Developing solvents containing ammonia, immediately before use should be shaken: 122.22.1. Acetone/chloroform/toluene 35:25:40 (v/v/v). 122.22.2. Chloroform/cyclohexane/absolute alcohol/25% ammonia 80:10:10:1 (v/v/v/v). 122.22.3. Benzene butane-2-ol//water 50:25:25 (v/v/v). Shake well and after separation at room temperature (20 – 25 ° C), use the upper phase. 122.22.4. n-butanol/chloroform/reagent M 7:70:23 (v/v/v). At room temperature (20 – 25 ° C) carefully separate and use the lower phase.

Reagent preparation M ammonia solution, 25% (v/v) 24 v v.

Fosforpaskāb, 50% (122.13) 1 v. v.

Water 75 vol. v.

122.23. Developers: 122.23.1. Diazo reagent. Prepare the appropriate reagent 5% (m/v) solution in water (122.14). Solution must be prepared immediately before use the horse. 122.23.2. Ērlih reagent. Dissolve 2 g p-dimethylaminobenzaldehyde (122.16.) 100 ml of 10% (m/v) hydrochloric acid solution in water (122.19. below). 122.23.3.-dimetilfenol 2.5-iron (iii) chloride hexahydrate: the first solution: dissolve 1 g of dimetilfenol (122.17) 100 ml of 96% ethanol (122.3). The second solution: dissolve 4 g of iron (iii) chloride heksahidrāt (122.18. bottom) 100 ml of 96% ethanol (122.3). The development of these two solutions are sprayed separately, first the first solution, then the second solution. 122.23.4. ammoniacal silver nitrate solution. 5% (m/v) solution of silver nitrate in water (122.15) add 25% ammonia (122.4. bottom) until the precipitate dissolves. This reagent must be freshly prepared before use the horse. Do not keep. 123. Oxidizing the colouring agent for qualitative and semi-quantitative determination of hair color uses the following equipment: 123.1. Normal laboratory equipment for thin layer chromatography: 123.1.1. Plastic or glass cover, which created so that chromatographic plate, carried a solution and drying are in a nitrogen atmosphere. This precaution is necessary so as to prevent some dye oxidizes. 123.1.2. Microsyringe, 10, 0.2 µ µ l with l section and a needle with a straight end or – better – 50 µ l automatic dispenser, which strengthens the rack so that the plate could hold nitrogen. 123.1.3. ready to Use 0.25 mm thick 20 × 20 cm of silica gel thin-layer plate (Macherey and Nagel, silica G-HR, which are plastic basis, or equivalent). 123.2. Centrifuge, 4000 RPM. 123.3. Centrifuge Tubes, 10 ml, with screw plastic cover, coated with PTFE or equivalent. 124. Oxidising colouring agents for qualitative and semi-quantitative determination of hair color out in the following order: 124.1. Test sample preparation is carried out as follows: 124.1.1. Remove the first 2 or 3 cm cream extruded from tube. 124.1.2. Previously rinsed with nitrogen in the centrifuge tube (123.3. bottom) makes 300 mg Ascorbic acid and 3 g cream or 3 g homogenized liquid. 124.1.3. Drop by drop, add 25% ammonia until the pH is 10.124.1.4. Make up to 10 ml with 96% ethanol (122.3). 124.1.5. Homogenize the nitrogen (122.8), stopper and centrifuge for 10 minutes with 4000 RPM 124.1.6. Use the supernatant. 124.2. Chromatography: 124.2.1. Spotting plates: 124.2.1.1. Nitrogen (122.8) on the plate (123.1.3) nine points situated about 1.5 cm from each other on the line, which is approximately 1.5 cm from the edge of the plate, deck 1 µ l of the standard solution of each of the above. 124.2.1.2. Standard solution spots deployed as follows: 1 2 3 4 5 6 7 8 9 R P H PPD DAP OTD CPA-a RTD OPD MTD 124.2.1.3. beyond the ninth N standard solution spots (CPA) Board respectively 2 µ l sample control solution obtained in accordance with this annex 124.1. section. 124.2.1.4. Wide there nitrogen (122.8) until the end of the chromatographic analysis. 124.2.2. Development: 124.2.2.1 Makes wide Chamber. previously flushed out with nitrogen (122.8), loaded with one of the four solvents (122.22. below) and develop at room temperature (20 – 25 ° C) in the dark until the solvent front has moved about 15 cm from the starting line. 124.2.2.2. Remove plate and dry at room temperature, nitrogen (122.8. below). 124.2.3. immediately spray the plate with one of the four solvents indicated in this annex in 122.23. 124.2.4. Identification. Compare the Rf values of the sample and the reference color with hromatografēt Rf value and color. This table I of the annex is the Rf values and colours for each of the reference substances depending on the solvent and the indicator. In case of doubt, the approval can sometimes reap with the spiking method, adding the reference to the solution of the sample extract. 124.2.5. the Semi-quantitative assessment. Visually compare all 124.2.4 of this annex in certain spots of the substances with the intensity of a standard range of concentrations. If one or more of the substances found in the sample concentration is in excess, the extract is diluted and the measurement repeated. Table I Rf values and colours produced immediately after development of the standard substance (122.20). Developing solvents developers Rf values for color (122.22.1) (122.22.2) (122.22.3) (122.22.4.) diazo reagent (122.23.1) Ērlih (122.23.2) reagent dimethyl phenol (122.23.3) (122.23.4.) OPD 0.62 0.60 0.30 0.57 AgNO3 pale brown – – pale brown CPA 0.40 0.60 0.47 0.48 purple brown yellow to pale brown, pale brown PPD 0.20 0.50 0.30 0.48 bright red brown purple grey * brown * 0.60 0.60 0.53 0.60 OTD pale orange, pale brown gray Brown MTD 0.40 0.67
0.45 0.60 reddish brown yellow brown black purple orange RTD 0.33 0.65 0.37 0.70 Brown * – 0 0.07 0.05 DAP gray brown orange purple brown orange purple 0.50 0.35 0.80 0.20 H-black * · N orange brown-violet 0.90 0.80 0.90 0.75 * black 0.37-0.67 0.05 Brown very pale purple very pale brown brown * orange * 0.50 0.37 0.80 0.17 pale violet very pale brown, pale brown notes. 1. the OPD only appears a little. To clearly differentiate it from, you must use the solvent OTD (122.22.3). 2. indicates the best color attīstījum.

125. two-dimensional thin-layer chromatography test carried out in the following order: 125.1. Two-dimensional chromatography procedure shall use the following additional standards and reagents: 125.1.1. β (β naphthol · · · 125.1.2. N). 2-aminophenol (OAP). 125.1.3.3-aminophenol (MAP). 125.1.4.4-aminophenol (PAP). 125.1.5.2-Nitro-1.4-Phenylenediamine (2-NPPD). 125.1.6.4-Nitro-1.2-Phenylenediamine (4-NOPD). From each additional standard or reagent, prepare a 0.5% m/v solution in accordance with this annex 122.21. section. 125.2. additional developing solvent ethyl acetate/cyclohexane is/ammonia solution, 25% 65:30:5 (v/v/v). 125.3. additional indicator system: the glass jar makes developing tank for thin-layer chromatography, add about 2 g of crystalline iodine and affix the camera cover. 125.4. Chromatography is performed in the following order: 125.4.1. To a thin layer plates (123.1.3) sorbent surface draws two lines (Figure 6). 125.4.2. Nitrogen atmosphere (123.1.1) 1-4 µ l extract (124.1) Board starting point 1 (Figure 6), which is 2 cm from the two sides. Extract depends on the intensity of the spots this annex described in chromatogram 124.2. 125.4.3. Among the points 2 and 3 (Figure 6) split the oxidation colorants identified or that deemed identified (124.2) (distance between points 1.5 cm). Deck 2 µ l of each of the reference solutions-except DAP, the deck 6 µ l. This activity is carried out nitrogen (125.4.2). 125.4.4. Starting point 4 and 5 (Figure 6) repeats this 125.4.3. of the annex referred to in action and there wide nitrogen to chromatography (distance between points 1.5 cm). 125.4.5. Rinse the chromatography tank with nitrogen (122.8) and pour into a suitable quantity of developing solvent (122.22.2). Extra wide (125.4.4) and in the dark develop the first Elution direction (Figure 6). Elute until the solvent front reaches the line marked on the plate (approximately 13 cm). 125.4.6. Remove the plate from the tank and forces the chromatography tank previously flushed out with nitrogen and steam for at least 60 minutes of eluent. 125.4.7. the test tube with a suitable quantity of eluent section (125.2. the bottom) place the camera that flushed out with nitrogen (122.8). Inside the Chamber (125.4.6) wide, rotated 90 ° and take the grāfij hromat in the other direction (in the dark) until the solvent front reaches the line drawn on the surface of the sorbent. Remove the plate from the tank and evaporate the eluent. 125.4.8. place the plate for 10 minutes in the chromatography tank with iodine vapour (125.3) and interpret two-dimensional chromatogram using the hromatografēt reference at the Rf values and colours (Rf values and colors listed in table II of this annex). To obtain maximum colouring of the spots, the chromatogram after developing a half hour left in the air. 125.4.9. in accordance with paragraph 125.4.8. of this annex the presence of oxidizing colouring agent completely can confirm by repeating 125.4.1. of this annex, 125.4.2., 125.4.3., 125.4.4., 125.4.5., 125.4.6., 125.4.7. and 125.4.8. the activities referred to in paragraph 1, and start adding to this annex referred to in paragraph 125.4.2. below extract 1 µ l 125.4.8. of this annex the reference referred to. If compared with the chromatogram obtained in accordance with this annex, paragraph 125.4.8 does not find any other spots, 125.4.8. of this annex) (described in the interpretation of the chromatogram is correct. (II) the reference color table by chromatography and developing with iodine vapour reference color after development with iodine vapour R P brown beige (a) · N violet β · Pale brown H n violet Brown CPA yellowish brown PPD violet Brown dark brown RTD MTD yellowish brown dark brown DAP ODA orange yellow brown CARDBOARD FOLDER violet Brown 2-4 Brown-NPPD NOPD Orange Figure 6 10. quality and Nitrite determination 10.1. Qualitative determination of nitrite quality 126. method of determining the procedure for the determination of the quality of nitrite in cosmetic products, particularly creams and pastes. 127. the presence of nitrite indicates a color of fenilhidr-2-aminobenzaldehīd area (Nitrin ®)-containing derivative. 128. qualitative determination of Nitrite using such reaģentus1:128.1. Dilute sulphuric acid: dilute 2 ml concentrated sulphuric acid (d204 = 1.84) with 11 ml distilled water. 128.2. Dilute hydrochloric acid: dilute 1 ml concentrated hydrochloric acid (d204 = 1.19) with 11 ml distilled water. 128.3. Methanol. aminobenzaldehīd-fenilhidrazon 2-128.4 (Nitrin ® reagent) solution in methanol: 2.0 g ® 128.4.1. Weigh Nitrin and transfer quantitatively to a 100 ml volumetric flask. 128.4.2. Drop by drop, add 4 ml of dilute hydrochloric acid (128.2. below) and shake. 128.4.3. Make up to the mark with methanol and mix until the solution is completely clear. 128.4.4. The solution is stored in a dark glass bottle (129.3). 129. qualitative determination of Nitrite uses the following equipment: 129.1. Beakers, 50 ml graduated flask, 100 ml 129.2.. 129.3. Dark glass bottle, 125 ml. Glass plate 129.4., 10 x 10 cm. 129.5. Plastic spoon. 129.6. filter paper, 10 x 10 cm. 130. qualitative determination of Nitrite is performed in the following order: 130.1. Part of the test sample evenly spread on glass plates (129.4) round that is not thicker than 1 cm. 130.2. Soak filter paper (129.6) sheet in distilled water. It imposes on the sample and pressed with a plastic spoon. 130.3. Wait for about one minute, and the center of the filter, drops two drops of dilute sulphuric acid (128.1), then two drops Nitrin ® solution (128.4). 130.4. In 5-10 seconds, remove the filter paper and look to the light of day. The presence of nitrite show purple coloration. If the nitrite content is low, the purple tint 5-15 seconds turns yellow. If nitrite is large, the color changes after only one to two minutes. Purple red color intensity and time in which it becomes yellow, can testify about the nitrite content of the sample.

10.2. Determination of nitrites 131. quantification method for determination of nitrite in cosmetic products. 132. With nitrite determination method of nitrite content is expressed as percentage by mass of sodium nitrite. 133. when the sample is diluted with water and clarified, nitrite seems to react with sulphanilamide and N-1-naphthylethylenediamine and 538 nm size get the color density. 134. the quantification of Nitrite method uses the following reaģentus1:134.1. Clarification reagents (may not be used for more than one week after preparation): 134.1.1. Carrez I reagent: dissolve 106 g of potassium cyanoferrate (II) k4fe (CN) 6 x 3H2O in distilled water and dilute with water to 1000 ml. 134.1.2. Carrez II reagent: dissolve 219.5 g of zinc acetate Zn (CH3CO) 2 x 2H2O and 30 ml of glacial acetic acid in distilled water and dilute with water to 1000 ml. 134.2. Sodium nitrite solution : 0.500 g of sodium nitrite dissolved in distilled water 1000 ml volumetric flask and dilute with water to the mark. Dilute 10.0 ml of this solution to a 500 ml. 1 ml of the solution to the last is equal to 10 mikrogr tions of NaNO2. 134.3.1 n sodium hydroxide solution. 0.2% sulphanilamide hydrochloride 134.4. solution: dissolve 2.0 g of sulphanilamide heated 800 ml of water. Cool and add 100 ml of concentrated hydrochloric acid. Dilute with water to 1000 ml. 134.5.5 n hydrochloric acid. 134.6. N-1-naftilreaģent: finished the day of use. Dissolve 0.1 g of N-1-naphthylethylenediamine dihydrochloride in water and dilute with water to 100 ml. 135. quantification of Nitrite method uses the following equipment: 135.1. Analytical balance. 135.2. volumetric flasks, 250, 500 and 1000, 100 ml. Graduated pipettes pipettes 135.3. or by sections. 135.4. Measuring cylinders, 100 ml. 135.5. Fluted filter without nitrite, diameter 15 cm. 135.6. Water bath. 135.7. Spectrophotometer with cuvettes 1 cm long. 135.8. pH meter. 135.9. Microburette, 10 ml. 250 ml beakers, 135.10.. 136. quantitative determination of Nitrite is performed in the following order: 136.1. With 0.1 mg weigh approximately 0.5 g (m gram) of sample zēt, homogen with hot distilled water quantitatively into a 250 ml beaker and make up for the approximately 150 ml with hot distilled water. On the half hour, place the beaker in a water bath at 80 ° c. During this time, occasionally shake. 136.2. Cool to room temperature and stirring sequentially add 2 ml of the carrez I reagent (134.1.1) and 2 ml of the carrez II reagent (134.1.2 below). 136.3. Add 1 n sodium hydroxide solution to adjust pH to 8.3 (use the pH meter). Content transfer quantitatively to a 250 ml volumetric flask and make up to the mark with distilled water. 136.4. Mix and filter through a fluted filter paper (135.5). 136.5. pipette (135.3) a suitable aliquot (V ml) part, but not more than 25 ml of clear filtrate pipette 100 ml volumetric flask and add distilled water to 60 ml. 136.6. mix, add 10.0 ml of sulphanilamide hydrochloride solution (134.4) and then 6.0 ml of 6 n hydrochloric acid (134.5). Mix and allow to stand for five minutes. Add 2.0 ml of N-1-naftilreaģent (134.6. below), mix and three minutes allow to stand. Dilute to the mark with water and mix. 136.7. Prepare a blank test, repeating this annex and 136.6. bottom 136.5. the operations referred to in point without N-1-naftilreaģent. 136.8. Size (135.7) under this annex, the bottom point of the resulting 136.6. the optical density of the solution to 538 nm, the standard using the blank solution (136.7). 136.9. From the calibration curve (136.10.) reads the sodium nitrite content in micrograms per 100 ml of the solution (m1 micrograms), which corresponds to the optical density of which is measured in accordance with this annex 136.8. section. using 10 mg to 136.10. ml sodium nitrite solution (134.2. the bottom), draws a calibration curve for sodium nitrite 0, 20, 40, 60, 80, 100 µ g concentration. 137. Calculate the sodium nitrite content of the sample, in percentage by mass using the formula:% NaNO2 = ((250 V) × 10-6 m1 × × (100/m)) = ((m1)/(V × m × 40)), where m-determination of the sample taken (136.1) mass (in grams); M1 – sodium nitrite contents (micrograms), established in accordance with this subparagraph annex 136.9.; V – used for measurements (in millilitres) of the filtrate (136.5). 138. From the same sample of 0.2% (m/m) content of sodium nitrite the difference between the results of two determinations in parallel should not exceed 0.005% of absolute vērtību4. 11. free formaldehyde qualitative and quantitative determination of Free formaldehyde 139. qualitative and quantitative methods of determination used to determine qualitative and quantitative presence of formaldehyde donors or not. It is applicable to all cosmetic products. 140. Quantitative determination by pentane-2.4-Dione Colorimetry applied when formaldehyde is used alone or in combination with other preservatives that are not formaldehyde donors. In this method of derivation time of formaldehyde donors split and go too high results (and associated polymerized formaldehyde). Liquid chromatography to separate the free formaldehyde. 141. The quantification of free formaldehyde content of the sample, in percentage by mass. 11.1 identification 142. Free and formaldehyde associated sulphuric acid medium shade of the Schiff's reagent pink or reddish purple. 143. free formaldehyde qualitative method uses the following reaģentus1:143.1. Magenta. 143.2. sodium sulphite, hydrated to 7h2o. 143.3. Concentrated hydrochloric acid (d = 1.19). 143.4. Sulphuric acid, about 1 M 143.5. Schiff's reagent: 100 mg magenta weigh a beaker and dissolved in 75 ml 80 ° C water. After cooling, add 2.5 g of sodium sulphite heptahydrate (Na2SO3 · 7h2o) and 1.5 ml of concentrated hydrochloric acid (d204 = 1,19). Make up to 100 ml (after two weeks this reagent should no longer be used). 144. free formaldehyde quality test is performed in the following order: 144.1. Weigh 2 g of the test sample in a 10-ml beaker. 144.2. Add two drops of 2n sulphuric acid and 2 ml of Schiff's reagent (using this reagent must be absolutely colourless). Shake and leave for five minutes. 144.3. If this annex referred to in paragraph 144.2. five minutes watching the pink or reddish-purple coloured, formaldehyde concentration in solution is in excess of 0.01% and is determined quantitatively, making this annex 11.2. bottom free referred to in sections and associated method and, if necessary, this section 11.3 of the annex to this procedure. 11.2. the General determination by pentane-2.4-Dione Colorimetry 145. Formaldehyde in the presence of ammonium acetate reacts with pentane-2.4-Dione, forming a 1.4-diacetil-3.5-dihidrolutidīn. It is extracted with Butan-1-ol and the size of 410 nm of the extract of the absorption level. 146. The General quantification with pentane-2.4-Dione Colorimetry using such reaģentus1:146.1. Anhydrous ammonium acetate. 146.2. concentrated acetic acid, d204 = 1.05.-2.4-Dione 146.3. Pentane (freshly distilled under reduced pressure 25 mm Hg 25 °-it should not be absorbed at 410 nm). 146.4. Butan-1-ol. 146.5. Hydrochloric acid, 1 m. 146.6. Hydrochloric acid, approximately 0.1 M sodium hydroxide, 146.7.1 m. 146.8. Dissolved starch, freshly prepared in accordance with the European Pharmacopoeia (1 g/50 ml water), 2nd Edition, 1980, I-VII-1-1. 146.9.37 – 40% (w/v) formaldehyde. 146.10. Iodine solution, 0.05 M 146.11. Sodium Thiosulphate solution, 0.1 M.-2.4-Dione 146.12. Pentane reagent (reagent is prepared immediately before use): 146.12.1.1000 ml volumetric flask to dissolve 150 g ammonium acetate, 2 ml pentane-2.4-Dione (freshly prepared, distilled under reduced pressure, it should not be absorbed at 410 nm) and 3 ml of glacial acetic acid. 146.12.2. Make up to 1000 ml with water (pH of solution about 6,4). 146.13. Reagent (146.12) without pentane-2.4-Dione. 146.14. Formaldehyde-standard: stock solution: 146.14.1.5 g 37-Valley 40% formaldehyde solution 1000 ml volumetric flask and make up to 1000 ml. 146.14.2. the strength of this solution as follows: remove 10.00 ml, add 25.00 ml of 0.1 n iodine solution and 10 ml of the sodium hydroxide solution. 146.14.3. Allow to stand for five minutes. 146.14.4. Add 11 ml of HCl and quantitatively determine the excess iodine with the Sodium Thiosulphate solution 0.1 n, using starch indicator solution. 1 ml of 0.05 M iodine solution absorbed is equivalent to 1.5 mg formaldehyde. 146.15. Formaldehyde-standard: diluted solution: a solution of formald hīd sequentially diluted with water 1/20 and then 1/100.1 ml of this solution contains about 1 mg of formaldehyde. Calculate the exact content. 147. The General quantification with pentane-2.4-Dione Colorimetry uses the following equipment: 147.1. standard laboratory equipment. 147.2. Phase separation filter of 1 p vatmaņpapīr (or equivalent). 147.3. Centrifuge. 147.4. Water bath temperature set to 60 ° c. 147.5. Spectrophotometer. 147.6. Glass cells with optical path lengths of 1 cm. 148. General quantitative determination by pentane-2.4-Dione Colorimetry is performed in the following order: 148.1. sample solution. 100-ml volumetric flask weigh to 0.001 g a quantity of test sample in g corresponding to a presumed approx 150 micrograms of formaldehyde in houses. Make up to 100 ml of demineralized water and mix well (S solution) (check the pH to near 7 pH. If not, dilute in the hydrochloric acid solution). 50 ml Erlenmeyer flask with a capacity of 10.00 ml S solution added 5.00 ml pentane-2.4,-Dione reagent and deminerl to zēt water to a final volume of 30 ml. 148.2. Reference solution. With the control solution test sample prevents a potential interfering effect of the background color. 50 ml Erlenmeyer flask, add 10.00 ml S solution, 5.00 ml reagent (146.13) and demineralized water to a final volume of 30 ml. 148.3. Blank test. A 50 ml Erlenmeyer flask add 5.00 ml pentane-2.4-Dione reagent-(146.12.), demineralized water to 30 ml. 148.4. Flasks (148.1., 148.2. and 148.3) shaken and directly immersed for 10 minutes in a water bath at 60 ° c. Allow to cool two minutes in the ice water bath. 148.5. Into a 50 ml separating funnels containing 10.00 ml of Butan-1-ol. Rinse each flask with 3 to 5 ml of water and use to add piltuvj content. Exactly 30 seconds the mixture vigorously. Let it decompose. the Filter cells through 148.6. phase-separating filter. You can centrifuge (5 minutes, 3000 rpm). the size of this annex 148.7.148.1 in the extract of the sample solution in a specified absorbance A1 at 410 nm and compared with the reference solution (148.2) extract. 148.8. Size blank absorbance A2 of the extract against Butan-1-ol (all 148.4 of this annex, 148.5., 148.6. and 148.7. activities referred to in subparagraph must be carried out within 25 minutes from the moment when the Erlenmeyer flasks are placed in the water bath at 60 ° C). 149. The calibration curve shall be the following: 149.1.50 ml Erlenmeyer flask 5.00 ml of the stock solution (146.15), 5.00 ml pentane-2.4-Dione reagent (146.12), make up to 30 ml with demineralized water. 149.2. Continue in accordance with this annex, 148.4, 148.6, 148.7 148.5 and 148.8., measure the absorbance against Butan-1-ol. Repeat the procedure with 149.3.10, 15, 20 and 25 ml of the diluted standard solution (146.15.). 149.4. value of zero moment is obtained in accordance with this annex 148.8. the procedure referred to in the paragraph below. 149.5. The calibration curve shall be established by deducting the value of zero moment from each absorbance obtained in accordance with this annex and section 149.1.149.3.. The funeral rule is in effect, if not exceeding 30 µ g formaldehyde. 150. Calculations performed in the following order: 150.1. Subtract A2 A1 and read off from the calibration curve (C) the quantity, in micrograms of formaldehyde test solution. 150.2. sample of formaldehyde content as a percentage by mass (% m/m) is calculated by the following formula: formaldehyde content in% = ((C)/(103 × m)), where m-mass of the test portion (in grams). 151. If formaldehyde content of 0.2% in the product is from a single sample, the difference between the results of two determinations in parallel should not exceed 0.005% for determination by pentane-2.4-Dione kolorometrij. 152. in accordance with this annex 11.3. subdivision of work referred to in the Act if the determination of free formaldehyde produces results that are greater than the maximum laid down in these provisions: 152.1 concentrations. 0,05 – 0,2% in the product not labelled. 152.2. Product, whether or not marked, concentration is greater than 0.2%. 11.3. Determination of the presence of formaldehyde donors 153. Separate formaldehyde into a yellow lutidīn derivatives via reaction with the pentane-2.4-Dione in a post-column reactor and the derivative obtained is determined by the absorption of 420 nm. 154. A quantitative approach in the presence of formaldehyde donors using such reaģentus1, 3:154.1. Anhydrous ammonium acetate. 154.2. concentrated acetic acid. Pentane-2.4-Dione 154.3. (kept in a 4 ° C). 154.4. Anhydrous disodium phosphate. 154.5.85% orthophosphoric acid (d = 1,7). 154.6. Metanols2. 154.7. Dichloromethane. 37-40% V 154.8 formaldehyde. 154.9. sodium hydroxide, 1 M hydrochloric acid, 154.10.1 m. 154.11. Hydrochloric acid, 0.002 M. 154.12. Freshly prepared starch dissolved (146.8). 154.13. Iodine solution, 0.05 M 154.14. Sodium Thiosulphate solution, 0.1 M. 154.15. Mobile phase: water solution of sodium phosphate (154.4), 0.006 M adjusted to pH 2.1 with orthophosphoric acid (154.5). 154.16. Post-column reagent: with 1000 ml volumetric flask dissolve 62.5 g ammonium acetate (154.1), 7.5 ml acetic acid (154.2. bottom) and 5 ml of the pentane-2.4-Dione (154.3). Make up with water to 1000 ml. hold reagent a dark place. The maximum storage period is three days at 25 ° c. Should not be a color change. 154.17. Formaldehyde-standard: stock solution: 154.17.1.37-Valley 10 g 40% formaldehyde solution into a 1000 ml graduated flask and make up to 1000 ml. 154.17.2. Formaldehyde solution strength shall be determined as follows: remove 5.00 ml; add 25.00 ml of the iodine solution and 10 ml of the sodium hydroxide solution. 154.17.3. Allow to stand for five minutes. 154.17.4. Add 11 ml of HCl and quantitatively determine the excess iodine with the Sodium Thiosulphate solution 0.1 n, using starch indicator solution. 1 ml of 0.05 M iodine solution absorbed is equivalent to 1.5 mg formaldehyde. 154.18. Formaldehyde-standard: diluted solution. Formal dehīd the standard solution diluted to 1/100 the stock solution in the mobile phase (154.15.). 1 ml of this solution contains about 37 mg formaldehyde. Calculate the exact content. 155. A quantitative approach in the presence of formaldehyde donors uses the following equipment: 155.1. standard laboratory equipment. 155.2. HPLC pump, without vibration. 155.3. Low, non-vibrating pump for the reagent (or a second HPLC pump). 155.4. Injector valve with 10 ml loop. 155.5. Post-column reactor with the following components: 155.5.1. One 1-litre flask of trīskakl. 155.5.2. One 1-litre flask heater. 155.5.3. two Vigreux columns with a minimum of 10 plates, two of which are cooled by air. 155.5.4. Stainless steel tube (for heat exchange) 1.6 mm, internal diameter 0.23 mm, length 400 mm. 155.5.5. Teflon tube 1.6 mm, internal diameter 0.30 mm, length 5 m (response loop). 155.5.6. One T-shaped part without any dead volume (valco or equivalent). 155.5.7. Three connections without dead volume or one post-column Applied Biosystem PCR coupling of 520 or equivalent fitted with a 1-ml reactor. 155.6. Membrane Filter, pore size 0.45 mm. is 155.7. SEP-PAKRI C18 cartridge or equivalent. 155.8. Ready columns: Bischoff hypersil RP 18 (type NC reference C 25.46 1805) (5 mm, length 250 mm, internal diameter 4.6 mm) or DuPont, Zorbax ODS (5 mm, length 250 mm, internal diameter 4.6 mm) or phase SEP, spherisorb, ODS 2 (5 mm, length 250 mm, internal diameter 4.6 mm). Bischoff K1 hypersil 155.9. Pirmskolonn of RP 18 (reference K1 G 6301 1805) (5 mm, length 10 mm, or equivalent). 155.10. Column and pre-column are connected to the Ecotub system (reference (A) 15020508 Bischoff) or equivalent. 155.11. Device (155.5) Kit, inject the volume of connections by saving the moment possible. In this case, the stainless-steel tube between the reactor outlet and the detector inlet is intended to cool the mixture prior to detection and quantification, the temperature in the detector is unknown but constant. 155.12. Visible UV detector. 155.13. Recorder. 155.14. Centrifuge. 155.15. ultrasonic bath. 155.16. Vibration type mixer (virpuļmaisītāj or equivalent). 156. the quantitative determination in the presence of formaldehyde donors made the following order: 156.1. Calibration Curve. It is produced by plotting peak heights that are formaldehyde-standard: diluted concentrations. Prepare the standard solutions, formaldehyde solution (154.18. bottom) diluted with the mobile phase (154.15.): 1.00 ml of solution 156.1.1. (154.18) diluted to 20.00 ml (about 185 mg/100 ml). 156.1.2.2.00 ml of solution (154.18) diluted to 20.00 ml (about 370 mg/100 ml). 156.1.3.5.00 ml of solution (154.18) diluted to 25.00 ml (about 740 mg/100 ml). 156.1.4.5.00 ml of solution (154.18) diluted to 20.00 ml (about 925 mg/100 ml). 156.1.1. Of this annex, 156.1.2, 156.1.3. and 156.1.4.. reference solutions referred to stand for one hour at laboratory temperature and must be freshly prepared. The linearity of the calibration curve is good for concentrations between 1.00 up to 15.00 mg/ml. Samples preparation carry out 156.2. in this order: 156.2.1. Emulsions (creams, make-up, kontūrzīmuļ). Stoppered 100-ml flask weigh to 0.001 g a quantity of test sample (m g) corresponding to a presumed quantity of 100 mg of formaldehyde. Add 20.00 ml dichloromethane are accurately measured and 20.00 ml hydrochloric acid. Mix with vibration mixer using an ultrasonic bath. Centrifugation is divided by two phases (3000 g for two minutes). Meanwhile, wash with 2 ml methanol cartridges, then conditioned with 5 ml of water. 4 ml of the aqueous phase of the extract through the conditioned multiannual drain cartridge, discard the first 2 ml and the next part is recovered. 156.2.2. Lotions, shampoos. 100 ml stoppered flask weigh to 0.001 g a quantity of test sample (m g) corresponding to a presumed quantity of formaldehyde of about 500 mg. Make up to 100 ml with the mobile phase (154.15.). This solution is filtered through a filter (155.6) and inject or pass through the cartridge (155.7), conditioned to this annex referred to in subparagraph 156.2.1.. All solutions injected immediately after preparation. 156.3. Chromatographic conditions: 156.3.1. Mobile phase flow rate of 1 ml/min 156.3.2. Reagent flow rate 0.5 ml/min. 156.3.3. total flowrate at the detector outlet 1.5 ml/min. 156.3.4. Inject 10 ml. of 156.3.5. Elution temperature. If the substance is difficult to decompose by phases, immerse the column in a bath of melting ice and wait for the temperature to stabilize (15-20 min). 156.3.6. Post-column reaction temperature 100 ° c. 156.3.7. Determination of 420 nm. 157. the entire chromatographic system and the pēckolonn be rinsed after use with water. If the system is not used for more than two days after rinsing with water must be rinsed with methanol. Through it before rekondicionēšan drain water, to avoid rekristalizācij. 158. the calculation as follows: emulsion-in accordance with 156.2.1. of this annex. Formaldehyde content in% (m/m): lotions, shampoos in this phase is the following formula:, where m-analyze the mass (in grams) (156.2.1); C – formaldehyde concentration mg/100 ml, read from the calibration curve (156.1). 159. One sample with a content of 0.05% of formaldehyde the difference between the results of two determinations in parallel should not exceed 0.001%. From a single sample with 0.2% of formaldehyde content, the difference between the results of two determinations in parallel should not exceed 0.005%, which is equivalent to 1.5 mg formaldehīda4. 12. determination of resorcinol in shampoos and hair lotions With resorcinol 160. method of determining the quantitative gas chromatography determination of resorcinol in shampoos and hair lotions. Method to use the samples with concentrations from 0.1 to 2.0%. 161. The quantification of resorcinol content of the sample, in percentage by mass. Resorcinol and 3.5-162. dihydroxytoluene, (5-methylresorcinol) added as an internal standard, are separated from the sample to TLC. Both the shed be isolated, scraping their spots from the thin layer plates and extracting with methanol. Finally the extracted compounds dried silil and determination of gas chromatography. 163. for the quantitative determination of Resorcinol using such reaģentus1:163.1. Hydrochloric acid, 25% (m/m). 163.2. Methanol. 163.3. Ethanol, 96% (v/v). ready to Use silica gel 163.4. TLC sheets (plastic or aluminium) with fluorescent lights. Deactivated as follows: 163.4.1. normal spray pre-coated silica sheets with water until glazed coating. 163.4.2. Apsmidzinātaj plates allow to air dry at room temperature for one to three hours. If the plate is not deactivated, irreversible adsorption silica can cause loss of resorcinol. 163.5. Developing solvent: acetone/chloroform/acetic acid 20:75:5 (v/v/v). 163.6. Resorcinol standard solution: dissolve 400 mg resorcinol in 100 ml of 96% ethanol (163.3) (1 ml corresponds to 4000 µ g resorcinol). 163.7. Internal standard solution: dissolve 400 mg 3.5-dihydroxytoluene (DHT) in 100 ml of 96% ethanol (1 ml corresponds to 4000 µ g DHT). 163.8. Standard: 100 ml volumetric flask, mix 10 ml of solution specified in this annex, and the 163.6.10 ml of the solution specified in this annex 163.7, make up to the mark with 96% ethanol and mix (1 ml corresponds to 400 g resorcinol and 400 µ µ g DHT). 163.9. Silylating agents: 163.9.1. N, O-bis (trimethylsilyl) trifluoracetamīd (bstfa). 163.9.2 hexamethyldisilazane (hmds).. 163.9.3. Trimethylchlorosilane (TMCS). 164. for the quantitative determination of Resorcinol uses the following equipment: 164.1. standard thin-layer and gas chromatography equipment. 164.2. Glassware. 165. the quantitative determination of Resorcinol is performed in the following order: 165.1. sample preparation: 165.1.1. Weigh accurately into a 150-ml beaker a test of the product quantity (m in grams), containing approximately 20 – 50 mg resorcinol. 165.1.2. Acidify with hydrochloric acid (163.1), until the mixture is acidic (requires approximately 2-4 ml), add 10 ml (40 mg DHT) of the internal standard solution (163.7) and mix well. Transfer to a 100 ml volumetric flask with ethanol (163.3), make up to the mark with ethanol and mix. 165.1.3. Approximately 8 cm long continuous line deck 250 ml (165.1.2) to a deactivated silica sheet (163.4. below). The line forms a narrow as possible. 165.1.4. in accordance with subparagraph 165.1.3. of this annex on the same plate of the standard 250 ml (163.8). 165.1.5. Two points on the starting line makes 5 ml of each solution specified in this annex and 163.7 in 163.6. to facilitate the development by locale. 165.1.6. Develop broad unsaturated Chamber filled with developing solvent specified 163.5. of this annex, until the solvent front reaches the line located 12 cm from the starting line. Usually requiring 45 minutes. Dry the plate and UV light (254 nm) determines the resorcinol/DHT area. Both compounds have roughly the same Rf value. With a pencil at 2 mm from the outer dark borders. This area is separated and each substance separately collect the sorbent 10 ml bottle. 165.1.7. Different adsorbent containing the sample and the absorbent containing the standard mixture: add 2 ml methanol and, stirring constantly, is extracted in one hour. Filter the mixture and repeat the extraction for another 15 minutes with 2 ml methanol. 165.1.8. Combined extracts and evaporate the night vacuum desiccator filled with a suitable desiccant. Do not heat. 165.1.9. (165.1.8. the Silil balances in accordance with subparagraph 165.1.9.1. of this annex or 165.1.9.2.: 165.1.9.1. To add 200 ml microsyringe bstfa (163.9.1) and leave the mixture in a closed vessel for 12 hours at room temperature. 165.1.9.2. With a microsyringe add successively 200 hmds ml (163.9.2 below) and 100 ml of TMC (163.9.3) and heated in a closed container in a bag you 30 minutes 60 ° C temperature. Cool the mixture. 166. Gas Chromatography is performed in the following order: 166.1. Chromatographic conditions: 166.1.1. Column provides the resolution R equal to, or better than, 1.5 If R = (((r2-r1) 2d ')/(w1 × w2)), where r1 and r2-two peak retention time (in minutes); W1 and w2-the same width at half peak (mm); (d) ' – a chart speed (in millimetres per minute). 166.1.2. the following shall be considered suitable column and Gas chromatographic conditions column material: stainless steel length 200 cm ~ 3 mm internal diameter by filling 10% OJ 17 on Chromosorb WAW 100 to 120 flame ionization detector temperature of 185 ° C column (closed) 250 ° C detector, 250 ° C carrier gas nitrogen flow ml/min 45.166.1.3 hydrogen and air flow follow the manufacturer's instructions. enter 1-3 166.2. ml of the solution obtained by gas chromatography under 165.1.9. of this annex. Each solution (165.1.9) five times, measure the peak areas, average and calculate the peak area ratio: S = peak area resorcinol/peak area DHT. 167. the concentration of Resorcinol in the sample, expressed as a percentage by mass (% m/m) is calculated using the formula:% resorcinol = (1/M) x (Sparaug/Sstandartmaisījum), where M-the amount of sample (g) (165.1.1.); Sparaug-sample solution for the average peak area ratio in accordance with 166.2.2. of this annex. Sstandartmaisījum – average of the standard area ratios in accordance with 166.2.2. of this annex. 168. From the same sample 0.5% resorcinol content, the difference between the results of two determinations in parallel should not exceed 0.025% of absolute vērtību4. 13. determination of Methanol in relation to ethanol or propan-2-ol With 169. quantitative determination of methanol in relation to ethanol or propan-2-ol method gas chromatography determine methanol in all types of media the Kosmas (including aerosols). You can determine the percentage concentration from 0 to 10%. 170. Methanol content shall be expressed as a percentage by mass of methanol in relation to ethanol or propan-2-ol. 171. The determination made by gas chromatography. 172. the quantitative determination of Methanol in relation to ethanol or propan-2-ol method uses the following reaģentus1:172.1. Methanol. 172.2. Ethanol, absolute. 172.3. Propan-2-ol. 172.4. Chloroform, first with water from the alcohol. 173. the quantitative determination of Methanol in relation to ethanol or propan-2-ol method uses the following equipment: 173.1. Gas Chromatograph with a catharometer spray patterns with flame ionization detector for non-aerosol samples. 173.2.100 ml volumetric flasks, pipettes, 173.3.2. ml, 20 ml, 0.1 ml Microsyringe of 100 173.4.0 and µ µ l l and 0-5 (spray models only) special airtight syringe with valve (Figure 5). 174. the quantitative determination of Methanol carried out in the following order: 174.1. Preparation of the sample: 174.1.1. Aerosol sampling in accordance with Chapter 2 of this annex and then analyzed by gas chromatography with 174.2.1. of this annex the conditions referred to in point. 174.1.2. The samples of cosmetic products that are sprays, taken in accordance with this annex, Chapter 2, and dilute with water to ethanol or propan-2-ol concentration is 1-2%, and then analyzed by gas chromatography with 174.2.2. of this annex the conditions referred to in point. 174.2. Gas Chromatography: 174.2.1. for the analysis of the sample Aerosol uses a catharometer: 174.2.1.1. The column is filled with 10% Hallcomid M18 on Chromosorb WAW 100 to 200 size. 174.2.1.2. The column must yield a resolution, R, equal to, or better than, 1.5 If R = ((2) ((d ' r2-d ' r1)/(w1 + w2))) where r1 and r2-two peak retention time (in minutes); W1 and w2-the same width at half peak (mm); (d) ' – a chart speed (in millimetres per minute). 174.2.1.3. This resolution allows you to ensure the following conditions are true: the column material stainless steel length 3.5 m diameter 3 mm power 150 mA catharometer carrier gas helium pressure 2.5 bar 45 ml/min flow temperature 150 ° C injector detector column camera 65 ° C peak area measurements can be improved by integrating electronic 174.2.2. non-aerosol Samples: 174.2.2.1. The column is filled with Chromosorb 105 or Porapak QS and used a flame ionization detector. 174.2.2.2. Column must yield a resolution, R, equal to, or better than, 1.5 If R = ((2) ((d ' r2-d ' r1)/(w1 + w2))) where r1 and r2-two peak retention time (in minutes); W1 and w2-it same width at half peak (mm); (d) ' – a chart speed (in millimetres per minute). 174.2.2.3. This resolution provides the following conditions column material: stainless steel length 2 m diameter 3 mm sensitivity elektrometr 8 × 10-10 a. carrier gas nitrogen gas pressure is 2.1 bar feed 40 ml/min auxiliary gas hydrogen pressure 1.5 bar flow 20 ml/min, temperature of 150 ° C injector detector 230 ° C column camera 120 – 130 ° C 175. standard timetable consists of the following: 175.1. Gas Chromatography under subparagraph 174.2.1. of this annex (Hallcomid M18 column) uses the following standard mixture (mixture prepared by measuring with pipettes but find the exact amount is determined by the weighing of the pipette or flask after each addition): percentage concentration (m/m%)
Methanol, ethanol or propan-2-ol (ml) chloroform, which adds such a volume of approximately 2.5% 0.5 ml of 5.0% 20 100 20 100 ml approx. 1.0% 7.5 ml approximately 1.5 2.0 10.0% 20 100 20 100 ml approximately in accordance with 174.2.1. of this annex shall enter the 2 to 3 ¶l into the chromatograph. A mixture of each peak area ratio (methanol/ethanol) or (methanol/propan-2-ol). Plot standard graph on x% methanol versus ethanol or propan-2-ol, on the y axis and the peak area ratio (methanol/ethanol) or (methanol/propan-2-ol). 175.2. Gas Chromatography under subparagraph 174.2.2. of this annex (Porapak QS or Chromosorb 105) uses the following standard mixture (in the bag you prepared, measured with a microsyringe and pipette, but the exact amount is determined by the weighing of the pipette or flask immediately after each addition): percentage concentration (m/m%)
Methanol, ethanol or propan-2-ol (ml) water, which adds such a volume of approximately 2.5% 50 2 100 ml approx. 5.0% 7.5% 100 2 100 ml approx. 150 2 100 ml approx. 10.0% 200 2 100 ml according to the 174.2.2. of this annex shall enter in hromatograf 2-3 ml. A mixture of each peak area ratio (methanol/ethanol) or (methanol/propan-2-ol). Plot standard graph on x% methanol versus ethanol or propan-2-ol, on the y axis and the peak area ratio (methanol/ethanol) or (methanol/propan-2-ol). 175.3. Standard graph must be a straight line. 176. From the same sample of methanol content of 5% relative to ethanol or propan-2-ol, the difference between the results of two determinations in parallel should not exceed 0.25% 4.14. Dichloromethane and 1,1,1-trichloro discovery 177. With dichloromethane and 1,1,1-trichloro detection method determines the dichloromethane (methylene chloride) and 1,1,1-trichloroethane (methyl chloroform) in all cosmetic products where it could be. 178. Dichloromethane and 1,1,1-trichloroethane content of the sample determined according to the dichloromethane and 1,1,1-trichloro-detection method is expressed as percentage by mass. 179. The use of dichloromethane and 1,1,1-trichloro-detection method using gas chromatography with chloroform as internal standard. 180. Dichloromethane and 1,1,1-trichloro detection method uses the following reaģentus1:180.1. Chloroform (CHCl3). carbon tetrachloride (CCl4) 180.2.. Dichloromethane (CH2Cl2) 180.3.. 180.4.1,1,1-trichloroethane (CH3CCl3). 180.5. Acetone. 180.6. Nitrogen. 181. Dichloromethane and 1,1,1-trichloro detection method uses the following equipment: 181.1. standard laboratory equipment. 181.2. Gas Chromatograph equipped with a catharometer. 181.3. transfer bottle, 50 to 100 ml (19). 181.4. gas spiedšļirc, 25, or 50 ¶l (19.2.2.). 182. Dichloromethane and 1,1,1-trichloro-test is performed in the following order: 182.1. Pressure not to sample: weigh accurately a sample into a conical flask with stopper. Enter the accurately weighed quantity equal to the advance of dichloromethane and 1,1,1-trichloroethane in sample quantities of chloroform as internal standard. Mix thoroughly. 182.2. Increased pressure sample: uses the method described in this annex, Chapter 2, but with the following refinements: 182.2.1. when the sample is transferred to the transfer bottle, it enters the chloroform (internal standard) in the amount equal to the advance of dichloromethane and (or) 1,1,1-trichloroethane in the sample. Mix thoroughly. Empty valve with 0.5 ml of carbon tetrachloride in the rinse. After drying, based on the difference, drawing the exact mass of the internal standard added. 182.2.2. when the syringe is filled with sample, clean the nozzle with nitrogen before entering the chromatograph would not remain in the balance. 182.2.3. check out after each sample valve surface and the swap device rinse several times with acetone (if necessary, using the injection syringe) and then carefully dried with nitrogen. 182.2.4. For each analysis measuring with two different transfer bottles, five measurements with each bottle. 183. Dichloromethane and 1,1,1-trichloro-: the chromatographic conditions of determining 183.1. Pirmskolonn conditions are as follows: 183.1.1. Pipe: stainless steel. 183.1.2. Length: 300 mm. Diameter: 183.1.3.3 or 6 mm. Packing: 183.1.4. the same substance, with full analytical column. 183.2. column stationary phase Hallcomid M 18 on form hromosorb. Column provides the resolution R equal to, or better than, 1.5, where: where r1 and r2-retention times (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). 183.3. Example. This column gives the desired results: column I II material stainless steel tube stainless steel pipe length 350 cm 400 cm diameter 3 mm 6 mm medium: hromosorb in WAW WAW-DMC-HP sieve analysis particle size particle size 100-120 60-80 stationary phase 10% Hallcomid M 18 M 18, 20% Hallcomid temperature can vary depending on the equipment functions. These examples it is set as follows: column I column II temperature: 65 ° C 75 ° C 150 ° C injector 125 ° C 150 ° C 200 ° detector (C) carrier gas: helium flow rate 45 ml/min 60 ml/min at 2.5 bar pressure injector 2 bar 15 ml 15 ml injection 184. To determine the response factor, a conical flask with stopper, prepare the following accurately weighed mixture : dichloromethane 30% (m/m), 1, 1, 1-trichloroethane 35% (m/m), chloroform 35% (m/m). 185. the calculation shall be effected in the following order: 185.1. Response Unit of substance p mass calculated in relation to a substance that is used as the internal standard. If the first substance is p, which CP – response factor; mp-its mass in the mixture; Around its peak area; the second substance is (a) where that-its response factor; Ma-its mass in the mixture; AA – its peak area, then:. For example, the following is obtained response (for chloroform: k = 1): dichloromethane: k1 = 0.78 ± 0,03 1,1,1-trichloroethane: k1 = 0.78 ± 0,03 185.2. the calculation.% (m/m) of dichloromethane and 1,1,1-trichloroethane in the test sample. Where: ma – enter the chloroform in the mass (in grams); Ms-test sample mass (in grams); AA-chloroform peak area; A1 – dichloromethane peak area; A2-1, 1, 1-trichloroethane peak area, then: 186. From a single sample with dichloromethane and (or) 1,1,1-trichloroethane content of 25% (m/m) the difference between the results of two determinations should not exceed 2.5% (m/m), 4.15. Quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate evidence and discovery. With 187 quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate and detection method of proof and determination of quinolin-8-ol and its sulphate. 188. Certain quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate content of quinolin-8-ol expressed as a percentage by mass. 189. the quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate demonstrated by thin-layer chromatography and determined by the complex spectrophotometry 410 nm, obtained by reaction of fehling's solution. 190. the quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate and method of proof uses the following reaģentus1:190.1. Quinolin-8-ol. 190.2. the benzene. Whereas benzene is toxic, it should work particularly carefully. 190.3. Chloroform. 190.4. Sodium hydroxide solution, 50% (m/m). 190.5. Copper sulphate pentahydrate. potassium 190.6. sodium tartrate. 190.7.1 M hydrochloric acid. 190.8.0.5 M sulphuric acid. 190.9. sodium hydroxide 1 M solution. 190.10. Ethanol. 190.11. Butan-1-ol. 190.12. Glacial acetic acid. 190.13.0.1 n hydrochloric acid. 190.14. Celite 545 or equivalent. 190.15. Standard solutions: Weigh 100 mg of 190.15.1. quinolin-8-ol 100 ml volumetric flask. Dissolve in a little sulphuric acid (190.8). Make up to the mark with sulphuric acid. Weigh 100 mg of 190.15.2. quinolin-8-ol 100 ml volumetric flask. Dissolve in ethanol. Make up to the mark with ethanol and mix. 190.16. Fehling's solution. Solution A: weigh 7 g of copper sulphate pentahydrate in a 100 ml volumetric flask. Dissolve a small amount of water. Make up to the mark with water and mix. Solution B: weigh 35 g of potassium sodium tartrate 100 ml volumetric flask. Dissolve in 50 ml of water. Add 20 ml of sodium hydroxide (190.4). Make up to the mark with water and mix. Just before use, pipette 10 ml of solution A and 10 ml of solution B to 100 ml volumetric flask. Make up to the mark and mix. 190.17. Eluent for thin layer chromatography: 190.17.1. Butan-1-ol/acetic acid/water 80:20:20 (v/v/v). 190.17.2. Chloroform/acetic acid 95:5 (v/v). 190.18.2.6-Dichloro-4-(hlorimin) cikloheks-2.5-dienon, 1% (m/v) solution in ethanol. 190.19. sodium carbonate, 1% (m/v) solution in water. 190.20. Ethanol, 30% (v/v) solution in water. 190.21. dihidrogēnetilēndiamīntetraacetāt disodium, 5% (m/v) solution in water. 190.22. Buffer solution, pH 7: weigh 27 g anhydrous potassium dihidrogēnort phosphate and 70 g of DIPOTASSIUM hydrogenorthophosphate trihydrate graduated one-litre flask. Make up to the mark with water. 190.23. Ready for thin plate, of a thickness of 0.25 mm (e.g. Merck Kieselgel 60 or equivalent) before use, spray with 10 ml of reagent (190.21) and dry at 80 ° c. 191. the quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate and method of proof uses the following equipment: 191.1. Round-bottomed flask with ground glass neck, 100 ml volumetric flasks. 191.2. 191.3. Graduated pipettes, 10 and 5 ml pipettes, 191.4.20, 15, 10 and 5 ml. 191.5. Separating funnel, 100, 50 and 25 ml. 191.6. Fluted filter paper, diameter 90 mm. 191.7. Rotary evaporator. 191.8. Reflux condenser with ground glass neck. 191.9. Spectrophotometer. 191.10. Cells with a 10 mm optical path length. 191.11. Mixer with electric heating. 191.12. Glass chromatography column dimensions: 160 mm long with a diameter of 8 mm, narrow constriction, which is glass-fibre Plug and adapter to the top of the pressure. 192. the quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate was performed in the following order: 192.1. liquid samples: 192.1.1. part of the test sample is adjusted to pH 7.5 and 10 μl spotted on preprocessed silica gel thin-layer plate (190.23) starting line. 192.1.2. Standard solution (190.15.2) 10 and 30 ¶l spotted on two more points of the starting line, then develop the plate in one of the two Eluents (190.17). 192.1.3. when the solvent front has moved about 150 mm, 110 ° C dry (15 minutes). UV light (366 nm) inolīn-8-ol spots fluoresce yellow. 192.1.4. Spray the plate with sodium carbonate solution (190.19. below). Dry and sprayed with 2.6-Dichloro-4-(hlorimin) cikloheks-2.5-dienon solution (190.18). Quinolin-8-ol becomes visible as blue spots. 192.2. Solid/dry samples or creams: 192.2.1. Disperse 1 g of sample in 5 ml of buffer solution (190.22). Then, transfer 10 ml of chloroform to the funnel and shake. After the separation of the chloroform layer the aqueous layer is extracted twice more with 10 ml of chloroform. Combined and izfiltrēto in chloroform extracts almost completely evaporate 10 ml round-bottom flask on the Rotary evaporator. Dissolve the residue in 2 ml of chloroform and 10 and 30 ¶l of the solution obtained on a silica gel thin-layer deposit plate (190.23) according to this annex referred to 192.1. method. 192.2.2. On the plate carrying the 10 and 30 ¶l of standard solution (190.15.2 below) and continues under this annex, 192.1.2, 192.1.3 and 192.1.4. below. points. 193. the quinolin-8-ol and bis (8-hydroxyquinolinium) sulphate test is performed in the following order: 193.1. liquid samples: 193.1.1. Weigh 5 g of the sample into a 100 ml round-bottom flask. Add 1 ml of sulphuric acid solution (190.8) and evaporate until the mixture almost to dryness under reduced pressure at 50 ° C. 193.1.2. Dissolve the residue in 20 ml of warm water. Transfer to a 100 ml volumetric flask. Wash three times with 20 ml of water. Make up to 100 ml with water and mix. 193.1.3. Pipette 5 ml of this solution into a 50 ml separating funnel. Add 10 ml of fehling's solution (190.16). Extract the quinolin-8-ol copper complex [oxine copper (ISO)] obtained with three times 8 ml of chloroform. 193.1.4. Filter and collect the chloroform layer into a 25 ml graduated flask. Make up to the mark with chloroform and shake. Determine the optical density of the yellow solution against chloroform 410 nm 193.2. Solid/dry samples or creams: Weigh 0.500 g of the sample 193.2.1.100 ml round-bottom flask (191.1). Add 30 ml of benzene and 20 ml hydrochloric acid (190.7). Using a reflux condenser, boil, stirring the contents of the flask for 30 minutes. 193.2.2. The contents of the flask into a 100 ml separating funnel. Rinse with 5 ml of 1 N HCl. Transfer aqueous phase to a round-bottomed flask and wash the benzene phase with 5 ml of hydrochloric acid. 193.2.3. If further treatment interfere with emulsion 0.500 g of the sample, mix with 2 g of Celite 545 (190.14), to form the free-flowing powder. In small doses the mixture into a glass chromatography column (191.12. below). After each addition, tamp the column packing. As soon as all the mixture is transferred to the column, elute with hydrochloric acid (190.13) to acquire about 10 minutes 10 ml of eluate (if necessary, may elute the small nitrogen pressure). To ensure that eluted over the column filling process is little hydrochloric acid. The first 10 ml of eluate is further processed, in accordance with 193.2.4. of this annex. 193.2.4. The collected aqueous phases (193.2.2) or the eluate (193.2.3) with the Rotary evaporator to evaporate under reduced pressure to almost dryness. 193.2.5. Dissolve the residue in 6 ml of sodium hydroxide solution (190.9). Add 20 ml of fehling's solution (190.16) and the contents of the flask into a 50 ml separating funnel. Rinse the flask with 8 ml of chloroform. Shake well and filter the chloroform phase into a 50 ml graduated flask. 193.2.6. repeat the extraction three times with 8 ml of chloroform. Filters out chlorine to form phases and collect 50 ml flask. Make up to the mark with chloroform and shake. Size the optical density of the yellow solution against chloroform 410 nm. 194. Calibration Curve consists of the following: four 100 ml round-bottomed flask, each containing 3 ml of 30% aqueous ethanol (190.20), pipette 5, 10, 15 and 20 ml portions of the standard solution (190.15.1), corresponding to 5, 10, 15 and 20 mg of quinolin-8-ol. Then proceed in accordance with this annex 193.1. section. 195. The calculation shall be made in the following order: 195.1. liquid samples: quinolin-8-ol content (% m/m) =, where A-milligrams of quinolin-8-ol on the calibration curve (194); m-discovery of the sample taken (193.1.1) mass (in milligrams). 195.2. Solid/dry samples or creams: quinolin-8-ol content (% m/m) =, where a-milligrams of quinolin-8-ol on the calibration curve (194); m-discovery of the sample taken (193.2.1) mass (in milligrams). 196. If quinolin-8-ol content of about 0.3%, from the same sample, the difference between the results of two determinations should not exceed 0.02% of absolute vērtību4. 16. determination of ammonia With 197. method for the determination of ammonia down the free ammonia in cosmetic products. 198. the ammonia determination method of ammonia content of the sample as a percentage by mass of ammonia. 199. The test sample of the product, which dissolved in methanol – compare aqueous solution, add the barium chloride solution. By filtration or centrifugation separates the all precipitate. In this procedure, the distillation with water vapor, saves without loss of ammonia in some ammonium salts, for example, hidrogēnkar bonāt and fatty acids than the ammonium acetate. The ammonia is steam distilled from the filtrate or supernatant and determined by potentiometric titration or otherwise. 200. The ammonia method uses the following reaģentus1:200.1. Methanol. 200.2. Barium chloride dihydrate, 25% (m/v) solution. 200.3. Orthoboric acid, 4% (m/v) solution. 200.4. sulphuric acid, 0.25 M standard solution. 200.5. Anti-Foaming agent. 200.6. sodium hydroxide, 0.5 M solution. 200.7. The indicator light (if necessary): 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. 201. The ammonia method uses the following equipment: 201.1. standard laboratory equipment. 201.2.100 ml Centrifuge with stoppered bottle. 201.3. Equipment for distillation with water vapor. 201.4. Potentiometer. 201.5. indicating glass electrode and mercury (I) chloride (calomel) reference electrode. 202. The ammonia test is performed in the following order: 202.1.100 ml volumetric flask, weigh the sample with the mass (m), corresponding to the maximum 150 mg of ammonia. 202.2. Add 10 ml of water and 10 ml methanol 10 ml of barium chloride solution (200.2). Make up to 100 ml with methanol 202.3. Mix and leave overnight in the refrigerator (5 ° C). 202.4. Then filters or 10 minutes in closed tubes centrifuge the still cold solution to obtain a clear filtrate or supernatant. 202.5. Pipette 40 ml of the supernatant solution equipment for distillation with water vapor (201.3), then, if necessary, 0.5 ml of antifoam. 202.6. Distilled and collect 200 ml of distillate 250 ml beaker containing 10 ml of sulphuric acid solution (200.4) and 0.1 ml of indicator (200.7. the bottom). 202.7. Titrate the excess of acid with the sodium hydroxide solution (200.6.). Potentiometric determination of 202.8. collect 200 ml of distillate in a 250 ml beaker containing 25 ml of orthoboric acid solution (200.3) and Titrate with the sulphuric acid solution (200.4) by recording the neutralization curve. 203. the calculation shall be effected in the following order: 203.1. the calculation of titration. Where: V1-spent sodium hydroxide solution (ML); M1 – its actual Molarity (200.6.); M2 – sulphuric acid solution (200.4) actual title; m-discovery of the sample taken (202.1) mass (in milligrams), then: ammonia,% (m/m) = 203.2. calculation of direct potentiometric titration, if carried out. Where: spent sulphuric acid solution-V2 is the volume (in ml); M2 – its actual Molarity (200.4); M-discovery of the sample taken (202.1) mass (in milligrams), then: ammonia,% (m/m) = 204. If the ammonia content of about 6%, the results of two determinations carried out in parallel on the same sample should not exceed the difference between the absolute vērtību4 0.6%. 17. the burden of proof and determination of Nitromethane 205. With Nitromethane and detection method of proof and determination of nitromethane, if the content is up to 0.3% in cosmetic products. 206. the Nitromethane content of the sample as a percentage by mass of ammonia aerosol balloons. 207. Nitromethane demonstrated by color reaction. Nitromethane is determined gas chromatographically after addition of the internal standard. 17.1.208. demonstration of Nitromethane Nitromethane was used the following reaģentus1:208.1. sodium hydroxide, 0.5 M solution. 208.2. Folin reagent: dissolve 0.1 g of sodium 3.4-dihydro-3.4-dioks-1-naphthalene sulfonate in water and dilute to 100 ml. 209. Nitromethane proof shall be made by adding 1 ml of the sample 10 ml 208.1. of this annex and point 1 of this annex, 208.2 ml. the substances referred to in (a). A violet coloration indicates the presence of Nitromethane. 17.2. determination of Nitromethane 210. determination of Nitromethane used the following reaģentus1:210.1. Chloroform (internal standard 1). 210.2.2.4-dimethylheptane (internal standard 2). 210.3.95% ethanol. 210.4. Nitromethane. 210.5. Chloroform solution: Tared 25 ml graduated flask approximately 650 mg of chloroform. Again, accurately weigh the flask and its contents. Make up to 25 ml with 95% ethanol. Weighed and calculated the percentage by mass of chloroform in this solution. 2.4-dimethylheptane 210.6. standard solution: solution of chloroform make up under this annex, but the 210.5.25 ml volumetric flask, weigh 270 mg 2.4-dimethylheptane. 211. determination of Nitromethane uses the following equipment: 211.1. Gas Chromatograph with a flame ionization detector. 211.2. the apparatus for sampling of aerosols (transfer bottle, microsyringe connectors of the away, etc.) in accordance with Chapter 2 of this annex. 211.3. Laboratory equipment. 212. the determination of Nitromethane in the following order: 212.1. Preparation of the sample: 100 ml of the solution in a steady transfer of the bottle eroded or exhausted in accordance with this annex 17, 18 and 19 above, the procedure of approximately 5 ml of the internal standard solution (210.5. or 210.6). Use a 10 or 20 ml glass syringe without needle, adapted to the swap device in accordance with this annex 17, 18 and 19 above. Reweigh to determine the amount you entered. With the same take on the bottle across Member into approximately 50 g of the sample, taken from the aerosol dispenser. Reweigh to determine the quantity of the sample transferred. Mix thoroughly. With a microsyringe (211.2) approximately 10 μl. Enter five times. 212.2. preparation of the Standard: weigh accurately into a 50 ml graduated flask approximately 500 mg and 500 mg of nitromethane, chloroform or 2.4-dimethylheptane 210 mg. Make up to the mark with 95% ethanol. Mix thoroughly. Transfer 5 ml of this solution to 20 ml volumetric flask. Make up to the mark with 95% ethanol. With a microsyringe (210.2) approximately 10 μl. Enter five times. 212.3. Gas chromatographic conditions: 212.3.1. Column has two parts: the first with didecilftalāt with Gas Chrom Q filling with Ucon 50 HB, 280 x with Gas Chrom Q filling. Prepared combined column must yield a resolution, R, equal to, or better than, 1.5, where: r1 and r2-retention times (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). For example, these two components provide the required resolution: column (A) material: stainless steel. Length: 1.5 m. diameter: 3 mm. Packing: 20% didecilftalāt on Gas Chrom Q (100-120). Column (B) material: stainless steel. Length: 1.5 m. diameter: 3 mm. Packing: 20% Ucon 50 HB 280 x on GasChrom Q (100-120). 212.3.2. appropriate flame ionization detector sensitivity elektrometr is 8 × 10-10 a. 212.3.3. Temperature: 212.3.3.1 ° C, Injector: 150.. 212.3.3.2. The detector: 150 ° C. 212.3.3.3. Column: 50 – 80 ° C depending on the respective column, and equipment. 212.3.4. Suitable gas: 212.3.4.1. Carrier gas: nitrogen. 212.3.4.2. Pressure: 2.1 bar. 212.3.4.3. Flow: 40 ml/min. detector supplies: 212.3.4.4. after detector manufacturer instructions. 213. the calculation shall be effected in the following order: 213.1. Nitromethane response factor, calculated in relation to the internal standard used. If Nitromethane denoted by n, then: CN-it response factor; m ' n – its mass (in grams) in the mixture; S ' n – its peak area. If the internal standard, chloroform or 2.4-dimethylheptane, denoted by c, then: m ' c-its mass (in grams) in the mixture; S ' c-peak area, and: (kn is a function of the equipment) 213.2. concentration of Nitromethane in the sample if the Nitromethane is denoted by n, then: CN-it response factor; SN-the peak area. If the internal standard, chloroform or 2.4-dimethylheptane, denoted by c, then: mc-its mass (in grams) in the mixture; SC-the peak area; M-ported aerosol mass (in grams) and Nitromethane% (m/m) in the sample is: 214. Nitromethane content of about 0.3% (m/m) of the results of two determinations carried out in parallel on the same sample should not exceed the difference between the absolute 0.03% (m/m) vērtību4. 18. proof and determination of mercaptoacetic acid Perm, hair straightening and depilatory products. With mercaptoacetic acid proof 215 and determination method and determination of mercaptoacetic acid Perm, hair straightening and hair removal products that may contain other reducing agents. 216. the mercaptoacetic acid content of the sample as a percentage by mass of mercaptoacetic acid. 217. Mercaptoacetic acid demonstrated by color reaction, making a thin layer of chromium and togrāfij determined by iodometry or gas chromatography. 18.1. the showing of mercaptoacetic acid by colour reaction with 218. proof of mercaptoacetic acid color reaction uses the following reaģentus1:218.1. Lead acetate paper. 218.2. Hydrochloric acid solution (one unit of volume of concentrated hydrochloric acid and one unit of volume of water). 219. proof of Mercaptoacetic acid by colour reaction is performed in the following order: 219.1. Mercaptoacetic acid proof color reaction with lead acetate: one drop of the sample to be analyzed on lead di(acetate) paper. If it's dyed bright yellow, then probably it is of mercaptoacetic acid. Sensitivity of 0.5%. 219.2. characterization of inorganic sulphides by the medium acidification: the formation of the tube enters a few milligrams of test sample. Add 2 ml of distilled water and 1 ml of hydrochloric acid (218.2). Sulphide, which occurs after the smell, and the lead acetate paper a black lead sulphide precipitate. Sensitivity 50 ppm. 219.3. characterization of Sulphites by the formation of sulphur dioxide acidifies: Act in accordance with this annex, 219.2. section. The boil. Sulphur dioxide is found after the fragrance and its reducing properties, for example, in relation to the permanganate ions. 18.2. the demonstration of Mercaptoacetic acid thin-layer chromatography for identification of mercaptoacetic acid 220. thin-layer chromatography using reaģentus1:220.1. Mercaptoacetic acid (tioglikolskāb), 98% minimum purity test by iodometry. 220.2.2,2 ' ditiod (acetic acid), at least 99% purity, by check by iodometry. 220.3.2-merkaptopropionskāb (tiopienskāb), at least 95%, by check by iodometry. 220.4.3-merkaptopropionskāb, at least 98% purity, the Jodo metric. 220.5.3-merkaptopropān-1.2-diol (1-tioglicerīn), at least 98% purity test by iodometry. 220.6. Ready 0.25 mm thick silica gel thin-layer plate. 220.7. Aluminium oxide, Merck F 254 E or similar thin-layer plate. 220.8. concentrated, = 1.19 g/ml hydrochloric acid. 220.9. Ethyl acetate. 220.10. Chloroform. 220.11. Diizopropilēter. 220.12. Carbon tetrachloride. 220.13. Glacial acetic acid. 220.14. Potassium Iodide, 1% (m/v) solution in water. 220.15. Platinum tetrachloride, 0.1% (m/v) solution in water. 220.16. Eluent: 220.16.1. Ethyl acetate, chloroform, diizopropilēter, acetic acid (20:20:10:10 v/v). 220.16.2. Chloroform, acetic acid (90:20 v. v.). 220.17. Developers: 220.17.1. Directly before use, mix equal quantities of solution (220.14) and solution (220.15). 220.17.2. Bromine solution, 5% (m/v). Dissolve 5 g of bromine 100 ml Tetra hloroglekļ. 220.17.3 fluorescein solution, 0.1.% (m/v). Dissolve 100 mg of fluorine ceīn 100 ml of ethanol. 220.17.4 heptamolybdate, 10 of the Heksaamonij.% (m/v) solution in water. 220.18. Standard solutions: 220.18.1. Mercaptoacetic acid (220.1), 0.4% (m/v) solution in water. 220.18.2.2, 2 '-ditiod (vinegar) acid (220.2), 0.4% (m/v) solution in water. 220.18.3.2-merkaptopropionskāb (220.3), 0.4% (m/v) solution in water. 220.18.4.3-merkaptopropionskāb (220.4), 0.4% (m/v) solution in water. 220.18.5.3-merkaptopropān-1.2-diol (220.5), 0.4% (m/v) solution in water. 221. the showing of mercaptoacetic acid is used in thin-layer chromatography TLC apparatus. 222. proof of Mercaptoacetic acid by thin layer chromatography is carried out in the following order: 222.1. Treatment of samples: acidify to pH 1 with a few drops of hydrochloric acid (220.8) and filter. In some cases it may be advisable to dilute the sample. In that case it before dilution, acidify with hydrochloric acid. 222.2. Elution: spotted on plate 1 µL of the sample solution (222.1. bottom) and one litre of each of the five reference solutions (220.18. below). Carefully dry the easy flow of nitrogen and elute the plate with solvents (220.16.1. or 220.16.2.). Dry the plate as quickly as possible to minimize the oxidation of thiols. 222.3. Development: spray the plate with one of the three reagents (220.17.1.220.17.3.220.17.4., or). If the plate is sprayed with reagent (220.17.3), then it is treated with bromine vapour (e.g. camera, which is a small beaker with reagent (220.17.2)) until the spots are visible. With detection reagents (220.17.4) has turned the rinoš only if the thin layer drying time shall not exceed 30 minutes. 222.4. Interpretation: compare the Rf values and standard color with standards. The table shows the average Rf values in rough salīdz to Morrow. They depend on the thin-layer chromatography of the State of the activation time and the temperature of the chromatography tank. The silica gel layer Rf value obtained examples for 220.16.1.220.16.2) (Eluent. subparagraph merkaptopropionskāb of the Mercaptoacetic acid 0.25 0.80 0.40 0.95 2-2, 2 '-ditiod (vinegar) acid 3-merkaptopropionskāb 0.00 0.35-0.45 0.95 3-merkaptopropān-1.2-diol 0.45 0.35 18.3. determination of Mercaptoacetic acid. 223. the determination to prevent oxidation, mercaptoacetic acid is determined not to use cosmetic feature taken from the newly opened container. Always start with the determination to detection. 224. Mercaptoacetic acid determined by oxidizing the-SH group with iodine in an acid medium according to the equation: 2 HOOC CH2SH + I2 (HOOC-CH2-S) 2 + 2 I-+ 2 H + 225. Mekaptoetiķskāb determination of iodine used in determination, 0.05 M standard solution. 226. for the determination of Mekaptoetiķskāb in determination of laboratory equipment to be used. 227. Mekaptoetiķskāb determination of the determination is carried out in the following order: accurately weigh 0.5-1 g of the sample into a 150 ml stoppered conical flask containing 50 ml of distilled water. Add 5 ml of hydrochloric acid (solution pH around 0) and Titrate with iodine solution (225) until the yellow coloration. Optionally, use the indicator (e.g. starch solution or carbon tetrachloride). 228. the mercaptoacetic acid content is calculated by the following formula:% (m/m) =, where m-test sample mass (in grams); n-iodine solution used in volume. If the calculation result of mercaptoacetic acid is 0.1% or more below the permitted maximum concentration, there is no need to continue. If the result is equal to or higher than the allowed maximum concentration and is found more proof, reducing agents, requires a determination by gas chromatography. 18.4. determination of Mercaptoacetic acid. Gas chromatography 229. Mercaptoacetic acid is separated from the excipient by precipitation with cadmium di(acetate) solution. After methylation with diazomethane, prepared in situ or in advance of diethyl ether solution of mercaptoacetic acid is measured by gas/liquid chromatography, as internal standard using methyl octanoate. 230. the determination of Mercaptoacetic acid by gas chromatography using the following reaģentus1:230.1., 98% Mercaptoacetic acid. 230.2. Hydrochloric acid, = 1.19 g/ml. 230.3. Methanol. 230.4. cadmium di(acetate) dihydrate, 10% (m/v) solution in water. 230.5. Methyl octanoate, 2% (m/v) solution in methanol. 230.6. Acetate buffer (pH 5): 230.6.1. Sodium acetate trihydrate, 77 g. 230.6.2. Acetic acid (glacial), 27.5 g. 230.6.3. Demineralized water, which make up to one litre. 230.7. Hydrochloric acid, freshly prepared 3 M solution in methanol. 230.8. the 1-methyl-3-Nitro-1-nitrozoguanidīn. 230.9. Sodium hydroxide, 5 M solution. 230.10. Iodine, 0.05 M standard solution. 230.11. diethyl ether. 230.12. Diazomethane solution prepared from N-methyl-N-nitrozotoluol-4-sulfonamide (Fieser, Reagent for Organic Synthesis (Wiley), 1967). The 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 in a strong draught and avoid ground glass equipment (for this purpose is particularly kits). 231. the determination of Mercaptoacetic acid by gas chromatography using such equipment. 231.1. Laboratory equipment. 231.2. equipment for the preparation of diazomethane for in situ methylation (Fal, H.M., T.M. and Babashak, Jaoun, J.F., analyt. Chem. in 1973, 45, 2302). 231.3. Equipment for the advance preparation of diazomethane (Fieser). 232. sample preparation determination of mercaptoacetic acid gas hromat the grāfij in the following order: 232.1. Weigh accurately into a 50 ml centrifuge tube enough sample for the previously adopted 50-70 mg of mercaptoacetic acid quantity. 232.2. Acidified with a few drops of hydrochloric acid (230.2) for approximate pH 3.294.3. Add 5 ml of demineralized water and 10 ml of acetate buffer (230.6) and with a pH paper checks that the pH value is about 5.232.4. Add 5 ml of cadmium di(acetate) solution (230.4). Wait 10 minutes. incur 232.5. Centrifuge for at least 15 minutes at 4000 RPM 232.6. Separate the supernatant, which might be insoluble fat (if the sample taken from the cream). These fats are not to be confused with the thiols, which accumulates in a compact mass at the bottom of the tube. 232.7. Check that no precipitate is formed when the supernatant to add a few drops of cadmium di(acetate) solution (230.4). If the previous proof of 232.8. no reducing agents, with the exception of the thiols, check iodometrically or thiols in the supernatant liquid does not exceed 6-8% of the initial quantity. 232.9. introductory 10 ml of methanol into the centrifuge tube, which is sediment, and easily disperse the precipitate with a glass rod. Centrifuge again for at least 15 minutes at 4000 RPM 232.10. Wash the precipitate in the light of the above procedure. The same centrifuge tube add 2 ml of the solution of methyl octanoate (230.5) and 5 ml of hydrochloric acid in methanol (230.7.). 232.11. Completely dissolve the thiols (can stay slightly soluble substance Assistant). This is a solution With this solution. aliquot check iodometrically, thiols content is at least 90% of it obtained in accordance with this annex subsection 18.3. 233. Methyl, preparing in situ (231.2) or with previously prepared diazomethane solution (231.3): 233.1. Methylation in situ. Methylation, which is 1 ml of diethyl ether, enter 50 µl of solution "S" and methylate by the method (231.2) with 300 mg of 1-methyl-3-Nitro-1-nitrozoguanidīn. After 15 minutes (the ether solution should be yellow, which means excess diazomethane) transfer the sample solution to 2 ml bottle, which has a solid stub. Overnight refrigerator. Methylate two samples simultaneously. 233.2. Methylation with diazomethane solution prepared earlier. Enter a 5 ml stoppered flask, 1 ml of diazomethane solution (230.12.), then 50 ¶l of solution "S". Overnight refrigerator. 234. the following Standards: preparing a standard solution of mercaptoacetic acid containing about 60 mg 2 ml of pure mercaptoacetic acid. This is a solution E. Precipitates, verify and methylate in accordance with this annex, 231, 232 and 233... 235. Gas chromatographic conditions for determination of mercaptoacetic acid: 235.1. Column: 235.1.1 type: stainless steel. 235.1.2. Length: 2 m diameter: 235.1.3.3 mm. Packing: 20% 235.2. didecilftalāt/hromosorb, WAW 80 to 100 the size of 235.3. is Appropriate. flame ionization detector with elektrometr sensitivity settings of 8 × 10-10 a. 235.4. Gas: 235.4.1. Carrier gas: nitrogen. 235.4.2. Pressure: 2.2 bar. 235.4.3. Flow: 35 ml/min. 235.4.4. Auxiliary gas: hydrogen. 235.4.5. Pressure: 1.8 bar. 235.4.6. Flow: 15 ml/min. detector supplies: 235.4.7. after the machine instructions of the manufacturer. 235.5. Temperature: 235.5.1. Injector: 200 ° C. 235.5.2. Detector: 200 ° C. 235.5.3. Column: 90 ° C. 235.6. Recording speed: 5 mm/min 235.7. quantity: 3 ml entered. Enter five times. 235.8. Chromatographic conditions are indicative. They enable you to provide resolution R equal to 1.5 or better: where r1 and r2-retention times (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). We recommend that you stop adjusting the chromatography temperature from 90 to 150 ° C 10 ° C per minute to eliminate substances that can interfere with subsequent measurements. 236. the calculation shall be effected in the following order: 236.1. the proportionality factor of mercaptoacetic acid. It calculates the relati construction to methyl octanoate on the basis of the standard mixture. If t represents mercaptoacetic acid: kt its response factor; m ' t-its mass (in milligrams) in the mixture; S ' t – the peak area. If "c" represents methyl octanoate on then: m ' c-its mass (in milligrams) in the mixture; S ' c-peak area, and: This coefficient will vary depending on the equipment. concentration of Mercaptoacetic acid 236.2. sample. If t represents mercaptoacetic acid: kt its response factor; St – the peak area. If "c" represents methyl octanoate on: mc-its mass (in milligrams) in the mixture; SC-the peak area; M – the initial mass of the test sample (mg), and: of mercaptoacetic acid% (m/m) in the sample is: 237. If the mercaptoacetic acid content is 8% (m/m), the results of two determinations carried out in parallel on the same sample should not exceed the difference between the absolute 0.8% (m/m) vērtību4.

19. the evidence and determination of Hexachlorophene 19.1.238. demonstration of Hexachlorophene Hexachlorophene probative method is suitable for all cosmetic products. 239. Hexachlorophene in the sample is extracted with ethyl acetate and thin-layer chromatography. 240. Hexachlorophene probative method uses the following reaģentus1:240.1. sulphuric acid, 4 M solution. 240.2. Celite AW. 240.3. Ethyl acetate. 240.4. Eluent: benzene containing 1% (v/v) glacial acetic acid. 240.5. The developer is rhodamine B solution I prepared as follows: dissolve 100 mg of rhodamine B in a mixture containing 150 ml of diethyl ether, 70 ml of absolute ethanol and 16 ml of water. 240.6. Developer II-dibromo-2.6 4-hloriminocikloheks-2.5-dienon solution prepared as follows: dissolve 400 mg of 2.6-dibromo-4-hloriminocikloheks-2.5-dienon 100 ml of methanol (prepared fresh each day). Sodium carbonate solution: dissolve 10 g of sodium carbonate in 100 ml of demineralized water. 240.7. Solution: hexachlorophene, 0.05% (m/v) solution in ethyl acetate. 241. Hexachlorophene probative method uses the following equipment: 241.1. Silica Gel 254 TLC plates, 200 × 200 mm (or equivalent). 241.2. Tlc apparatus. 241.3. Bath with thermostat set at 26 ° C, the chromatography tank. 242. preparation of the test sample was: 242.1 hexachlorophene. Well mix 1 g of homogenized sample with 1 g of Celite AW and 1 ml of sulphuric acid (240.1.). 242.2. Dry at 100 ° C for two hours. 242.3. Cool and balance dry pulverized. 242.4. extract two times, each time you use 10 ml of ethyl acetate, after each extraction centrifuge and combine the ethyl acetate layers. 242.5. Evaporate at 60 ° c. 242.6. Dissolve the residue in 2 ml of ethyl acetate. 243. proof of Hexachlorophene in the following order: 243.1. Spotted 2 ¶l of the test sample solution (242.6) and 2 ¶l of the standard solution (240.7) on a TLC plate. 243.2. Saturate the camera (241.3) with eluent (240.4. below). 243.3. Feel the TLC plate in the tank and elute up to 150 mm. thin-layer hromatogrāfijasplat 243.4. Remove and dry the ventilation type oven for about 105 ° c. 243.5. Hexachlorophene spots on thin-layer plates developed in accordance with 243.5.1. of this annex or 243.5.2.: 243.5.1. Plate evenly sprayed with developers I (240.5.). After 30 minutes the plate under UV light at 254 view nm. 243.5.2. Plate evenly sprayed with developer II (240.6) 2.6-dibromo-4-hloriminocikloheks-2.5-dienon solution. Then spray the plate with sodium carbonate solution (240.6), dry at room temperature for 10 minutes and see daylight. 244. Interpretation: 244.1. Developer I (240.5.): hexachlorophene is revealed bluish spot on a yellow-orange fluorescent background and has an Rf of approximately 0.5.244.2. Developer II (240.6): hexachlorophene is revealed as a sky-blue to turquoise coloured spot on a white background and has an Rf of approximately 0.5. determination of Hexachlorophene 19.2.245. method for the determination of Hexachlorophene is applicable to all cosmetic products. 246. the Hexachlorophene content of the sample as a percentage by mass of hexachlorophene. 247. Hexachlorophene is determined after conversion by gas chromatography with electron capture detection. 248. the determination of Hexachlorophene method uses the following reaģentus1:248.1. Ethyl acetate. 248.2. N-methyl-N-nitroso-p-toluenesulphonamide (diazald). 248.3. diethyl ether. 248.4. Methanol. 248.5.2-(2-ethoxyethoxy) ethanol (carbitol). 248.6. Formic acid. 248.7. potassium hydroxide, 50% (m/m) aqueous solution (prepare fresh daily). 248.8. Hexane spectroscopic. 248.9. Bromochlorophen (standard 1). 4, 4 ', 6 ', 6, 248.10.-tetrahlor-2, 2 '-tiodifenol (Standard No 2). 248.11.2, 4, 4 '-trichloro-2-hidroksidifenilēter (Standard No 3). 248.12. Acetone. 248.13.4 M sulphuric acid. Celite AW. 248.14. 248.15. Formic acid/ethyl acetate, 10% (v/v) solution. 248.16. Hexachlorophene. 249. the determination of Hexachlorophene method uses the following equipment: 249.1. standard laboratory glassware. 249.2. Mikroiekārt preparation of diazomethane (analyt. Chem., 1973, 45, 2302-2). 249.3. gas chromatograph equipped with a 63 Ni source electron capture detector. 250. determination of Hexachlorophene is carried out in the following order: 250.1. Solution for standard choose one that does not incorporate the jas to any adjuvant test product. The best is often the standard no 1 (248.9): 250.1.1. Weigh accurately about 50 mg of standard no 1, 2 or 3 (248.9., 248.10. or 248.11.) and 50 mg of hexachlorophene 100 ml volumetric flask. Make up to the mark with ethyl acetate (solution A). Dilute 10 ml of solution A to 100 ml with ethyl acetate (solution B). 250.1.2. Weigh accurately about 50 mg of standard no 1, 2 or 3 (248.9., 248.10. or 248.11.) 100 ml volumetric flask. Make up to the mark with a high etilac (solution C). 250.2. sample preparation: accurately weigh 1 g of homogenized sample and mix thoroughly with 1 ml of sulphuric acid (248.13.), 15 ml of acetone and 8 g of Celite AW. Air dry the mixture for 30 minutes in a steam bath, then dry for one and a half hours ventilation type drying oven. Cool, the remainder being pulverized and transfer to a glass column. Elute with ethyl acetate and collect 100 ml. Add 2 ml of internal standard solution (solution C) (250.1.2.). Whereas Hexa hlorofēn might be different types of cosmetic products, it is important to check the recovery of hexachlorophene from the sample in this proceeding before the result recorded in the horse. If the recovery is low, then, interested parties, changes the procedure (for example, using another solvent (benzene ethyl acetate) URu.tml.). 250.3. methylation of the sample: cool all reagents and equipment up to the 0-4 ° C for two hours. Into the external compartment of the diazomethane apparatus forces 1.2 ml of the solution prepared in accordance with this paragraph and annex 250.2.0.1 ml of methanol. Makes approximately 200 mg of diazald in the Central reservoir, add 1 ml of carbitol, 1 ml of diethyl ether and dissolve. Assemble the equipment, half submerged in the bath at 0 ° C and the Central reservoir syringe with approximately 1 ml of cooled potassium hydroxide solution (248.7). Ensure that the yellow coloration, caused by the formation of diazomethane persists. If the yellow colour does not persist, repeat the methylation with a further 200 mg of diazald. If the yellow coloration, it shows the remains of diazomethane superiority necessary to ensure complete methylation of the sample. Equipment removed from the bath after 15 minutes and leaves the conclusion of ambient temperature for 12 hours. Open the machine, add a few drops of 10% (v/v) solution of formic acid in ethyl acetate (248.15.), to the izreaģ of diazomethane superiority, and transfer the organic solution to a 25 ml volumetric flask. Make up to the mark with hexane. 1.5 µl of the prepared input solution into the chromatograph. 250.4. standard methylation: cool all reagents and equipment up to the 0-4 ° C for two hours. Into the external compartment of the diazomethane apparatus type: 0.2 ml of solution B (250.1.1), 1 ml of the ethyl acetate and 0.1 ml of methanol. Continue the methylation under this subparagraph annex 250.3.. Enter the resulting solution 1.5 ml chrome togrāf. 251. Gas Chromatography for the determination of hexachlorophene in the following order: the column must yield a resolution, R, which is 1.5 or better: where r1 and r2-retention times (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). 251.1. the following shall be considered suitable gas chromatography conditions: 251.1.1. Column: stainless steel: 251.1.1.1. Length: 1.7 m, diameter: 3 mm. 251.1.1.2. Media: hromosorb: WAW. 251.1.2. The sieve analysis: particle size 80 – 100.251.1.3. Stationary phase: 10% OV 17.251.1.4. Temperature: 251.1.4.1. Column: 280 ° c. 251.1.4.2. Injector: 280 ° c. 251.1.4.3. Detector: 280 ° c. 251.1.5. Carrier gas: nitrogen, without oxygen. 251.1.6. Pressure 2.3 bars. 251.1.7. Flow: 30 ml/min. 252. Calculations performed in the following order: 252.1. The proportionality coefficient of hexachlorophene. Depending on the standard calculated in relation to the standard mixture. Where: h-hexachlorophene; KH-the proportionality factor; m ' h-its mass (in grams) in the mixture; (A) ' h-peak area; s-selected Standard; m's-its mass (in grams) in the mixture; A's-its peak area, then the quantity of 252.2. Hexachlorophene in the sample. Where: h-hexachlorophene; KH-the proportionality factor; Ah, the peak area; s-selected Standard; Ms-its mass (in grams) in the mixture; Axis-the peak area; M-take the mass (in grams):% (m/m) of hexachlorophene in the sample is: 253. From a single sample with a 0.1% (m/m) of hexachlorophene content of the difference between the results of two determinations should not exceed an absolute 0.005% (m/m) vērtību4. 20. Tosylchloramide sodium (INN) (chloramine-T) determination With chloramine-T 254. quantification method for determination of tosylchloramide sodium (chloramine-T) in cosmetic products by using thin-layer chromatography. 255. the chloramine-T content of the sample, in percentage by mass (m/m). 256. Chloramine-T completely hydrolyzed to 4-toluenesulphonamide by boiling with hydrochloric acid. The resulting quantity of 4-toluenesulphonamide fotodensitometrisk down thin-layer chromatography. 257. Chloramine-T quantitative detection method uses the following reaģentus1:257.1. Tosylchloramide sodium (chloramine-T). 257.2. standard solution of 4-toluenesulphonamide: 50 mg of 4-toluenesulphonamide in 100 ml of ethanol (257.5). 257.3. Hydrochloric acid 37% (m/m) = 1.18 g/ml. 257.4. diethyl ether. ethanol, 96% 257.5. (v/v). 257.6. Development solvent: 257.6.1.1-butanol/ethanol (257.5)/water 40:4: 9 (v/v/v). 257.6.2. Chloroform/acetone 6:4: 4 (v/v). 257.7. Ready for thin-layer chromatography plates, silica gel 60, without fluorescence indicator. 257.8. Potassium permanganate. 257.9. Hydrochloric acid, 15% (m/m). 257.10. Spray reagent: 2-toluidine, 1% (m/v) solution in ethanol (257.5). 258. Chloramine-T quantitative detection method uses the following equipment: 258.1. Laboratory equipment. 258.2. standard thin-layer chromatography. 258.3. Fotodensitometr. 259. Chloramine-T the determination shall be made in the following order: 259.1. Hydrolysis. Weigh accurately 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 (257.3) and reflux for one hour with stirring. Hot water immediately the suspension into a 50 ml volumetric flask. Allow to cool and make up to the mark with water. Centrifuge for five minutes at least to 3000 rpm and filter the supernatant. 259.2. Extraction: 259.2.1.30 ml of the filtrate and extract three times with 15 ml of diethyl ether. If necessary dry the Ethereal phases and collect the 50 ml volumetric flask. Make up to volume with diethylether. 259.2.2. Take 25 ml dried ether extract and evaporate to dryness of the nitrogen in the atmosphere. Dissolve the residue in 1 ml again ethanol. 259.3. Thin layer chromatography: 259.3.1. Spotted 20 μl of ethanol (259.2) on a TLC plate (257.7). At the same time the same deck 8, 12, 16 and 20 ¶l of the standard solution of 4-toluenesulphonamide (257.2). 259.3.2 enables you to develop approximately 150 mm in the development solvent (257.6.1. or 257.6.2.). 259.3.3. when the developing solvent is completely evaporating, extra wide for two or three minutes of chlorine vapour in the atmosphere, resulting in a closed container, pouring about 100 ml of hydrochloric acid (257.9) to about 2 g of potassium permanganate. The superiority of the chlorine is separated, five minutes by heating to 100 ° C plate. Then spray the plate with reagent (257.10.). 259.4. Measuring: after about one hour of 525 nm size fotodensitometr with purple spots. 259.5. Calibration Curves: note the maximum height of the peak value corresponding to four 4-toluenesulphonamide spots against the corresponding quantities of 4-toluenesulphonamide (i.e. 4, 6, 8, 10 ¶g of 4-toluenesulphonamide per spot). 260. The method can be controlled with the 0.1 or 0.2% (m/v) of chloramine-T solution processed in an identical manner as the sample (259). 261. the chloramine-T content of the sample, in percentage by mass, is calculated as follows:% (m/m) = where: 1.33 tosylchloramide sodium 4-toluenesulphonamide-chloramine-T conversion factor; a-4-toluenesulphonamide in the sample (mg) in accordance with the calibration curves; m-take the mass (in grams). 262. From a single sample with 0.2% (m/m) of chloramine-T content of the difference between the results of two determinations should not exceed an absolute 0.03% (m/m) vērtību4. 21. determination of total fluorine in toothpaste By 263. determination of total fluorine in toothpaste method determines the total amount of fluoride toothpaste if the fluoride level does not exceed 0.25%. 264. the Fluorine content of the sample, in percentage by mass. 265. determination of total fluorine in gas chromatography is carried out. Fluorine fluorine-containing compounds is in triethylfluorosilane (tefs) direct reaction with chlorotriethylsilane (TECs) in acid solution and simultaneously extracted with xylene containing cyclohexane as internal standard. 266. determination of total fluorine in toothpaste using the method reaģentus1:266.1. Sodium fluoride, which is 120 ° C dried to constant weight. distilled water, double-266.2. or equivalent quality. 266.3. Hydrochloric acid, = 1.19 g/ml. 266.4. Cyclohexane (CH). 266.5. Xylene, which is not in the peak of the chromatogram prior to the solvent peak when the hromatograf under the same conditions as the sample (268.1.). If not difficult, to purify the distillation (267.8.). 266.6. Chlorotriethylsilane (TECs Merck or equivalent). fluorine standard solutions: 266.7.266.7.1. Solution. 0.250 mg F-/ml. Weigh accurately 138.1 mg of sodium fluoride (266.1) and dissolve in water (266.2). Kvantit the light into a 250 ml volumetric flask on the solution (267.5). Dilute with water (266.2) up to the mark and mix. 266.7.2. Diluted solution, 0.050 mg F-/ml. Pipette 20 ml of the stock solution (266.7.1) to a 100 ml volumetric flask (267.5. below). Dilute to the mark with water and mix. 266.8. Internal standard solution: mix 1 ml of cyclohexane and 5 ml of xylene (266.5). 266.9. Chlorotriethylsilane/internal standard solution: transfer by pipette (267.7. bottom point) into a 0.6 ml of TECs and 0.12 ml of the internal standard solution (266.8. bottom) to a 10 ml volumetric flask. Dilute with xylene (266.5) up to the mark and mix. Every day fresh solution. 266.10. Perchloric acid, 70% (m/v). 266.11. Perchloric acid, 20% (m/v) in water (266.2). 267. for the determination of total fluorine in toothpaste method uses the following equipment: 267.1. Laboratory equipment. 267.2. Gas Chromatograph equipped with flame ionisation detector. 267.3. Virpuļmaisītāj or equivalent. 267.4. Shaker, type SMB1 or equivalent. volumetric flasks, 100 and 267.5.250 ml, made of polypropylene. 267.6. Centrifuge Tubes (glass); 20 ml with teflon lined screw caps, Sovirel type 611-56 or equivalent. Clean the tube and screw the jamo covers, several hours keeping in perchloric acid (266.11), then five times with water (266.2), and finally dry at 100 ° C. 267.7. Pipettes that can be adjusted to 50-200 µl volume transfer, with disposable plastics tips. 267.8. Distillation apparatus which is Schneider's column with three beads or an equivalent Vigreux column. 268. determination of total fluorine in the following order: 268.1. sample analysis: 268.1.1. Having toothpaste that has not been previously opened, open and remove all the content. Transfer to a plastic container, mix thoroughly and store in circumstances where the mail does not change. weigh accurately 150 mg, 268.1.2. (m) sample centrifuge tube (267.6), add 5 ml of water (266.2) and homogenize for virpuļmaisītāj. 268.1.3. Add 1 ml of xylene. 268.1.4. Drop by drop, add 5 ml of hydrochloric acid (266.3) and homogenize for virpuļmaisītāj. 268.1.5. pipette into the centrifuge tube (267.6) 0.5 ml of chlorotriethylsilane/add internal standard solution (266.9). 268.1.6. Close the tube with screw cap (267.6) and 45 minutes carefully mix with Shaker set at 150 strokes per minute. 268.1.7. Centrifuge for 10 minutes at such a speed as to clearly separate the phases, unscrews the tube, remove the organic layer and inject 3 ¶l of the organic phase gas chromatograph column. After about 20 minutes, all components are eluted. 268.1.8. Again, calculate the average peak area ratio (atefs/ACH) and from the calibration curve (268.3) reads the amount of fluorine (in milligrams (m1)). 268.1.9. calculation of the total fluorine content of the sample (percentage by mass of fluorine), as specified in the annex in the 269. 268.2. Chromatographic conditions: 268.2.1. Column: stainless steel. length: 1.8 m 268.2.1.1.. 268.2.1.2.3 mm. Diameter 268.2.1.3. Media: Gaschrom Q 80 to particle size 100.268.2.1.4. Stationary phase: silikoneļļ DC 200 or equivalent, 20%. Overnight conditioned column 100 ° C (carrier gas flow: 25 ml nitrogen per minute), it repeats every night. After every fourth or fifth injection recondition the column by heating 100 ° C for 30 minutes. 268.2.2. Temperature: 268.2.2.1. column: 70 ° c. 268.2.2.2. injector: 150 ° C. 268.2.2.3. detector: 250 ° c. 268.2.3. Carrier gas flow: 35 ml of nitrogen per minute. 268.3. Calibration Curve: pipette 268.3.1. six centrifuge tubes (267.6) pipette 0, 1, 2, 3, 4 and 5 ml of the diluted fluoride standard solution (266.7.2). All tubes make up to 5 ml with water (266.2). 268.3.2. Continue activities under this annex, 268.1.4 268.1.5 268.1.3., 268.1.6. and section. 268.3.3. Enter 3 ¶l of the organic phase gas chromatograph column. 268.3.4. Enter it again and calculate the average peak ratio (atefs/ACH). 268.3.5. Plot a calibration graph, comparing the mass of fluorine (in milligrams) in the standard (268.3.1) and the peak area ratio (atefs/ACH) measured in accordance with 268.3.4. of this annex. Curve points connecting with the appropriate straight line calculated by regression analysis. 269. the concentration of the total fluorine sample (percentage by mass of fluorine) (% (m/m) F) is given by the formula: F = m – which the sample quantity (in milligrams) (268.1.2); M1-F (in milligrams) read from the calibration curve (268.1.8 below). 270. One sample to 0.15% (m/m) content of fluorine, the difference between the results of two determinations in parallel should not exceed an absolute 0.012% (m/m) vērtību4. 22. the burden of proof and the Organomercury compounds determination of organomercury compounds 271. With evidence and determination method and determination of organomercury derivatives of such used as preservatives in cosmetics: eyes of thiomersal (INN), sodium 2-(etildzīvsudrab) benzoate and phenylmercuric and its salts. 22.1. The Organomercury compounds prove Organomercury compounds are 272. complete with 1.5-diphenyl-3-tiokarbazon. When ditizonāt is extracted with carbon tetrachloride, silica gel thin-layer chromatography. Ditizonāt spots appear orange. 273. The Organomercury compound method of proof uses the following reaģentus1:273.1. Sulphuric acid 25% (v/v). 1.5-diphenyl-3 273.2.-tiokarbazon (dithizone): 0.8 mg in 100 ml of tetrahlor carbon (273.4). 273.3. Nitrogen. 273.4. Carbon tetrachloride. 273.5. Development solvent: hexane/acetone, 90:10 (v/v). standard solution, 0.001% 273.6. water: sodium 2-(etildzīvsudrabti) ben zoāt, etildzīvsudrab chloride or methylmercury chloride, phenylmercuric nitrate or phenylmercuric acetate, mercury dichloride or mercury di(acetate). 273.7. Ready silica gel plates (e.g. Merck 5721 or equivalent). 273.8. sodium chloride. 274. The Organomercury compounds demonstrating method uses the following equipment: 274.1. Laboratory equipment. 274.2. normal TLC apparatus for thin-layer chromatography. 274.3. Phase-separating filter. 275. The Organomercury compounds prove out in the following order: 275.1. extraction: 275.1.1. Centrifuge tube, dilute 1 g of the sample titration with 20 ml of distilled water. Retrieves the maximum variance and the warms up to 60 ° C in a water bath. Add 4 g of sodium chloride. Shake. Allow to cool. 275.1.2. Centrifuge for at least 20 minutes at 4500 revolutions per minute, separated from the fluid in most solids. Filter the separating funnel and add 0.25 ml of sulphuric acid solution (273.1). 275.1.3. Extract several times with 2 or 3 ml of dithizone solution (273.2) until the last organic phase remains green. 275.1.4. Each organic phase in turn filtered through a phase-separating filter. 275.1.5. Evaporate the atmosphere of nitrogen. dissolve 0.5 ml 275.1.6. carbon tetrachloride. This solution is used immediately in accordance with 275.2.1. of this annex. separation and identification of 275.2.275.2.1.50 ml carbon tetrachloride: solution obtained in accordance with this annex, 275.1.6., now covered on silica gel plates. At the same time in accordance with this annex, point processes 10 275.1. ml standard solution (273.6. below) and on the same plate 50 ¶l of the solution obtained in accordance with 275.1.6. of this annex. 275.2.2. Extra wide solvent (273.5) and permit the development of 150 mm. The Organomercury compounds appear colored spots sustainable manner if the plate immediately after evaporation of the solvent, covered with glass. For example, the following Rf values are obtained: Rf color thiomersal 0.33 Orange Etildzīvsudrab chloride 0.29 Orange Methylmercury chloride 0.29 Orange phenylmercuric salts 0.21 Orange mercury (II) salts of Mercury diacetate 0.10 0.10 Orange Orange-diphenyl-3-tiokarbazon 1.5 a 0.09 pink 22.2. determination of Organomercury compounds * 276. With the determination of organomercury compounds method of organomercury compounds content of the sample in the sample as a percentage by mass of mercury (m/m). 277. The Organomercury detection method of connection is the common measurement of mercury. So first you need to make sure that the sample is inorganic mercury and organomercury derivatives must be demonstrated in the sample. After the release of the mercury mineralization measured by flameless atomic absorption. 278. The Organomercury compounds method uses the following reaģentus1:278.1. concentrated nitric acid, = 1.41 g/ml. 278.2. Concentrated sulphuric acid, = 1.84 g/ml. water thoroughly 278.3. 278.4. Potassium permanganate, 7% (m/v) solution. 278.5. Hidroksilamonij chloride, 1.5% (m/v) solution. DIPOTASSIUM peroksodisulfāt, 278.6.5% (m/v) solution. 278.7. Tin dichloride, 10% (m/v) solution. 278.8. Concentrated hydrochloric acid = 1.18 g/ml With Palladium dichloride 278.9. impregnated glass wool, 1% (m/m). 279. The Organomercury compounds method uses the following equipment: 279.1. Laboratory equipment. 279.2. equipment, including glass jars, which are required for the determination of mercury using a flameless atomic absorption (cold vapour technique). The length of the cell at least 100 mm. 280. Subject to any mikrodzīvsudrab analysis standard security measures, organomercury compounds shall be carried out in the following order: weigh accurately 150 mg 280.1. sample (m). Add 10 ml of nitric acid (278.1) and allowed to react for three hours in an airtight flask in the water bath at 55 ° C, shake regularly. At the same time make the reagent blank check. 280.2. After cooling, add 10 ml of sulphuric acid (278.2) and again puts in a water bath at 55 ° C for 30 minutes. 280.3. Flask in an ice bath and add carefully 20 ml of water (278.3). 280.4. Add 2 ml of 7% potassium permanganate solution into aliquots until the solution stains. Put back in the water bath at 55 ° C for another 15 minutes. 280.5. Add 4 ml of DIPOTASSIUM peroxodisulphate solution (278.6. below). Continue heating for 30 minutes in the water bath at 55 ° c. 280.6. Allow to cool and transfer the contents of the flask to a 100 ml volumetric flask. Rinse the flask with 5 ml 1.5% hidroksilamonij chloride solution and then rinse four times with 10 ml of the water thoroughly. The solution should be colourless. Make up to the mark with double-distilled water. 280.7. Makes a 10 ml test solution (280.6.) glass container for the determination of mercury by cold vapour technique (279.2). Diluted with 100 ml of water, then thoroughly with 5 ml of a 25% sulphuric acid and 5 ml of 10% solution of Tin dichloride. Mix after each addition. Wait 30 seconds for all mercury ions reduced to metallic mercury, and take the measurements (n). 280.8. Places with Palladium dichloride impregnated glass wool between the mercury reduction vessel and cell (379.2). Repeat this annex 280.7. the activities referred to in point and record the measurement. If the reading is not zero mineralization has not been completed and the test must be repeated. 281. the mercury mercury quantity, expressed as a percentage by mass, is given by the formula:% of mercury = m – which the mass (in milligrams); n – the measured quantity of mercury (μg). 282. From the same sample 0.007% mercury concentration difference between the results of two determinations should not exceed an absolute 0.00035% vērtību4. * Notes. To improve digestion, it may be necessary to start with the sample dilution. If you suspect that absorbs mercury substrate shall be carried out with a standard attached ery method. 23. Alkali and alkaline-earth sulphide discovery 283. With alkali and alkaline-earth sulphide method detects sulphides in cosmetic products. Thiols or other reducing agents (including sulphites) does not interfere. 284. Sulphide concentrations are expressed as a percentage by mass of sulphur. 285. on environmental acidification of the medium scale with a stream of nitrogen, then locks the cadmium sulphide. The last is filtered and rinsed, and then determined iodometrically. 286. the alkali and alkaline-earth sulphide discovery method, use the following reaģentus1:286.1. concentrated hydrochloric acid, = 1.19 g/ml. 286.2. Sodium Thiosulphate, 0.1 M standard solution. 286.3.0.05 M iodine solution. disodium sulphide 286.4.. 286.5. cadmium diacetate. 286.6. concentrated ammonia, = 0.90 g/ml. 286.7. Ammoniacal cadmium di(acetate) solution: dissolve 10 g of cadmium di(acetate) about 50 ml of water. Add ammonia (286.6) until the precipitate dissolves (i.e. any other. approximately 20 ml). Make up to 100 ml with water. 286.8. Nitrogen. 286.9. Ammonia M solution. 287. the alkali and alkaline-earth sulphide method uses the following equipment: 287.1. Laboratory equipment. 100 ml round-bottom flask of 287.2. trijkakl with a ground-glass necks. 150 ml conical 287.3. Two flasks with ground-glass necks, fitted with the device, which is comprising and entraining gas release. 287.4. One funnel with a long handle. 288. Alkali and alkaline-earth sulphide discovery performed in the following order: 288.1. Sulphide separation: 288.1.1. View packaging has not been opened. Weigh accurately into a round-bottom flask (287.2) cosmetic (m) weight (in grams), corresponding to not more than 30 mg of sulphide ion. Add 60 ml of water and two drops of anti-foaming liquid. 288.1.2. Transfer 50 ml of the solution (286.7) on both koniskaj flasks (287.3.). 288.1.3. Round-bottomed flask (287.2) be fitted with a dropping funnel, comprising and duct. At the time of koniskaj duct the flasks (287.3) connected by teflon tubing. Separation equipment tightness test: simulating the test conditions, replace the product to be determined by 10 ml of a sulphide solution (prepared from 286.4. this annex referred to disodium sulphide) containing "X mg of sulphide (iodometrically determined). "Y" shall be taken as the number of milligrams of sulphide at the end of this operation. The difference between the quantity "X" and "Y" must not exceed 3%. 288.1.4. nitrogen passes through 15 minutes at a speed of two bubbles per second to displace air, which is a round-bottomed flask (287.2). 288.1.5. Heat in a round-bottom flask to 85 ± 5 ° c. 288.1.6. release nitrogen atmosphere and drop by drop, add 40 ml of hydrochloric acid (286.1.). 288.1.7. Nitrogen atmosphere restored, when almost all the acid is transferred, leaving a small layer of the liquid, to prevent the medium from leaking. 288.1.8. Repeat the heating stops after 30 minutes. Allow the flask (287.2. bottom) cool and continue to put through the nitrogen atmosphere for at least an hour and a half. 288.2. Titration: 288.2.1. Filter the cadmium sulphide through a funnel with a long handle. 288.2.2. Rinse the conical flasks (288.3) with ammonia solution (286.9) and discard the filter. Then rinse with distilled water and wash the filter with the water held in the sediment. 288.2.3. The sediment washing complete with 100 ml of water. 288.2.4. Paper filter makes the first conical flask that contained the precipitate. Add 25 ml (n1) of the iodine solution (286.3), approximately 20 ml salt acid (286.1) and 50 ml of distilled water. 288.2.5. Determine the excess iodine using the Sodium Thiosulphate solution (n2) (286.2). 289. Sulphide content of the sample, expressed as a percentage by mass of sulphur, is calculated by the following formula: = n1% sulphur, which – in the iodine solution used (ML); x 1-the Molarity of this solution; N2 – the quantity of Sodium Thiosulphate solution (ML); x 2-the Molarity of this solution; m-sample mass (in grams). 290. One sample with approximately 2% (m/m) the sulphide content of the difference between the results of two determinations should not exceed an absolute 0.2% (m/m) vērtību4. 24. Glycerol 1-(4-aminobenzoate) demonstration and identification of glycerol 15.0.1-(4-aminobenzoate) demonstration With glycerol 1-291. (4-aminobenzoate) method of proof, proof of Alpha-monoglyceryl 4-aminobenzoate (glycerol 1-(4-aminobenzoate)) and ethyl-4-amino benzoate (benzocaine INN), which can be as impurities. 292. Glycerol 1-(4-aminobenzoate) demonstrates the grāfij of silica gel thin-layer hromat with fluorescent lights, and free primary amino group is determined by the diazokrāsviel formation on the plate. 293. Glycerol 1-(4-aminobenzoate) method of proof uses the following reaģentus1:293.1. The solvent mixture: cyclohexane/propan-2-ol/stabilized dichloromethane 48:64:9 (v/v/v). 293.2. Development solvent: petroleum (40-60)/benzola/acetona/amonija hydroxide solution (minimum 25% NH3): 35:35 35:1 (v/v/v/v). 293.3. Development solvent: 293.3.1. sodium nitrite: 1 g in 100 ml of 1 M hydrochloric acid (prepared immediately before use); 293.3.2.2-naphthol: 0.2 g in 100 ml of 1 M potassium hydroxide. 293.4. Standard solutions: Alpha-monoglyceryl 4-aminobenzoate: 0.05 g in 100 Mili liters of solvent mixture (293.1); ethyl-4-amino-benzoate of this Annex: 0.05 g in 100 ml of solvent mixture (293.1). silica gel 60 F254 293.5. plates, 0.25 mm thick, 200 × 200 mm. 294. Glycerol 1-(4-aminobenzoate) method of proof uses the following equipment: 294.1. Tlc apparatus. 294.2. ultrasonic bath. Millipore filter FH 294.3., 0.5 mm or equivalent. 295. Glycerol 1-(4-aminobenzoate) demonstration is performed in the following order: 295.1. Preparation of the sample: weigh 1.5 g of the product to be analysed 10 ml in a volumetric flask with stopper. Make up to the mark with the solvent (293.1. the bottom). Stopper and leave for one hour at room temperature in an ultrasonic vibrator. Filter through a Millipore filter (294.3) and use the filtrate for the Papua New Guinea hromatogr. 295.2. Thin layer chromatography: deposit 10 ml of the sample solution (295.1. below) and each standard solution (293.4) on the plate (293.5. bottom). Develop the chromatogram until 150 mm height Chamber saturated with solvent (293.2). Allow the plate to dry at ambient temperature. 295.3. Developing: 295.3.1. view the plate under UV light at 254 nm. 295.3.2. Completely wet plate sprayed with solution (293.3.1 below). Allow to dry at room temperature for 1 minute and immediately spray with solvent (293.3.2). Dry the plate in an oven at 60 ° c. Spots appear orange. Alpha-monoglyceryl 4-aminobenzoate: Rf = 0.07, ethyl-4-aminobenzoate: Rf = 0.55.24.2. Glycerol 1-(4-aminobenzoate) * 296. With glycerol 1-(4-aminobenzoate) method determines Alpha monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate. It can detect more than 5% (m/m) alpha-monoglyceryl 4-aminobenzoate and 1% (m/m) ethyl 4-aminobenzoate. 297. Alpha-monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents of the product expressed as a percentage by mass (% m/m). 298. the product to be analyzed is suspended in methanol and after relati sample processing timely is determined by high-performance liquid chromatography (HPLC). 299. Glycerol 1-(4-aminobenzoate) method uses the following reaģentus1 2:299.1. Methanol. 299.2. Potassium dihidrogēnortofosfāt (KH2PO4). 299.3. diacetate Zinc (Zn (CH3CO) 2 72h2o). 299.4. Acetic acid (d = 1,05). 299.5. potassium hexacyanoferrate (K4 (Fe (CN) 6) · 3 H2O). 299.6. Ethyl 4-hydroxybenzoate. 299.7. Alpha-monoglyceryl 4-aminobenzoate. 299.8. Ethyl 4-aminobenzoate. 299.9. Phosphate buffer solution (0.02 M): dissolve 2.72 g of potassium dihidrogēn phosphate (299.2) in one litre of water. 299.10. Eluant: phosphate buffer (298.9)/metanols 61:39 (v/v). The composition of the mobile phase may be changed in order to achieve a resolution factor R = 1.5, where R1 and R2 – peak retention time (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). 299.11. Alpha-monoglyceryl 4-aminobenzoate standard solution: weigh accurately about 40 mg of Alpha-monoglyceryl 4-aminobenzoate and introduce it into a 100 ml volumetric flask. Dissolve in 40 ml of methanol. Make up to the mark with the buffer solution (299.9. bottom) and mix. 299.12. stock solution of ethyl 4-aminobenzoate: weigh accurately about 40 mg of ethyl 4-aminobenzoate and introduce it into a 100 ml volumetric flask. Dissolve in 40 ml of methanol. Make up to the mark with the buffer solution (299.9) and mix. 299.13. Internal standard solution: weigh accurately about 50 mg of ethyl 4-hydroxybenzoate, transfer to a 100 ml standard flask, dissolve in 40 ml of methanol, make up to the mark with the buffer solution (298.9) and mix. 299.14. Reference solutions: prepare four standard solutions by dissolving in 100 ml eluant (298.10.) in accordance with the following table: standard solution Alpha-monoglyceryl 4-aminobenzoate ethyl-4-aminobenzoate ethyl 4-hydroxybenzoate (μg/ml) ml (299.11.) (μg/ml) ml (299.11.) (μg/ml) ml (299.11.) I II III IV 8 2 8 2 50 10 16 4 12 3 50 10 24 6 16 4 50 10 40 10 20 5 50 10 * these values are specified and correspond to the exact masses (299.11. , and 299.13 819.15.). These solutions may be prepared differently.

299.15. Carrez I solution: dissolve 26.5 g of potassium hexacyanoferrate in water and make up to 250 ml. 299.16. Carrez II solution: dissolve 54.9 g of zinc di(acetate) and 7.5 ml of acetic acid (298.4.) in water and make up to 250 ml. Merck Lichrosorb RP-18 299.17. or equivalent, with an average particle size of 5 mm. 300. Glycerol 1-(4-aminobenzoate) method uses the following equipment: 300.1. Laboratory equipment. 300.2. high performance chromatography equipment with a variable length UV detector and column oven, set at 45 ° c. 300.3. Stainless-steel column: length 250 mm, internal diameter 4.6 mm Lichrosorb RP-18, fill (299.17.). 300.4. ultrasonic bath. 301. Glycerol 1-(4-aminobenzoate) test is performed in the following order: 301.1. sample preparation: 301.1.1. Accurately weigh approximately 1 g of the sample into a 100 ml beaker and add 10 ml of methanol. 301.1.2. Place the beaker in the ultrasonic bath for 20 minutes to occur. The suspension thus obtained quantitatively into a 100 ml volumetric flask with to no more than 75 ml eluant (299.10). Consecutively add 1 ml of carrez solution I (299.15.) and 1 ml of carrez solution II (299.16.) and mix after each addition. Make up to the mark with eluant (299.10), mix and filter through a pleated filter paper. 301.1.3. Pipette 3.0 ml of this annex in accordance with 301.1.2 below the point of the filtrate obtained and 5.0 ml of the internal standard solution (299.13.) to a 50 ml volumetric flask. Make up to the mark with eluant (299.10) and mix. This solution is used for the chromatographic analysis (301.2). 301.2. Chromatography: 301.2.1. Mobile phase (299.10) flow rate shall be adjusted to 1.2 ml/min and the column temperature to 45 ° c. 301.2.2. Set the detector wavelength (300.2) tuned to 274 nm. 301.2.3. microsyringe With at least two times over 20 ¶l of solution (301.1.3) enter the chromatograph and measure the peak areas. 301.3. Calibration Curve: 301.3.1. Enter 20 ml of each standard solution (299.14.) and measure the peak areas. 301.3.2. For each concentration calculate the alpha-monoglyceryl 4-aminoben zoāt peak and the internal standard peak area ratio. The notes on the abscissa and the corresponding masses on the ordinate axis. 301.3.3. The same procedure shall apply to ethyl 4-hydroxybenzoate. 302. the calculation shall be effected in the following order: 302.1. From the calibration curve obtained under subparagraph reads 301.3. mass ratios (RP1, RP2) corresponding to the section under 301.2.3. estimated peak area ratio where RP1-Alpha-monoglyceryl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate mass; Rp2-ethyl 4-aminobenzoate/mass of ethyl 4-hydroxybenzoate. 302.2. From this mass relation obtained calculate the alpha-monoglyceryl 4-aminobenzoate and ethyl 4-aminobenzoate contents as a percentage by mass (% m/m), using the formula: Rp% (m/m) alpha-monoglyceryl 4-aminobenzoate = Rp% (m/m) ethyl 4-aminobenzoate = q-ethyl 4-hydroxybenzoate (internal standard) (in milligrams) of the annex, in accordance with this subparagraph; 819.15. p-sample quantity (in grams) in accordance with 301.1.1. of this annex. 303. One sample with 5% (m/m) alpha-monoglyceryl 4-aminobenzoate contents, the difference between the results of two determinations carried out should not exceed 0.25% 4.304. One sample with 1% (m/m) ethyl 4-aminobenzoate contents, the difference between the results of two determinations carried out should not exceed 0.10% 4 notes. Before analysis, check that the sample contains substances which may overlap in the chromatogram peaks with the internal standard (ethyl 4aminobenzoāt) spear. To verify that there is no interference, repeat the determination by changing the proportion of methanol in the mobile phase by 10% relative. 25. determination of Chlorobutanol 305. With the determination of chlorobutanol method determines the chlorobutanol (INN) up to a maximum concentration of 0.5% (m/m) in any cosmetic product, except aerosols. 306. the content of Chlorobutanol in the product is expressed as a percentage by mass (% m/m). 307. when test a cosmetic feature is properly treated, the determination is carried out in gas chromatography internal standard using a 2, 2,2-trichloroethanol. 308. method for the determination of Chlorobutanol uses the following reaģentus1:308.1. Chlorobutanol (1,1,1-trichloro-2-metilpropan-2-ol). 2,2,2-trichloroethanol 308.2.. 308.3. Absolute alcohol (ethanol). standard solution of Chlorobutanol: 308.4.0.025 g in 100 ml ethanol (m/v). 308.5. Solution: 4 mg, 2, 2-2 in 100 ml of ethanol trichloroethanol (m/v). 309. the determination of Chlorobutanol method uses the following equipment: 309.1. Laboratory equipment. 309.2. Gas Chromatograph with electron detector, Ni 63.310 determination of Chlorobutanol takes such.: 310.1. sample preparation: accurately weigh 0,1-0,3 g (p g) of the sample. Makes 100 ml volumetric flask. Dissolve in ethanol, add 1 ml of the internal standard solution (308.5.) and make up to the mark with ethanol. 310.2. Gas chromatographic conditions: 310.2.1. operating conditions must yield a resolution factor R = 1.5. where R1 and R2 – peak retention time (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). 310.2.2. For example, the following operating conditions provide the required resolution: column I II Material glass stainless steel length 1.80 m 3 m diameter 3 mm 3 mm stationary phase 10% Carbowax 20 M TPA on Gaschrom Q, with particle sizes 80-100% on Chromosorb WAW 5 OJ NO 17 the DMCA, with particle size of 80-100 sample conditioning 2-3 days 190 ° C temperature: 150 ° C, column 100 ° C 150 ° C 200 ° C 150 ° detector (C) carrier gas nitrogen Argon/methane 95:5 (v/v)

Flow rate 35 ml/min 35 ml/min 310.3. standard curve. Using five 100 ml volumetric flasks, add 1 ml of the standard solution (308.5.) and 0.2, 0.3, 0.4, respectively 0.5 and 0.6 ml of solution, (308.4), make up to the mark with ethanol and mix. Inject 1 µL of each solution into the chromatograph in accordance with the conditions of work referred to in paragraph 310.2.2. of this annex, and construct a calibration curve by plotting the abscissa the ratio of the mass of chlorobutanol, 2, 2, 2-mass and trichloroethanol on the ordinate axis – the peak area ratio. 310.4. Inject 1 μl of this annex, in accordance with section 310.1. get solution and continues in accordance with the conditions referred to in paragraph 310.2.2. of this annex. 311. the calculation shall be effected in the following order: 311.1. by standard curve (310.3) calculates the quantity a, expressed in milligrams of chlorobutanol, in the solution (310.1). the content of Chlorobutanol 311.2. sample is given by the formula:% (m/m) = 312. chlorobutanol from one sample with 0.5% (m/m) content of chlorobutanol, the difference between the results of two determinations carried out should not exceed 0.01% 4. If the result is equal to the maximum permitted concentration or exceed it, verify that there is no overlap. 26. the burden of proof and the determination of quinine 26.1. demonstration of quinine quinine 313. means of proving method By determine quinine shampoos and hair lotions. 314. the silica gel TLC Show. Quinine is determined by the blue fluorescence 360 nm in acidic media. Following approval of the fluorescence can be eliminated by bromine vapours, ammonia vapours will cause a yellowish fluorescence. 315. the showing of quinine method uses the following reaģentus1:315.1. Silica Gel plates, without fluorescence indicators, 0.25 mm thick, 200 × 200 mm. 315.2. Developing solvent: toluene/diethyl ether/dichloromethane/diethanolamine 20:20:20:8 (v/v/v/v). 315.3. Methanol. 315.4. sulphuric acid (96%; = 1,84). serial. diethyl ether. developing agent: 315.6. refrigerated container 95 ml of diethyl ether carefully add 5 ml of sulphuric acid (315.4). 315.7. Bromine. 315.8. Ammonium hydroxide solution (28%; = 0,90). 315.9. Quinine, anhydrous. 315.10. Standard solution: weigh accurately about 100.0 mg of anhydrous quinine flask and dissolve in 100 ml of methanol. 316. the showing of quinine method uses the following equipment: 316.1. Standard equipment for thin layer chromatography. 316.2. ultrasonic bath. Millipore filter, 316.3. FH 0.5 µm or equivalent with suitable filtration equipment. 317. the showing of quinine is performed in the following order: 317.1. sample preparation: weigh accurately into a 100 ml standard flask a quantity of the sample which may contain approximately 100 mg of quinine, dissolve and make up to the mark with methanol. Stopper the flask and leave for one hour at room temperature in ultra sonic bath. Filter (316.3.) and use the filtrate for chromatography. 317.2. Thin layer chromatography: deposit 1.0 ml of standard solution (315.10. bottom) and 1.0 ml of sample solution (317.1) on the silica gel plate (315.1). Develop the chromatogram of 150 mm in length with a solvent (315.2) camera, previously saturated with dissolved in the cities (315.2. below). developing: 317.3.317.3.1. Dry the plate at room temperature. 317.3.2. Spray with reagent (315.6). Allow the plate to dry 317.3.3. one hour at room temperature. 317.3.4. view the ultraviolet light of a lamp that has a wavelength of 360 nm. Quinine fluoresce a bright blue stain. The table contains the main alkaloids related to quinine Rf value examples relating to the development of a solvent (315.2).

Alkaloid RF Hinidīn 0.29 Cinhonīn of quinine to 0.20 Cinhonidīn of Hidrohinidīn of 0.27 0.33 0.17 317.3.5. Further confirmation of the presence of quinine in the sample plate approximately one hour is treated with bromine vapour. Fluorescence is lost. If the same plate is treated with ammonia vapours (315.8), spots newly appear brown in color, and if the plate is again examined under UV light at 360 nm, yellowish fluorescence can be observed. Detection limit: 0.1 mg of quinine. 16.2. determination of Quinine 318. With quinine method determines the quinine. You can determine the maximum 0.5% (m/m) concentration of 0.2% concentration in shampoos and hair lotions. 319. the detection method of quinine quinine content of the product as a percentage by mass (% m/m). 320. when test a cosmetic product is properly treated, the determination is carried out by high-performance liquid chromatography (HPLC). 321. the method for the determination of Quinine used such reaģentus1, 2:321.1. Acetonitrile. 321.2. Potassium dihidrogēnortofosfāt (KH2PO4). 321.3. Orthophosphoric acid (85%; = 1,7). tetramethylaminium bromide. 321.4. 321.5. Quinine, anhydrous. 321.6. Methanol. 321.7. Orthophosphoric acid solution (0.1 M): weigh 11.53 g of orthophosphoric acid (321.3) 1000 ml in a volumetric flask and dissolve in water. potassium dihydrogenorthophosphate 321.8. solution (0.1 M): weigh 13.6 g of potassium dihydrogenorthophosphate (321.2) 1000 ml in a volumetric flask and dissolve in water. tetramethylaminium bromide 321.9. solution: dissolve 15.40 g volumetric tetramethylaminium bromide 1000 ml of water. Eluant: orthophosphoric acid 321.10. (321.7)/potassium orthophosphate dihidrogēn (321.8)/tetrametilamonija bromide (321.9)/water/acetonitrile 10:50:100:340:90 (v/v/v/v/v). The composition of the mobile phase may be changed in order to achieve a resolution factor R = 1.5. where R1 and R2 – peak retention time (in minutes); W1 and W2-peak widths at (in millimetres); (d) ' – a chart speed (in millimetres per minute). 321.11. Silica treated with octadecylsilane, 10 mm. 321.12. Standard solution: weigh accurately approximately 5.0, 10.0, respectively, 15.0 and 20.0 mg of anhydrous quinine 100 ml flasks. Make up to the mark with methanol and shake until the quinine dissolves. All samples filtered through a 0.5 mm filter. 322. determination of quinine, the method uses the following equipment: 322.1. Laboratory equipment. 322.2. ultrasonic bath. 322.3. High-performance liquid chromatography equipment with a variable wavelength detector. 322.4. Column: length 250 mm, internal diameter 4.6 mm, packed-Silicon oxide (321.11.). Millipore filter, 322.5. FH 0.5 mm or equivalent suitable filtration equipment. 323. the determination of quinine, taken in the following order: 323.1. sample preparation: weigh accurately into a 100 ml volumetric flask, the many mu cosmetic product containing at least 10.0 mg of anhydrous quinine, add 20 ml of methanol and place the flask in an ultrasonic bath for 20 minutes. Make up to the mark with methanol. Mix the solution and then filter an aliquot portion (322.5. below). 323.2. Chromatography:. 323.2.1 flow rate: 1.0 ml/min 323.2.2. Set the detector wavelength: 332 nm. 323.2.3. capacity: entered 10 µ l of filtered solution (323.1). 323.2.4. measurements: peak area. 323.3. Calibration Curve: at least three times 10.0 ml of each standard solution (321.12.), measure the peak area and calculate the average area of each concentration. Construct the calibration curve and the battle of impeded, or is it straight. 324. the calculation shall be effected in the following order: 324.1. From the calibration curve (323.3) determines the quantity of anhydrous quinine milligrams entered volume (323.2). 324.2. concentration of anhydrous quinine in the sample, in percentage by mass (% m/m) is defined by the following formula:% (m/m) of anhydrous quinine = B-which filtered solution (323.1) 10 microlitres of anhydrous quinine determined quantities (micrograms); A-sample mass (in grams) (323.1). 325. One sample with 0.5% (m/m) of anhydrous quinine content, the difference between the results of two determinations should not exceed 0.02%. From a single sample with 0.2% (m/m) of anhydrous quinine content, the difference between the results of two determinations should not exceed 0.01% 4.27. Inorganic sulphites and hydrogen sulfite determination of demonstration and 326. With inorganic sulphites and hydrogen sulfite and the determination of the proof of the NASA method and determination of inorganic sulphites and hydrogen sulphite to Cosmas were products containing water or alcoholic phase and up to 0.2% sulphur dioxide concentrations. 27.1. Inorganic sulphites and hydrogen sulfite proof of 327. Sample is heated in hydrochloric acid, and sulphur dioxide liberated is demonstrated by smell or indicator paper with. 328. Inorganic sulphites and hydrogen sulfite method of proof of use the following reaģentus1:328.1. Hydrochloric acid (4 M). 328.2. Potassium iodate starch paper or equivalent. 329. Inorganic sulphites and hydrogen sulfite method of proof of the following equipment: 329.1. Laboratory equipment. 329.2. Flask (25 ml) with a short reflux condenser. 330. Inorganic sulphites and hydrogen sulfite prove out in the following order: 330.1. Makes the flask (329.2) about 2.5 g of the sample and add 10 ml of hydrochloric acid (328.1). 330.2. Mix and heat to boiling. 330.3. Check that emit sulphur. 27.2. Inorganic sulphites and hydrogen sulfite determination of sulphite or hydrogen sulphite 331. content of the sample, expressed as percentage by mass of sulphur dioxide. 332. acidification of the sample After release sulphur dioxide liberated the hydrogen peroxide solution. Sulphuric acid formed is titrated with a standard sodium hydroxide solution. 333. Inorganic sulphites and hydrogen sulfite method of using such reaģentus1:333.1. Hydrogen peroxide, 0.2% (m/v) (every day new). 333.2. Orthophosphoric acid (85%; = 1,75). 333.3. Methanol. 333.4. Sodium hydroxide (0.01 M), solution. 333.5. Nitrogen. 333.6. Indicator: mixture 1:1 (v/v) of methyl red (0.03% m/v in ethanol) and methylene blue (0.05% m/v in ethanol). Filter the solution. 334. Inorganic sulphites and hydrogen sulfite method uses the following equipment: 334.1. Laboratory equipment. 334.2. Distillation apparatus (Figure 7).
Figure 7 Tener (Tanner) sulphur dioxide distillation apparatus. All dimensions in mm 335. Inorganic sulphites and hydrogen sulfite determination shall be made in the following order: 335.1. Weigh accurately about 2.5 g of sample into the distillation flask A (Figure 7). 335.2. Add 60 ml water and 50 ml of methanol and mix. 335.3. Distillate tray (D) (Figure 7) pipette 10 ml of the hydrogen peroxide (333.1), 60 ml of water and a few drops of indicator (333.6. below). Add a few drops of sodium hydroxide (333.4) until the indicator turns green. 335.4. Repeat this 335.3. of the annex referred to in respect of the wash bottle E (Figure 7). 335.5. Assemble the apparatus and adjust the nitrogen flow to approximately 60 bubbles per minute. 335.6. Let in 15 ml ortho-phosphoric acid (333.2) from the funnel into the distillation flask a. 335.7. rapidly heated to boiling and then simmer gently for 30 minutes, total. detach the distillation receiver 335.8. d. Rinse the tube and then Titrate with sodium hydroxide solution (333.4) until the indicator turns green (333.6). 336. the calculation of the sulphite or hydrogen sulphite content of the sample by mass, using the formula:% m/m of sulphur dioxide =, where M-sodium hydroxide solution (333.4) molar concentration; V-titration (335.8) required sodium hydroxide (333.4) volume (ML); m-sample (335.1) mass (in grams). 337. From a single sample with 0.2% (m/m) content of sulphur dioxide the difference between the results of two determinations carried out should not exceed 0.006% dioxide by smell or indicator paper (328.2) 4.28. Alkali proof of chlorate and determination 338. With alkali proof of chlorate and determination method and determination of chlorates in toothpastes and other cosmetic products. 28.1. Alkali proof of chlorate Chlorate of 339. separated from other halates by thin layer chromatography and identified by the oxidation of iodide to form iodine. 340. Alkali proof of chlorate method uses the following reaģentus1: Solution: fresh 340.1. prepared potassium chlorate, bromate and iodate aqueous solutions of 0.2% (m/v). 340.2. Development solvent: ammonia solution 28% (m/v) acetone/butanol 60:130:30 (v/v/v). 340.3. Potassium Iodide aqueous solution 5% (m/v). 340.4. starch solution 1 – 5% (m/v). 340.5. Hydrochloric acid (1 M). 340.6. Ready to coated cellulose thin-layer plates (0.25 mm). 341. Alkali proof of chlorate method uses the standard equipment for thin layer chromatography. 342. Alkali proof make chlorate in the following order: 342.1. Extract about 1 g of the sample with water, filter, and dilute to about 25 ml. 342.2. On a plate (340.6) apply 2 ml of the solution (342.1. bottom) and 2 ml aliquots of each of the three reference solutions (340.1. below). Extra wide Chamber 342.3. and upstream in developing hromotogrāfij about three-quarters of the length of the plate with solvent (340.2). 342.4. camera removed from and allow the solvent to evaporate. Evaporation can take up to two hours. 342.5. Spray the plate with potassium iodide (340.3.) and allow to dry for about five minutes. 342.6. Spray the plate with starch solution (340.4.) and allow to dry for about five minutes. 342.7. Spray the plate with hydrochloric acid (340.5). 343. If the sample contains the chlorate, after half an hour, the blue (Brown) spots with an Rf value approximately 0,7 – 0,8.

RF Halogenāt 0-0,2 iodate Bromate 0,5 0,6 0,7 – 0,8 Bromate chlorate iodate and respond immediately. Bromates and chlorates don't mix. 28.2. the determination of alkali-Chlorate chlorate 344. quantity of the sample as a percentage by mass of chlorate. 345. in acidic environment of Chlorate is reduced by zinc powder. With chloride determines potentiometric titration with silver nitrate solution. Similarly, before reducing down the possible halides. 346. Alkali-chlorate method uses the following reaģentus1:346.1. Acetic acid, 80% (m/m). 346.2. Zinc powder. .346.3 silver nitrate standard solution (0.1 M). 347. Alkali-chlorate method uses the following equipment: 347.1. Laboratory equipment. 347.2. Potentiometer with silver indicating electrode. 348. Alkali-chlorate determination is carried out in the following order: 348.1. sample preparation: weigh accurately a quantity m approximately 2 g centrifuge tube. Add about 15 ml acetic acid and mix thoroughly. Wait 30 minutes and centrifuge for 15 minutes at a speed of 2000 RPM transfer the supernatant to a 50 ml volumetric flask. Repeat centrifuging twice by adding 15 ml acetic acid residue. Solution containing chlorate, collected at the same volumetric flask. Make up to the mark with acetic acid. reduction of Chlorate 348.2.: take 20 ml of the solution (348.1) and add 0.6 g of zinc powder. Boil in a flask fitted with a reflux condenser. After 30 minutes of cooking, cool and filter. Rinse the flask with water. Filter and combine the filtrate with the rises. 348.3. determination of Chlorides: Titrate 20 ml solution (348.2) with silver nitrate (. 346.3) by using the potentiometer (347.2.). Also, with the silver nitrate is titrated 20 ml solution (348.1). If the product is bromine or iodine derivatives which can release after reduction bromides or iodides, titration curve is more moderation points. In this case the titrated solution (. 346.3) volume corresponding to chloride is the difference between the last and the penultimate point of growth. 349. the Chlorate content of the sample (% m/m) is calculated by the formula:% (m/m) of chlorate (Clo3-) = where V-solution (348.2) silver nitrate titration (. 346.3 underneath) volume (ML); V '-solution (348.1) 20 millilitres, of silver nitrate titration (. 346.3) volume (ML); M-silver nitrate standard solution (. 346.3) Molarity; m-sample mass (in grams). 350. From one sample with 3-5% (m/m) of the chlorate content of the difference between the results of two determinations should not exceed 0.07% 4.29. Sodium iodate demonstration and determination of sodium iodate 351.Ar proof and determination method and determination of sodium iodate cosmetic slop. 29.1. Sodium iodate 352. burden of proof sodium iodate is separated from other halates by hromat the grāfij and identified by the oxidation of iodide to form iodine. 353. Sodium iodate demonstration method uses the following reaģentus1:353.1. Standard solution: fresh prepared potassium chlorate, bromate and iodate aqueous solution 0.01% (m/v). 353.2. Development solvent. Ammonia solution 28% (m/v) acetone/butanol 60:130:30 (v/v/v). 353.3. Potassium Iodide aqueous solution 5% (m/v). 353.4. starch solution 1 – 5% (m/v). 353.5. Hydrochloric acid (1 M). 354. proving of sodium iodate method uses the following equipment: 354.1. Ready-to-use cellulose thin-layer chromatography (0.25 mm) plates. 354.2. Tlc standard. 355. Sodium iodate was performed in the following order: 355.1. Extract about 1 g of the sample with water, filter, and dilute to about 10 ml. 2 μl 355.2. Spotted this solution and 2 ml aliquots of each of the three standard solutions (353.1) on the plate (354.1) starting line. Extra wide Chamber 355.3. and ascending chromatography developed in about three-quarters of the length of the plate with solvent (353.2). 355.4. Remove the plate from the tank and allow the solvent to evaporate at ambient temperature. Evaporation can take up to two hours. 355.5. Spray the plate with potassium iodide (353.3.) and allow to dry for about five minutes. 355.6. Spray the plate with starch solution (353.4) and allow to dry for about five minutes. 355.7. Finally spray with hydrochloric (353.5). 356. If the sample contains iodate, now appear blue (possibly Brown or even after the time appear immediately) spot with an Rf value approximately 0 to 0,2. It should be noted that bromates responds immediately when an Rf of approximately 0,5-0,6 and chlorates, after about 30 minutes if the Rf value is 0,7 – 0,8 respectively. 29.2. determination of sodium iodate 357. Sodium iodate content is expressed as percentage by mass of sodium iodate. 358. Sodium iodate is dissolved in water and determined by high-performance liquid chromatography, sequentially using reversed-phase C18 column and an anion-exchange column. 359. Sodium iodate method uses the following reaģentus1, 2:359.1. Hydrochloric acid (4 M). 359.2. Sodium sulphite in water solution, 5% (m/v). 359.3. Sodium iodate stock solution. Prepared standard solutions, which contain 50 mg sodium iodate to 100 ml of water. 359.4. Potassium dihidrogēnortofosfāt. disodium hydrogenorthophosphate; 359.5. 2H2O. 359.6. HPLC mobile phase: dissolve 3.88 g potassium dihydrogenorthophosphate 1.19 g disodium hydrogenorthophosphate and the 2H2O (359.5) 1 litre of water. The pH of the solution obtained is 6.2. Universal indicator paper, 359.7. pH 1-11.360. Sodium iodate method uses the following equipment: 360.1. Laboratory equipment. 360.2. Round paper filter with a diameter of 110 mm, Schleicher and Schuell no 575, or equivalent. 360.3. High-performance liquid chromatograph with a variable wavelength detector. column: length 360.4 120 mm, internal diameter 4.6 mm, number-two consecutive connected parts: first-cleosil R 5 C18 or equivalent Not column-Vydac TM,-301-SB or equivalent column. 361. Sodium iodate determination is carried out in the following order: 361.1. sample preparation: 361.1.1. Liquid samples (shampoos): 361.1.1.1. Weigh accurately approximately 1.0 g sample in a 10 ml graduated test tube or flask, which is glass stopper. 361.1.1.2. Make up to the mark with water and mix. 361.1.1.3. filter if necessary. 361.1.1.4. HPLC, determine the iodate in the solution in accordance with this annex, 361.2. section. 361.1.2. Solid samples (SOAP): 361.1.2.1. part of the grind of the sample and weigh accurately approximately 1.0 g 100 ml graduated cylinder test quantity of Glass stoppered. 361.1.2.2. Make up to 50 ml with water and shake vigorously for one minute. 361.1.2.3. centrifuge and filter through a filter paper or allow the mixture to stand for at least one night. 361.1.2.4. Shake gelatinous solution and filter through a filter paper. 361.1.2.5. determine the iodate in the filtrate, HPLC, in accordance with this annex 362.2. section. 361.2. Chromatography:. 361.2.1 flow rate: 1 ml/min. detector wavelength 361.2.2.: 210 nm. 361.2.3. Enter volume: 10 ml. 361.2.4. measurements: peak area. 361.3. Calibration: 361.3.1. pipette respectively 1.0, 2.0, 5.0 pipette 10.0 and 20.0 ml, sodium iodate stock solution (359.3) 50 ml volumetric flasks. 361.3.2. Make up to the mark and mix. 361.3.3. solutions thus obtained is 0.01, 0.02, 0.05 respectively, 0.10 and 0.20 mg sodium iodate per ml respectively. 361.3.4. Enter 10 μl of each standard iodate dose solution liquid chromatograph and hromatograf. 361.3.5. determine the peak area for iodate and plot a curve, peak area to the sodium iodate concentration. 362. Calculate the sodium iodate content as a percentage by mass (% m/m), using the formula:% (m/m) of sodium iodate =, where m-amount of test sample (361.1) mass (in grams); V-the total volume of the sample solution (ML) obtained in accordance with this subparagraph annex 361.1.; c – sodium iodate concentration (milligrams per millilitre), obtained from the calibration curve (361.3). 363. One sample with a 0.1% (m/m) of sodium iodate content, the difference between the results of two determinations must not exceed 0.002% 364 4. approval shall be determined as follows: 364.1. Principle: in the acidified cosmetic solution with iodate (IO3-) sulphite is reduced to iodide (I) and the solution obtained by HPLC research. If peak retention time which corresponds to the retention time of iodate disappears after treatment with sulphite, the original peak can most probably be attributed to iodate. 364.2. Procedure: 364.2.1. conical flask transfer by pipette pipette 5 ml of the sample solution obtained in accordance with this annex 361.1. section. 364.2.2. With hydrochloric acid (359.1) adjust the pH of the solution to 3 or lower. Check with the universal indicator paper. 364.2.3. Add three drops of sodium sulphite solution (359.2) and mix. 364.2.4. Inject 10 ìl of solution liquid chromatograph. 364.2.5. Compare this chromatogram with the chromatogram with that same sample obtained in accordance with this annex 361. section. 30. the burden of proof and silver nitrate in cosmetic products 30.1. proof silver nitrate in cosmetic products By 365. silver nitrate method of proof, proof silver nitrate as silver in cosmetic products on the water base. 366. Silver proof characteristic of white precipitate formed with chloride ions. 367. The silver nitrate method of proof uses the following reaģentus1:367.1. Hydrochloric acid solution, 2 M ammonia solution: 367.2. concentrated ammonium hydroxide solution (d20 = 0.88 g/ml) diluted with the same quantity of water and mix. 367.3. Nitric acid solution, 2 M. 368. Silver nitrate method of proof used in such equipment. 368.1. laboratory standard equipment. 368.2. Centrifuge. 369. proof silver nitrate is carried out in the following order: 369.1. Approximately 1 gram of the sample by centrifuge tube add 2 M hydrochloric acid solution until the end of the precipitation, mix and centrifuge. 369.2. Discard the supernatant liquid and wash the precipitate once with five drops of cold water. Decant mazgājum. 369.3. precipitate centrifuge tube add some water. Heat to boiling and stir. 369.4. centrifuge hot, supernatant. 369.5. Precipitate add a few drops of ammonia solution (367.2. below), mix and centrifuge. one drop of 369.6. supernatant to a slide Add a few drops of 2 M nitric acid solution. 369.7. White precipitate indicates the presence of silver. 30.2. Silver nitrate in cosmetic products 370. With the silver nitrate method determines the silver nitrate as silver in cosmetic products intended for colouring eyelashes or eyebrows. 371. Silver products is determined by atomic absorption spectrometry. 372. The silver nitrate method uses the following reaģentus1:372.1. Nitric acid solution, 0.02 M. Silver standard solutions: 372.2.372.2.1. Reserve silver standard solution, 1000 µ g/ml in 0.5 M nitric acid solution (SpectrosoL or equivalent). 372.2.2. Silver standard solution, 100 µ g/ml: transfer by pipette 10 ml of the silver standard solution (372.2.1) into a 100 ml volumetric flask. Make up to volume with 0.02 M nitric acid solution and mix. This solution uses fresh and stored in a dark glass bottle. 373. The silver nitrate method uses the following equipment: 373.1. laboratory standard equipment. 373.2. Atomic Absorption Spectrophotometer equipped with a silver hollow cathode lamp. 374. Silver nitrate test is performed in the following order: 374.1. Preparation of the sample: 374.1.1. Weigh accurately approximately 0.1 g (m gram) of an homogeneous sample of the product. 374.1.2. Transfer quantitatively into a one-litre volumetric flask and make up to volume with 0.02 M nitric acid solution and mix. 374.2. Atomic absorption spectrometry: 374.2.1. of the flame: air-acetylene. 374.2.2. Wavelength: 338.3 nm 374.2.3. Background: the corrections required. 374.2.4. Fuel condition: lean; for maximum absorption, the optimal length of the burner and combustion conditions. 374.3. Calibration: 374.3.1. pipette a number of 100-ml volumetric flasks transfer 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the stock solution, Silver (372.2.2). Each flask to the mark with 0.02 M nitric acid solution and mix. These solutions contain 1.0, 2.0, 3.0, respectively, 4.0 and 5.0 mg silver per millilitre. 374.3.2. Size of 0.02 M nitric acid solution and the absorbance of the resulting value of the calibration curve is used as the zero silver concentration. The size of each silver calibration standard (374.3.1). Plot a calibration curve of absorbance values refer to silver concentration. 374.4. Determination: measure the absorbance (374.1) absorption. From the calibration curve read off the concentration of silver meet the absorbance value of the sample. 375. Calculate the silver nitrate content of the sample, in percentage by mass (% m/m), using the formula:% (m/m) of silver nitrate =, where m-test sample (374.1) mass (in grams); c – silver in the sample concentration (374.1) (micrograms per millilitre), obtained from the calibration curve. 376. One sample with 4% (m/m) of silver nitrate content of the difference between the results of two determinations should not exceed 0.05% (m/m) of selenium disulphide 4.31. proof and discovery of anti-dandruff shampoos 31.1. Selenium disulphide in anti-dandruff shampoos proof 377. With selenium disulphide method of proof shows selenium disulphide as selenium in anti-dandruff shampoos. 378. Selenium proves the characteristic yellow-orange colour when reacting with urea and potassium iodide. 379. Selenium disulphide demonstration method uses the following reaģentus1:379.1. concentrated (d20 = 1.42 g/ml) nitric acid. 379.2. Urea. 379.3. Potassium Iodide solution, 10% (m/v): dissolve in 100 ml of water 10 g potassium iodide. 380. Selenium disulphide demonstration method uses the following equipment: 380.1. laboratory standard equipment. 380.2. reaction chamber where volume is 100 ml. with the heating Reactor 380.3. block. 380.4. filter paper (vatmaņpapīr No 42 or equivalent) or a 0.45 µm membrane filter. 381. Selenium disulphide was performed in the following order: 381.1. reaction Chamber approximately 1 g of shampoo add 2.5 ml of nitric acid koncen'd (381.1) and allowed to react for 30 minutes approx. 150 ° C block digestor. 381.2. Izreaģējuš sample is diluted to 25 ml with water and filter through a 0.45 mm membrane filter or filter paper. 381.3. Filtrate quantity equal to 2.5 ml, add 5 ml water, 2.5 ml of urea and cook. Cool and add 1 ml of potassium iodide solution (379.3). 381.4. Yellow to orange colour which darkens rapidly demonstrates the presence of selenium. 31.2. determination of selenium disulphide in anti-dandruff shampoos 382. With selenium disulphide method determines the Selenium disulphide as selenium anti-dandruff shampoos containing selenium disulphide content of up to 4.5% (m/m). 383. the sample is allowed to react with nitric acid and the reaction product selenium determined by atomic absorption spectrometry. 384. Selenium disulfide method uses the following reaģentus1:384.1. concentrated (d20 = 1.42 g/ml) nitric acid. 384.2. Nitric acid solution, 5% (v/v): 500 ml of water in a beaker, stirring continuously, add 50 ml of concentrated nitric acid. Transfer this solution to transfer the volumetric flask and make up to the mark. 384.3. Selenium stock standard solution, 1000 mg/ml in 0.5 M nitric acid solution (SpectrosoL or equivalent). 385. Selenium disulfide method uses the following equipment. 385.1. laboratory standard equipment. 385.2. reaction chamber where volume is 100 ml. with the heating Reactor 385.3. block. 385.4. filter paper (vatmaņpapīr No 42 or equivalent) or a 0.45 mm membrane filter. 385.5. Atomic Absorption Spectrophotometer equipped with a selenium hollow cathode lamp. 386. the determination of selenium disulphide in the following order: 386.1. Preparation of the sample: 386.1.1. reaction chamber accurately weigh approximately 0.2 g (m gram) of an homogenous sample of shampoo. 385.1.2. Add 5 ml of concentrated nitric acid and allows 150 ° C temperature respond one hour block digestor. 386.1.3. The solution allows you to cool and dilute to 100 ml with water. Filter through a filter paper or a 0.45 mm membrane filter and filter the solution store. 386.2. Atomic absorption spectrometry: 386.2.1. of the flame: air-acetylene; 386.2.2.: 196.0 nm wavelength; 386.2.3. Background correction: required; 386.2.4. Fuel condition: lean; for maximum absorption, the optimal length of the burner and combustion conditions. 386.3. Calibration: 386.3.1. pipette a number of 100-ml volumetric flasks transfer 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the stock solution, selenium (383.3). Each flask to the mark with 5% (v/v) nitric acid solution and mix. These solutions contain 10, 20, 30, 40 and 50 mg selenium per millilitre. 386.3.2. Size 5% nitric acid solution and the absorbance of the resulting value of the calibration curve is used as the zero selenium concentration. The size of each selenium calibration standard (386.3.1). Plot the calibration curve, the absorbance values against the Selenium concentration. 386.4. Detection: 386.4.1. Measure the absorbance of the sample solution (386.1.3). 386.4.2. From the calibration curve read off the concentration of selenium corresponding to the absorbance value obtained for the sample solution. 387. the calculation of selenium disulphide content of the sample, in percentage by mass (% m/m), using the formula:% (m/m) of selenium disulphide =, where m-test sample (386.1.1) mass (in grams); c-selenium concentration in the sample solution (386.1.3) (micrograms per millilitre), obtained from the calibration curve. 388. One sample with 1% (m/m) of selenium disulphide content of the difference between the results of two determinations should not exceed 0.05% (m/m) of soluble barium 4.32. determination of strontium from pigments and that is the form of salts or lakes 32.1. determination of soluble barium 389. With soluble barium method performs the extraction of soluble barium from pigments and determination in the form of salts or lakes. 390. The Pigment is extracted with 0.07 M hydrochloric acid solution under defined conditions and the quantity of barium in the extract determined by atomic absorption spectrometry. 391. the soluble barium method uses the following reaģentus1:391.1. Absolute ethanol. 391.2. Hydrochloric acid solution, 0.07 M. 391.3. Hydrochloric acid solution, 0.5 m. 391.4. Potassium Chloride 8% solution (w/v): dissolve 16 g of potassium chloride in 200 ml of 0.07 M hydrochloric acid solution. 391.5. Barium standard solution: 391.5.1. Barium stock standard solution, 1000 mg/ml in 0.5 M nitric acid solution (SpectrosoL or equivalent). 391.5.2. Barium standard solution, 100 mg/ml: transfer by pipette 20.0 ml of the barium standard solution (391.5.1) into a 100 ml volumetric flask. Make up to volume with 0.07 M nitric acid solution and mix. 392. the soluble barium method uses the following equipment: 392.1. Laboratory equipment. 392.2. pH meter with an accuracy of ± 0.02 units. 392.3. Mechanical Shaker. 392.4. Membrane Filter, pore size 0.45 mm. is 392.5. Atomic Absorption Spectrophotometer equipped with a barium hollow cathode lamp. 393. the determination of soluble barium in the following order: 393.1. Preparation of the sample: 393.1.1. Conical flask weigh accurately approximately 0.5 g (m gram) of pigment. To ensure sufficient capacity for an effective search, does not use flasks, of capacity less than 150 ml. 393.1.2. With pipettes help add 1.0 ml of ethanol and swirled the flask to ensure thorough wetting of the pigment. From a burette, add exactly the quantity of 0.07 M hydrochloric acid solution, which requires that the volume of acid to the pigment mass is exactly 50 millilitres per gram. And overall extracting ethanol capacity V ml. shake the contents of the flask for five seconds to ensure that the ingredients are well mixed. 393.1.3. pH meter size for suspension, and to pH, if it is above 1.5, add 0.5 M drop by hydrochloric acid solution until the pH reaches 1.4-1.5.393.1.4. Flask and shake for 60 minutes on a mechanical Shaker. Shaker run fast enough to form a foam. Filter through a 0.45 mm membrane filter and collect the filtrate. Do not centrifuge the extract before filtering. Transfer by pipette 5.0 ml of the filtrate into a 50 ml volumetric flask; make up to volume with 0.07 M hydrochloric acid solution and mix. This solution is also used for the determination of strontium (32.2. subchapter). 393.1.5. pipette 5.0 ml potassium chloride solution (391.4) and the diluted filtrate (393.1.4) an aliquot (WBA ml) into a 100 ml volumetric flask, to ensure a concentration 3 to 10 mg barium per millilitre (beginning would fit 10 ml aliquot part). Make up to volume with 0.07 M hydrochloric acid solution and mix. 393.1.6. On the same day by atomic absorption spectrometry, determine the barium concentration of the solution (393.1.5). 393.2. Atomic absorption spectrometry: 393.2.1. of flame: nitrous oxide-acetylene. 393.2.2. Background correction: not required. 393.2.3. Fuel condition: lean; for maximum absorption, the optimal length of the burner and combustion conditions. 393.3. Calibration: 393.3.1. pipette a number of 100-ml volumetric flasks transfer 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the barium, standard solution (391.5.2). To each flask transfer by pipette 5.0 ml potassium chloride solution (391.4); make up to volume with 0.07 M hydrochloric acid solution and mix. These solutions contain 2.0, 4.0, 6.0, respectively, 8.0 and 10.0 mg barium per millilitre. Similarly, prepare a blank solution without the barium standard solution. 393.3.2. The size of the blank solution (393.3.1) and the resulting absorption value in the calibration curve is used as the zero barium concentration. The size of each barium calibration standard (393.3.1). Draws a calibrated curve of absorbance values against the concentration of barium. size: 393.4. Determination of the sample solution (393.1.5). From the calibration curve read off the concentration of barium corresponding to the absorbance value obtained for the sample solution. 394. the soluble barium content (% m/m) of the pigment is given by the formula:% (m/m) of soluble barium =, where m-test sample (393.1.1) mass (in grams); c – soluble barium concentration of the sample solution (393.1.5) (micro grams per millilitre), obtained from the calibration curve; G – extracting substances total volume (ML) (393.1.2); WB-extract volume (ML) (393.1.5). 395. the best repeatability of this method reports, if the soluble barium content of 2% (m/m), shall be 0.3% 4 notes. 1. Under certain conditions the barium absorbance can be improved with calcium. This can be countered by adding magnesium ions concentration of 5 g per litre (magnesium as modifier for the determination of emission of bari by flame atomic spectrometry '. Jerrow, m. et al., Analytical proceedings, 1991, 28, 40). 2. Inductively coupled plasma – optical emission spectrophotometry is permissible as a flame atomic absorption spectrometry in the alternative. 32.2. determination of soluble strontium 396. With soluble strontium method performs the extraction of soluble strontium from pigments and discovery, which is the form of salts or lakes. 397. The Pigment is extracted with 0.07 M hydrochloric acid solution under defined conditions, and the amount of strontium in the extract quantitatively determined by atomic absorption spectrometry. 398. The soluble strontium method uses the following reaģentus1:398.1. Absolute ethanol. 398.2. Hydrochloric acid solution, 0.07 M potassium chloride 398.3.8% (m/v) solution: dissolve 16 g of potassium chloride in 200 ml of 0.07 M hydrochloric acid solution. 398.4. Strontium standard solution: 398.4.1. Strontium standard solution, 1000 µ g/ml in 0.5 M nitric acid solution (SpectrosoL or equivalent). 398.4.2. strontium standard solution, 100 mg/ml: transfer by pipette 10.0 ml of the stock standard solution of strontium (398.4.1) into a 100 ml volumetric flask. Make up to volume with 0.07 M hydrochloric acid solution and mix. 399. The soluble strontium method uses the following equipment: 399.1. laboratory standard equipment. 399.2. Membrane Filter, pore size 0.45 mm. is 399.3. Atomic Absorption Spectrophotometer equipped with a strontium hollow cathode lamp. 400. The soluble strontium determination is carried out in the following order: 400.1. Preparation of the sample (the solution prepared in accordance with 393.1.4. of this annex, using soluble strontium content): 400.1.1. Pipette 5.0 ml potassium chloride solution (398.3. below) and an aliquot (WSr ml) of diluted portion of the filtrate (393.1.4) to a 100-ml volumetric flask, providing a concentration of 2-5 mg strontium per millilitre (beginning would be appropriate for the 25 ml aliquot part). Make up to volume with 0.07 M hydrochloric acid solution and mix. 400.1.2. On the same day by atomic absorption spectrometry, determine the strontium concentration of the solution (400.1.1). 400.2. Atomic absorption spectrometry: 400.2.1. of flame: nitrous oxide-acetylene. 400.2.2. Wavelength: 460.7 nm 400.2.3. Background correction: not required. 400.2.4. Fuel condition: lean; for maximum absorption, the optimal length of the burner and combustion conditions. 400.3. Calibration: 400.3.1. pipette a number of 100-ml volumetric flasks transfer 1.0, 2.0, 3.0, 4.0 and 5.0 ml of the strontium standard solution, (398.4.2). To each flask transfer by pipette 5.0 ml potassium chloride solution (398.3.), make up to volume with 0.07 M hydrochloric acid solution and mix. These solutions contain 1.0, 2.0, 3.0 4.0 respectively, and 5.0 mg strontium per millilitre. Similarly, prepare a blank solution without strontium standard solution. 400.3.2. The size of the blank solution (400.3.1) absorption, and the value of the calibration curve is used as the zero strontium concentration. The size of each strontium calibration standard (400.3.1). Plot the calibration curve, the absorption maximum values to strontium concentration. 400.4.. Measure the absorbance of the sample solution (400.1.1). From the calibration curve read off the concentration of strontium corresponding to the absorbance value obtained for the sample solution. 401. The soluble strontium content (% m/m) of the pigment is given by the formula:% (m/m) of soluble strontium =, where m-test sample (393.1.1) mass (in grams); c – soluble strontium concentration in the sample solution (393.1.1) (micro grams per millilitre), obtained from the calibration curve; G – extracting substances total volume (ML) (393.1.2); WSr-extract volume (ML) (393.1.1). 402. the best repeatability of this method reports, if the soluble strontium content of 0.6% (m/m), is 0.09% 403 4. Inductively coupled plasma – optical emission spectrophotometry is allowed of flame atomic absorption spectrometry in the alternative. 33. the showing of benzyl alcohol in cosmetic products and 33.1. demonstration of benzyl alcohol in cosmetic products With benzyl alcohol proof 404. method proves of benzyl alcohol in cosmetic products. 405. proof of benzyl alcohol in the thin-layer chromatography on silica gel plates. 406. the showing of benzyl alcohol method uses the following reaģentus1:406.1. Benzyl alcohol. 406.2. Chloroform. 406.3. Absolute ethanol. 406.4. n-pentane. 406.5. Development solvent: diethyl ether. standard solution of benzyl alcohol: 406.6.100-ml volumetric flask weigh 0.1 g of benzyl alcohol, make up to the mark with ethanol and mix. 406.7. glass TLC plates 100 x 200 mm or 200 × 200 mm, coated with 0.25 mm silica gel 60 F254. 406.8. Developer: 10% (w/v) of ethanol on the 12-molibdēnfosforskāb. 407. the showing of benzyl alcohol method uses the following equipment: 407.1. Thin-layer chromatography of standard equipment. 407.2. Chromatography tank, camera with two partitions that total size is approximately 80 × 230 × 240 mm. 407.3. Chromatography paper: vatmaņpapīr or equivalent. 407.4. Ultraviolet lamp with a wavelength of 254 nm. 408. proof of benzyl alcohol in the following order: 408.1. Preparation of the sample. weigh 1.0 g of the test product 10-ml volumetric flask. Add 3 ml of chloroform and shake vigorously until the product has dispersed. Make up to the mark with ethanol and shake vigorously until a clear or almost clear solution. 409.2. Thin layer chromatography: chromatography tank 408.2.1. saturate with n-pentane: bin back fitted cameras wall lined with chromatography paper so that the bottom edge of the paper is in the bin. 25 ml of n-pentane is transferred into the rear compartment of the solvent to the casting of the chromatography paper the visible surface. Immediately place the lid on the container and leave it for 15 minutes. 408.2.2. Makes 10 ml of the sample solution (408.1) and 10 ml of the benzyl alcohol standard solution (406.6) at suitable points on the thin-layer chromatography plate (406.7) opening line. Allow to dry. 408.2.3. pipette the front compartment of the tank pipette 10 ml of diethyl ether and immediately put the plate on the same partition (408.2.2). Quickly replace the tank cover and plate 150 mm length developed. Remove the plate from the tank grāfij hromat and allow it to dry at room temperature. 408.2.4. view the plate (408.2.3) ultraviolet light and purple spots. Spray the plate with the developers (406.8. below) and 15 minutes heated 120 ° c. Benzyl alcohol appears dark blue spot. 408.2.5. Calculation of benzyl alcohol standard solution Rf value. Dark blue spots with the same Rf value shows the presence of benzyl alcohol. Demonstration: 0.1 mg benzyl alcohol limit. 33.2. determination of benzyl alcohol in cosmetic products With benzyl alcohol detection 409. method of benzyl alcohol in cosmetic products. 410. the amount of benzyl alcohol is expressed as a percentage by mass (% m/m). 411. The sample is extracted with methanol and the amount of benzyl alcohol in the extract determined by high-performance liquid chromatography (HPLC). 412. Benzyl alcohol method uses the following reaģentus2:412.1. Methanol. in 412.2.4-ethoxyphenol. 412.3. Benzyl alcohol. 412.4. Mobile phase: methanol/water 45:55 (v/v). 412.5. Benzyl alcohol stock solution: weigh accurately into a 100 ml graduated flask approximately 0.1 g of benzyl alcohol. Make up to the mark with methanol and mix. 412.6. Internal standard stock solution: weigh accurately into a 100 ml graduated flask approximately 0.1 g of 4-ethoxyphenol. Make up to the mark with methanol and mix. 412.7. Standard solutions: into a 25 ml volumetric flask for several of this subparagraph in accordance with the specified table into benzyl alcohol stock solution (412.5) and internal standard stock solution (412.6). Make up to the mark with methanol and mix.

Standard solution of benzyl alcohol concentration the concentration of 4-ethoxyphenol (412.5) added to the volume (ml) mg/ml (*) (412.6) added to the volume (ml) mg/ml (*) (I) (II) 1.0 2.0 80 40 20 0.5 2.0 2.0 2.0 80 80 80 (iii) (IV) 3.0 V 2.0 2.0 5.0 200 120 80 80 (*) these values correspond to the concentration of the standard solution, which is prepared with benzyl alcohol solution (412.5. point.) and 4-ethoxyphenol (412.6) solution that contain exactly 0.1% (m/v) benzyl alcohol and just 0.1% (m/v) 4-ethoxyphenol.

413. Benzyl alcohol method uses the following equipment: 413.1. laboratory standard equipment. 413.2. High-performance liquid chromatography equipment with a variable-wavelength UV detector and 10 ml injection loop. 413.3. Analytical column: 250 × 4.6 mm stainless steel column packed with 5 mm Spherisorb ODS, or equivalent. 413.4. Water bath. 413.5. ultrasonic bath. 413.6. Centrifuge. 413.7. Centrifuge Tubes, 15 ml. 414. determination of benzyl alcohol in the following order: 414.1. Sample preparation: centrifuge tube 414.1.1. weigh accurately approximately 0.1 g (m gram) of sample and add 5 ml of methanol. 414.1.2. Heat for 10 minutes in a water bath at 50 ° C, then the tube in an ultrasound bath until the sample is completely dispersed. 414.1.3. Cool for 5 minutes and then centrifuge at 3500 RPM. 414.1.4. The supernatant into a 25 ml volumetric flask. 414.1.5. Re-extract the sample with 5 ml of methanol. The extracts are combined into a 25 ml graduated flask. 414.1.6. With the pipette transfer 2.0 ml of internal standard stock solution (412.6) to a 25 ml volumetric flask. Make up to the mark with methanol and mix. This solution uses this annex 414.4. determination referred to in subparagraph. 414.2. Chromatography: 414.2.1. Installed in high-performance liquid chromatography equipment (413.2.). Adjust the mobile phase (412.4) flow rate 2.0 ml per minute. 414.2.2. Uv detector wavelength set at 210 nm. 414.3. Calibration: 414.3.1 from each of the benzyl alcohol standard solution (412.7) inject 10 ml of the benzyl alcohol and the 4-ethoxyphenol peaks and regions. 414.3.2. for each benzyl alcohol standard solution (412.7) calculate the benzyl alcohol and the 4-ethoxyphenol peak area ratio. Plot a calibration curve using these ratios as the ordinate and the corresponding benzyl alcohol in mg per millilitre, the focus as the abscissa. 414.4. Detection: 414.4.1. From the sample for each benzyl alcohol (414.1.6) inject 10 ml of the benzyl alcohol and the 4-ethoxyphenol peaks and regions. Calculate the benzyl alcohol and the 4-ethoxyphenol peaks. Repeat this procedure with 10 ml of the sample solution in aliquots, to obtain consistent results. 414.4.2. From the calibration curve (414.3.2) reads the concentration of benzyl alcohol corresponding to the peak area ratio of benzyl alcohol to 4-ethoxyphenol peaks. 415. benzyl alcohol content of the sample, is calculated and expressed as a percentage by mass, using the formula:% (m/m) of benzyl alcohol =, where m-test sample (414.1.1) mass (in grams); (c) the concentration of benzyl alcohol in the sample — (414.1.6) (micrograms per millilitre), obtained from the calibration curve. 416. One sample with 1% (m/m) of benzyl alcohol content, the difference between the results of two determinations in parallel should not exceed 0.10% 4.

34. demonstrating zirconium and zirconium, aluminium and chlorine in antiperspirants, which is not in the form of aerosol 34.1. Zirconium With zirconium 417. burden of proof method of proof demonstrating zirconium antiperspirants for cosmetic products which do not. 418. zirconium proves characteristic of sarkanviolet sediment that occurs with the alizarīnsarkan's strong acid environment. 419. Zirconium method of proof uses the following reaģentus1:419.1. concentrated (d20 = 1.18 g/ml) of hydrochloric acid; 419.2. Alizarin red S (CI. 58005) solution: 2% (m/v) of sodium alizarīn sulfonate in aqueous solution. 420. the method of demonstrating zirconium used standard laboratory equipment. 421. proof of Zirconium in the following order: 421.1. Approximately 1 g of sample in a test tube add 2 ml of water. Stopper and shake. 421.2. Add three drops of Alizarin red S solution and then in 2 ml of concentrated hydrochloric acid. Stopper and shake. 421.3. Stand for about two minutes. Sarkanviolet of uzpeldējum and 421.4. precipitate indicates the presence of zirconium. 21.3. determination of zirconium in zirconia 422. detection method By determine the zirconium in aluminium zirconium chloride hydroxide complexes up to a maximum concentration of zirconium 7.5% (m/m) products that are not antiperspirants. 423. zirconium is extracted from the product acid environment and determined by flame atomic absorption spectrometry. 424. Zirconium method uses the following reaģentus1:424.1. concentrated (d20 = 1.18 g/ml) of hydrochloric acid. 424.2. Hydrochloric acid solution, 10% (v/v): 500 ml of water in a beaker, stirring continuously, add 100 ml of concentrated hydrochloric acid. Transfer this solution to a graduated flask and make up to the mark with water. 424.3. Strontium standard solution, 1000 µ g/ml in 0.5 M hydrochloric acid solution (SpectrosoL or equivalent). 424.4. Aluminium chloride (hydrogenated) [AlCl3 · 6h2o]: 22.6 g of aluminium reagents chloride in 250 ml of dissolved heksahidrāt 10% (v/v) hydrochloric acid solution (424.2). 424.5. Ammonium chloride reagent: dissolve 5.0 g of ammonium chloride in 250 ml of 10% (v/v) hydrochloric acid solution (424.2). 425. Zirconium method uses the following equipment: 425.1. laboratory standard equipment. 425.2. Heater with magnetic stirrer. 425.3. filter paper (vatmaņpapīr No 41 or equivalent). 425.4. Atomic Absorption Spectrophotometer equipped with a zirconium hollow cathode lamp. 426. determination of Zirconium in the following order: 426.1. Preparation of the sample: 426.1.1. Weigh accurately approximately 1.0 g (m gram) of an homogeneous sample of the product 150 ml beaker. Add 40 ml of water and 10 ml of concentrated hydrochloric acid (424.1). 426.1.2. Place the beaker on a heater with magnetic stirrer. Begin to stir and heat to boiling. To prevent rapid drying out, cover the beaker with a glass. Boil for five minutes, remove the beaker from the heat and cool to room temperature. 426.1.3. The contents of the beaker through the filter paper in the filter 100 ml volumetric flask. Rinse the beaker with two 10 ml water and add mazgājum after filtering the contents of the flask. Make up to the mark with water and mix. This solution is also used for aluminum determination (subsection 3). 426.1.4. With the pipette to a 50 ml volumetric flask 20.00 ml of the sample into a (426.1.3), 5.00 ml of the aluminium chloride reagent (424.4) and 5.00 ml of the ammonium chloride reagent (424.5). Make up to the mark with 10% (v/v) hydrochloric acid solution (424.2) and mix. 426.2. Atomic absorption spectrometry: 426.2.1. of flame: nitrous oxide-acetylene. 426.2.2.: 360.1 nm wavelength. 426.2.3. Background correction: not required. 426.2.4. The combustion conditions: rich; for maximum absorption, the optimal length of the burner and combustion conditions. 426.3. Calibration: 426.3.1. pipette in several 50-ml volumetric flasks transfer 5.00, 10.00, 15.00, 20.00 and 25.00 ml of the stock standard solution of zirconium (424.3. below). Each pipette 5.00 ml in a volumetric flask is filled with aluminium chloride reagent (424.4) and 5.00 ml of the ammonium chloride reagent (424.5). Make up to the mark with 10% (v/v) hydrochloric acid solution (424.2) and mix. These solutions contain 100, 200, 300, respectively, 400 and 500 mg of zirconium per millilitre. Similarly, prepare a blank solution without the zirconium standard solution. 426.3.2. The size of the blank solution (426.3.1) and the resulting absorption value in the calibration curve is used as the zero zirconium concentration. The size of each zirconium calibration standard (426.3.1). Plot a calibration curve of absorbance values refer to zirconium concentration. 426.4.. Measure the absorbance of the sample solution (426.1.4). From from the calibration curve read off the concentration of zirconium corresponding to the absorbance value of the sample. 427. Calculate the zirconium content of the sample, in percentage by mass (% m/m), using the formula:% (m/m) of zirconium =, where m-test sample (426.1.1) mass (in grams); (c) the concentration of zirconium in the sample — (426.1.4) (micrograms per millilitre), obtained from the calibration curve. 428. From one sample to the 3.00% (m/m) of zirconium content of the difference between the results of two determinations should not exceed 0.10% (m/m) 429 4. Inductively coupled plasma-optical emission spectrometry is permitted flame atomic absorption spectrometry in the alternative. 3. determination of aluminium with aluminium 430. method of setting down the aluminum aluminum circus the nij chloride hydroxide complexes up to a maximum concentration of 12% aluminium (m/m) products that are not antiperspirants. 431. Aluminium is extracted from the product acid environment and determined by flame atomic absorption spectrometry. 432. Aluminium method uses the following reaģentus1:432.1. concentrated (d20 = 1.18 g/ml) of hydrochloric acid. 432.2. Hydrochloric acid solution, 1% (v/v): 500 ml of water in a beaker, stirring continuously, add 10 ml of concentrated hydrochloric acid. Transfer this solution to a graduated flask and make up to the mark with water. 432.3. Aluminium stock standard solution, 1000 µ g/ml in 0.5 M nitric acid solution (SpectrosoL or equivalent). 432.4. Potassium Chloride reagent: dissolve 10.0 g of potassium chloride in 250 ml of 1% (v/v) hydrochloric acid solution. 433. Aluminium method uses the following equipment: 433.1. laboratory standard equipment. 433.2. Atomic Absorption Spectrophotometer equipped with an aluminium hollow cathode lamp. 434. Aluminium test is performed in the following order: 434.1. Preparation of the sample: 434.1.1. for the determination of the content of aluminium used in the solution prepared in accordance with 426.1.3. of this annex. 434.1.2.100-ml volumetric flask transfer by pipette 5.00 ml of the sample and pipette 10.00 ml of the potassium chloride reagent. Make up to the mark with 1% (v/v) hydrochloric acid solution and mix. 434.2. Atomic absorption spectrometry: 434.2.1. of flame: nitrous oxide-acetylene. 434.2.2. Wavelength: 309.3 nm 434.2.3. Background correction: not required. 434.2.4. The combustion conditions: rich; for maximum absorption, the optimal length of the burner and combustion conditions. 434.3. Calibration: 434.3.1.100 ml volumetric flasks transfer 1.00, 2.00, 3.00, 4.00 and 5.00 ml of the stock standard solution of aluminium. To each volumetric flask transfer by pipette 10.00 ml of the potassium chloride reagent, make up to the mark with 1% (v/v) hydrochloric acid solution and mix. These solutions contain 10, 20, 30, 40 and 50 µ g of aluminium per millilitre. Similarly, prepare a blank solution without aluminium standard solution. 434.3.2. Measure the absorbance of the blank solution and get the value of the calibration curve is used as the zero aluminium concentration. The size of each of the standard calibrated aluminium absorption. Plot the calibration curve, the absorbance values against the aluminum concentration. 434.4. Detection: 434.4.1. Measure the absorbance of the absorption. 434.4.2. From the calibration curve read off the concentration of aluminium corresponding to the absorbance value obtained for the sample solution. 435. the calculation of the aluminium content of the sample, in percentage by mass using the formula:% (m/m) of aluminium = m – which of the sample taken for the determination of mass (in grams); c – aluminium in the sample concentrations (micrograms per millilitre), obtained from the calibration curve. 436. One sample with 3.5% (m/m) of aluminium content of the difference between the results of two determinations should not exceed 0.10% (m/m) 4 437. Inductively coupled plasma – optical emission spectrophotometry is allowed of flame atomic absorption spectrometry in the alternative. 21.4. determination of Chlorine With chlorine of 438. method of determining chlorine as chloride ion in aluminium zirconium chloride hydroxide complexes, which are not antiperspirants. 439. Chloride ion products, potentiometric titration with silver nitrate standard solution. 440. The chlorine method uses the following reaģentus1:440.1. Concentrated nitric acid (d20 = 1.42 g/ml). 440.2. Nitric acid solution, 5% (v/v): 250 ml water in a beaker, stirring rush odd, add 25 ml of concentrated nitric acid. Transfer this solution to a 500 ml volumetric flask and make up to the mark with water. 440.3. Acetone. 440.4. Silver nitrate, 0.1 M volumetric solution (AnalaR or līdzvēr bigger). 441. The chlorine method uses the following equipment: 441.1. standard laboratory equipment. 441.2. Heater with magnetic stirrer. 441.3. Silver electrode. calomel reference electrode 441.4. pH/441.5. millivoltmeter, suitable for potentiometric titration for. 442. Chlorine test is performed in the following order: 442.1. Preparation of the sample: 442.1.1. Weigh accurately approximately 1.0 g (m gram) of an homogeneous sample of the product 250 ml beaker. Add 80 ml of water and 20 ml of 5% (v/v) nitric acid solution; 442.1.2. Place the beaker on a heater with magnetic stirrer. Begin to stir and heat to boiling. To prevent rapid drying out, cover the beaker with a glass. Boil for five minutes, remove the beaker from the heat and cool to room temperature; 442.1.3. Add 10 ml of acetone, dip electrodes (441.3. and 441.4. bottom) below surface of solution and commence stirring. Titrate potentiometrically with 0.1 M silver nitrate solution and plot a differential curve to determine the balance point (V ml). 443. Calculate the chlorine content of the sample, in percentage by mass, using the formula:% (m/m) of chlorine = m – which of the sample taken for the determination of mass (in grams); v-0.1 M silver nitrate volume (ML), the balance point in the titration. 444. From a single sample with 4% (m/m) of chlorine content of the difference between the results of two determinations should not exceed 0.10% (m/m) of aluminium atoms 4.34.5. the relationship of the atoms to zirconium and aluminum and zirconium atoms to chlorine atoms calculation of aluminium atoms 445. to zirconium atoms calculate. Al: Zr ratio is calculated by the formula: Al: Zr ratio = 446. Aluminium and zirconium atoms to chlorine atoms. (Al + Zr): Cl ratio is calculated by the formula: Al: Zr ratio = 35. Hexamidine, dibromohexamidine, dibromopropamidine and chlorhexidine evidence and discovery, With 447. hexamidine dibromohexamidine, dibromopropamidine and chlorine proof and heksidīn detection method in cosmetic products lays down quantitative and qualitative hexamidine and its salts, including the isethionate and the 4-hydroxy benzoates, dibromohexamidine and its salts, including the isethionate, dibromprop-midīn and its salts, including the isethionate, chlorhexidine diacetate and dihydrochloride, diglukonāt. 448. Hexamidine, dibromohexamidine, dibromopropamidine and hlorheks to DIN concentration is given as a percentage by mass (% m/m). 449. Proof and shall be carried out over the Ionic by reversed-phase high-performance liquid chromatography (HPLC), followed by a spectrum of ultraviolet photometry. Hexamidine, dibromohexamidine, dibromopropamidine and hlorhek sidīn demonstrates the retention time of the chromatographic column. 450. Hexamidine, dibromohexamidine, dibromopropamidine and hlorheks to the Dean and probative method uses the following reaģentus1, 2:450.1. Methanol. 450.2.1-heptanesulphonic acid, sodium salt monohydrate. 450.3. Acetic acid, glacial (d20 = 1.05 g/ml). 450.4. sodium chloride. 450.5. Mobile phase: 450.5.1. Solvent I: 0.005 M 1-heptanesulphonic acid, sodium salt, monohydrate (450.2) solution in methanol (450.1), until a pH of 3.5 with glacial acetic acid adjusted (450.3). 450.5.2. Solvent II: 0.005 M 1-heptanesulphonic acid, sodium salt Mono hydrate (450.2) aqueous pH adjusted up to 3.5 with glacial acetic acid (450.3). 450.5.3. If you need to improve the shape of the peaks, the mobile phase can be modified and prepared as follows: 450.5.3.1.: dissolve 5.84 Solvent I g of sodium chloride and 1.1013 g of 1-heptanesulphonic acid, sodium salt, monohydrate 100 ml of water. Add 900 ml of methanol and glacial acetic acid (450.3) is adjusted to pH 3.5.450.5.3.2. Solvent II: 5.84 g sodium chloride, and heptane 1.1013 g of 1-sulfoskāb acid, sodium salt, monohydrate dissolved in one litre of water and adjust pH with glacial acetic acid to 3.5.450.6. Hexamidine diisethionate [C20H26N4O2 · · 2c2h6o4s]. 450.7. Dibromohexamidine diisethionate [C20H24Br2N4O2 · · 2c2h6o4s]. 450.8. Dibromopropamidine diisethionate [C17H18Br2N4O2 · · 2c2h6o4s]. 450.9. Chlorhexidine diacetate [C22H30Cl2N10 · 2C2H4O2]. standard solutions: prepare 450.10. Accordingly, all four preservatives (450.6.,.,., and 450.9 450.7 450.8) 0.05% (m/v) solution in solvent I (450.5.1). 450.11.3, 4, 4 '-trichlorocarbanilide (triclocarban). 450.12.4, 4 '-Dichloro-3-(trifluormetil) karbanilīd (halokarbān). 451. Hexamidine, dibromohexamidine, dibromopropamidine and proof and hlorhek sidīn method uses the following equipment: 451.1. standard laboratory equipment. 451.2. High-performance liquid chromatograph with variable-wavelength UV detector. 451.3. Analytical column: stainless steel, length 30 cm, with 4 mm internal diameter, fitted with μ-Bondapack C18, 10 mm, or equivalent. 451.4. ultrasonic bath. 452. Hexamidine, dibromohexamidine, dibromopropamidine and hlorheks are made of quality detection of Dean, in the following order: 452.1. Preparation of the sample: 452.1.1. Weigh accurately approximately 0.5 g of sample in a 10 ml volumetric flask and make up to volume with solvent I (450.5.1). 452.1.2. Place the flask for 10 minutes in an ultrasonic bath. 452.1.3. The solution is centrifuged or filtered. 452.1.4 Filtrate or supernatant collected. chromatography. 452.2. Chromatography: 452.2.1. Mobile phase gradient.

Time (min.) the solvent I (% v/v) (450.5.1) solvent II (% v/v) (450.5.2) 0 50 50 15 65 35 30 65 35 45 50 50 452.2.2. Mobile phase (452.2.1) adjust the flow rate of 1.5 ml/min and column temperature 35 ° c. 452.2.3. Set the detector wavelength to 264 nm. 452.2.4. adjusted from each standard solution (450.10) inject 10 µL and record their chromatograms. inject 10 ìl sample 452.2.5. (452.1) and record the chromatogram. Comparing this annex 452.3.452.2.5. referred to in point (o) (o) recorded peak retention time (s) (s) (s) with the time (s) get (s) in relation to stan dartšķīdum (452.2.4), demonstrates the hexamidine, dibromohexamidine, dibromopropamidine or chlorhexidine is present. 453. Hexamidine, dibromohexamidine, dibromopropamidine and hlorheks to DIN detection carried out quantitatively in the following order: preparing standard solutions 453.1., use one of the preservatives (450.6.,.,., or 450.9 450.8 450.7.), which is not in the internal model stan darts. If this is not possible, triclocarban or halokarbān may be used: 453.1.1. This annex in proven preservative 452.3 a 0.05% (m/v) stock solution in solvent I (450.5.1). 453.1.2. a 0.05% (m/v) stock solution of the preservative chosen as in internal standard, solvent I (450.5.1). 453.1.3. for each show for the preservative, prepare four standartšķīd must, transferring to multiple 10 ml volumetric flasks the preservative (453.1.1. bottom) stock solutions and the appropriate quantity of internal standard stock solution (453.1.2) in accordance with this point in the specified table. Each flask to the mark with the solvent I (450.5.1) and mix.

Solution of internal standard stock solution Proven preservative stock solution (453.1.2) added ml (453.1.1) added ml mg/ml (*) (I) (II) 1.0 1.0 1.0 0.5 25 50 75 100 III IV 1.0 2.0 1.0 1.5 (*) these values correspond to the concentration of the preservatives shown in the standard, prepared using a stock solution containing 0.05% proven preservative directly.

453.2. Preparation of the sample: 453.2.1. Weigh accurately approximately 0.5 g (p gram) of sample into a 10 ml volumetric flask, add 1.0 ml of the internal standard solution (453.1.2) and 6 ml of solvent I (450.5.1) and mix. 453.2.2. Place the flask for 10 minutes in an ultrasonic bath. Cool. Make up to volume with solvent I and mix. Centrifuge or filter through a fluted filter paper. Collect the supernatant or filtrate, respectively, for chromatography. 453.3. Chromatography: 453.3.1. adjust the mobile-phase gradient, flow rate, column temperature and detector wavelength of the HPLC equipment length under the conditions of proof stage (452.2.1., 452.2.2. and 452.2.3.). inject 10 ml of the sample 453.3.2. (453.2.2.) and measure the peak areas. Repeat this procedure with 10 ml of the sample solution in aliquots, to obtain consistent results. Calculate the peak area, resulting from the test connection, the peak area ratio of the internal standard. 453.4. Calibration: 453.4.1. Inject 10 ml of each of the solution (453.1.3 below) and measure the peak areas. 453.4.2. For each standard solution (453.1.3) calculates the hexamidine, dibromohexamidine, dibromopropamidine or chlorhexidine peak area ratio of the internal standard peak area. Plot a calibration curve using these ratios as the ordinate and the corresponding concentrations of the identified preservative in the standard, in micrograms per millilitre, the abscissa. 453.4.3. From the calibration curve (453.4.2) reads the proven preservative in concentration, corresponding to the peak area ratio calculated in accordance with 453.3.2. of this annex. 454. Calculate the hexamidine, dibromohexamidine, dibromopropamidine or chlorhexidine content of the sample, in percentage by mass, using the formula:% (m/m) = where p-sample (453.2.1) mass (in grams); (c) the concentration of the preservatives in the sample solution – (micrograms per millilitre), obtained from the calibration curve; MW1-preservative of the basic molecular weight; Mw2 – the salt molecular weight (456). 455. One sample with a 0.1% (m/m) of the hexamidine, dibromohexamidine, dibromopropamidine or chlorhexidine content of the difference between the results of two determinations should not exceed 0.005% 4.456. Molecular weight Hexamidine C20H26N4O2 354.45 Hexamidine table diisethionate C20H26N4O2 · 2c2h6o4s 606.72 Hexamidine di is ・-p-hydroxybenzoate C20H26N4O2 · C20H24Br2N4O2 512.24 Dibromohexamidine 2C7H6O3 630.71 dibromohexamidine diisethionate C20H24Br2N4O2 · 2c2h6o4s 764.51 Dibromopropamidine C17H18Br2N4O2 · a 470.18 dibromopropamidine diisethionate C17H18Br2N4O2 · · 2c2h6o4s 722.43 Chlorhexidine C22H30Cl2N10 505.45 chlorhexidine in diacetate C22H30Cl2N10 · 2C2H4O2 625.56 chlorhexidine C22H30Cl2N10 · 2C6H12O7 897.76 diglukonāt Chlorhexidine dihydrochloride C22H30Cl2N10 · 2HCl 578.37 36. Benzoic acid , 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid qualitative and quantitative determination of cosmetic products With 457. benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid qualitative and quantitative determination method and determination of benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid in cosmetic products. Separate procedures are laid down for the determination of these preservatives, the determination of propionic acid, as well as 4-Hydroxybenzoic acid, salicylic acid, sorbic acid and benzoic acid kvantit the light fixing. 458. Quantitative specific benzoic acid, 4-Hydroxybenzoic acid, salicil acid and propionic acid quantities are expressed in free acidity as a percentage by mass. 36.1. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid identification 459. Preservatives extraction with acid/base extract analysed in chromatography, thin-layer derivatizēj a on the plate. Depending on the results of the quantum tatīv measurement results confirm the high performance liquid hromat for the grāfij or-propionic acid, by gas chromatography. 460. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid in quality detection method using such reaģentus1, 3:460.1. Acetone. 460.2. diethyl ether. 460.3. Acetonitrile. 460.4. Toluene. 460.5. n-hexane. 460.6. Liquid paraffin. 460.7.4 M hydrochloric acid. 460.8.4 M potassium hydroxide solution. 460.9. Calcium chloride, CaCl2.2H2O 460.10. Lithium carbonate, Li2CO3. 460.11.2-bromo-2′-acetonaphthone. 460.12.4-Hydroxybenzoic acid. 460.13. Salicylic acid. 460.14. benzoic acid 460.15. sorbic acid 460.16. Propionic acid. 460.17. Standard solutions: prepare all the five preservatives (460.12.,.,., 460.14 460.15 460.13. and 460.16) 0.1% (m/v) solution in diethyl ether. 460.18. Derivatization reagent: 0.5% (m/v) 2-bromo-2′-acetonaphthone solution in acetonitrile (50 mg/10 ml). This solution is prepared each week and stored in a refrigerator. 460.19. Catalyst solution: 0.3% (m/v) solution of lithium carbonate the water (300 mg/100 ml). This solution prepared immediately before use. 460.20. Developing solvent: toluene/acetone 20:5 (v/v). 460.21. Liquid paraffin/n-hexane 1:2 (v/v). 461. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid in quality detection method using conventional laboratory equipment and such equipment: 461.1. Water bath, capable of maintaining a temperature of 60 ° C. 461.2. Developing tank. 461.3. Ultraviolet light source, 254 and 366 nm. 461.4. Thin Layer plates, Kieselgel 60, without fluorescence indicator, 20 × 20 cm, layer thickness 0.25 mm with concentrating zone 2.5 × 20 cm (Merck 11845, or equivalent). 461.5. Microsyringe, 10 µ l. 461.6. microsyringe, 25 µ l. 461.7. Oven, capable of maintaining a temperature of 105 ° C. 461.8. glass tubes, 50 ml, with screw cap. 461.9. Filter paper, diameter 90 mm, Schleicher and Schull, Weissband & Of 5892, or equivalent 461.10. Universal pH indicator paper, pH 1-11.461.11.5-ml glass sample vials. 461.12. Rotary evaporator (Rotavapor or equivalent). 461.13. Hotplate. 462. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid quality test is performed in the following order: 1 242.5. sample preparation: 462.1.1. Weigh approximately 1 g of sample in a 50-ml glass tube with screw cap. Add four drops of hydrochloric acid 4 M and 40 ml of acetone. Strongly basic cosmetic products (such as toilet SOAP) should add 20 drops of hydrochloric acid 4 M. With indicator paper check that the pH is about 2. Close the tube and shake vigorously for one minute. 462.1.2. If the extraction of the preservatives into the acetone phase needs to be speeded up, gently heat the mixture to approximately 60 ° C to obtain the liquid phase. 462.1.3. Cool the solution to room temperature and filter through a filter paper into a conical flask. 462.1.4. Transfer 20 ml of the filtrate into a 200 ml conical flask, add 20 ml of water and mix. With potassium hydroxide 4 M adjust the pH of the mixture to approximately 10 with indicator paper pH measured. 462.1.5. Add 1 g calcium chloride and shake vigorously. Filter through a filter paper in a 250-ml separating funnel containing 75 ml diethylether and shake vigorously for one minute. Allow to separate the water phase, and draining it 250 ml conical flask. Discard the ether layer. Using indicator paper, adjust the pH of the aqueous solution to approximately two with hydrochloric acid 4 M. Add 10 ml of diethyl ether, stopper the flask and shake vigorously for one minute. Allow to separate the ether layer, and transfer it to the Rotary evaporator. Discard the aqueous layer. 462.1.6. Evaporate the ether layer almost dry and again dissolved in 1 ml of diethyl ether. Transfer the solution to a sample vial. 462.2. Thin layer chromatography: 462.2.1. for each standard and sample that is supposed to pick up the chromatogram, the syringe equal distances on the thin-layer hromatogrāfijasplat (462.4) start line in the concentration zone, carrying 3 µ l lithium carbonate solution (460.19.) and dry in the cold air flow. 462.2.2. Transfer the TLC hromatogrāfijasplat on stove, heated to 40 ° C, in order to keep the spots as small. With a microsyringe apply 10 µ l of each standard solution (460.17) and of the sample solution (1 242.5. bottom) on the start line of the plate the exact spots where the lithium carbonate solution is imposed. 462.2.3. Finally spotted on the boards about 15 µ l derivatization reagent (460.18) (2-bromo-2′-acetonaphthone solution) the exact spots where the reference/sample imposed solutions and the lithium carbonate solution. 462.2.4. hromatogrāfijasplat 45 minutes for thin-layer in heated oven at 80 ° C. When the platter of chilled, camera, to stabilize for 15 minutes (without the filter of the spread), it developed with the attachment in the specified 460.20 developing solvents (toluene/acetone), until the solvent front moves 15 cm (can be required in about 80 minutes). 462.2.5. Cool plate cold air stream and view the spots obtained under UV light. To improve the weak spots, thin-layer fluorescence chrome togrāfij plates can immerse in liquid paraffin/n-hexane (460.21). 463. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid qualitative determination of the calculation shall be made in the following order: 463.1. Calculation of each spot of the Rf value. 463.2. Sample and standard solutions and changes to the ultraviol of the Rf light therein. 463.3. Make a prior finding of the presence of the preservative and identical as high. High-performance thin-layer chromatography under this annex subsection, or 36.2-if it turns out that in the sample of propionic acid-gas hromat grāfij in accordance with this annex subsection 22.6. Compare the retention times with standard solution retention times. Final quality 463.4. determining the preservatives in the sample, takes into account the thin-layer chromatography and high-performance thin layer chromatography or gas chromatography results. 36.2. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid and salicylic acid determination * 464. After acidification of the sample is extracted with a mixture of ethanol and water. After filtration the preservatives determined by high-performance liquid chromatography. 465. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid and salicylic acid quantitative detection method using such reaģentus1, 2, 3:465.1. Ethanol, absolute. 465.2.4-Hydroxybenzoic acid. 465.3. Salicylic acid. 465.4. benzoic acid 465.5. sorbic acid 465.6. sodium acetate, (ch3coona.3H2O) 465.7. Acetic acid, = 1.05 g/ml. 465.8. Acetonitrile. 465.9.2 M sulphuric acid. 465.10.0.2 M potassium hydroxide solution. 465.11.2-metoksibenzoskāb. 465.12. Ethanol/water mixture: mix nine volumes of ethanol and one volume of water (2:1). 465.13. Internal standard solution: prepare a solution containing about 1 g 2-500 ml of metoksibenzoskāb ethanol/water mixture (465.12. below). 465.14. Mobile phase high performance thin layer chromatography: 465.14.1. Acetate buffer: to 1 l of water add 6.35 g sodium acetate and 20.0 ml acetic acid and mix. 465.14.2. Prepare the mobile phase by mixing nine volumes acetate buffer and one volume acetonitrile. 465.15. Preservative stock solution: weigh accurately approximately 0.05 g 4-Hydroxybenzoic acid, 0.2 g salicylic acid, 0.2 g benzoic acid and sorbīn acid 0.05 g 50 ml volumetric flask and make up to volume with ethanol/water mixture (465.12). Keep this solution in a refrigerator. The solution is stable for one week. 465.16. Standard preservative solutions: 8.00, 4.00, 2.00 respectively, 1.00 and 0.50 ml of the standard solution (465.15) into a series of 20-ml volumetric flasks. Each flask, add 10.00 ml internal standard solution (465.13) and 0.5 ml sulfuric acid 2 M. Make up to volume with ethanol/water mixture (465.12). These solutions must be freshly prepared before use. 466. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid and salicylic acid quantitative detection method using conventional laboratory equipment and such equipment: 466.1. water bath temperature set to 60 ° c. 466.2. high-performance liquid chromatograph with variable-wavelength UV detector and 10 µ l injection loop. 466.3. analytical column: stainless steel, 12.5-25 cm long, with 4.6 mm internal diameter and Nucleosil 5C18 or equivalent. 466.4. filter paper, diameter 90 mm, Schleicher and Schull, Weissband & Of 5892, or equivalent 466.5. glass tube, 50 ml, with screw cap. 466.6.5-ml glass sample vials. 466.7. boiling chips, carborundum, 2-4 mm, or equivalent. 467. Benzoic acid, 4-Hydroxybenzoic acid, sorbic acid and salicylic acid quantitative determination is carried out in the following order: 467.1. sample preparation: 467.1.1. Sample preparation without addition of internal standard, as follows: weigh 1 g of the sample into a 50-ml glass tube with screw cap. Pipette in a test tube by pipette 1.00 ml sulfuric acid 2 M and 40.0 ml ethanol/water mixture (465.12. below). Add approximately 1 g of boiling chips (466.7.), close the tube and shake vigorously for at least one minute until a homogeneous suspension is obtained. To facilitate extraction of the preservatives into the ethanol phase place the tube for exactly five minutes in a water bath kept at 60 ° C. Immediately cool the tube in a stream of cold water and store the extract at one hour to 5 ° c. Filter the extract using a filter paper. Transfer approximately 2 ml of the extract into a sample vial. Store the extract at 5 ° C and 24 stun dās quantitative determination carried out high-resolution thin-layer chromatography. 467.1.2. sample preparation, adding an internal standard, as follows: to three decimal places 1 ± 0,1 g of weigh (a gram) of sample into a 50-ml glass tube with screw cap. Pipette in a test tube by pipette 1.00 ml sulfuric acid 2 M and 30.0 ml ethanol/water mixture (465.12). Add approximately 1 g of boiling chips (466.7) and 10.00 ml internal standard solution (465.13). Close the tube and shake vigorously for at least one minute until a homogeneous suspension. To facilitate extraction of the preservatives into the ethanol phase place the tube for exactly five minutes in a water bath kept at 60 ° C. Immediately cool the tube in a stream of cold water, and one hour in the store the extract at 5 ° C. Filter the extract using a filter paper. Transfer approximately 2 ml of the filtrate into a sample vial. There the filtrate at 5 ° C for 24 hours and perform the HPLC. 467.2. High-performance liquid chromatography: 467.2.1. Chromatographic conditions: 467.2.1.1. Mobile phase: acetonitrile/acetate buffer (465.15. bottom). 467.2.1.2. adjust the flow rate of mobile phase through the column to 2,0 ± 0,5 ml/minute. 467.2.1.3. Set the detector wavelength to 240 nm. adjusted 467.2.2. Calibration: 467.2.2.1. Enter each preservative solution (465.16 below) 10 µ l dose of liquid chromatograph. 467.2.2.2. After acquired the chromatogram of preservative solution peak Standart height relationship to the internal standard. 467.2.2.3. Designed curve of each of the preservative to extend this relationship to concentrations of the standard solution. 467.2.2.4. Determine whether the calibrating with standard solutions, obtain a linear relationship. 467.2.3. Identification: 467.2.3.1. Enter 10 µ l sample extract (467.1.1) liquid chromatograph and record the chromatogram. 467.2.3.2. Enter 10 µ l one preservative solution (465.16. the bottom) and record the chromatogram. 467.2.3.3. Compare the resulting chromatogram. If the sample extract (467.1.1) there are no peaks in the chromatogram with approximately the same retention time as 2-metoksibenzoskāb (recommended internal standard), liquid chromatograph enter 10 µ l sample extract with added internal standard (467.1.2), and record the chromatogram. If the sample extract (467.1.1) in the chromatogram is interfering substances which emit at the peak, for the period of time is approximately equal to 2-metoksibenzoskāb peak of the retention period, another internal standard must be chosen (if the test is not a preservative in the sample chromatogram, this preservative can be used as an alternative to the internal standard). 467.2.3.4. Determine whether the resulting solution and chromatogram of the sample solution meet the following requirements: minimum of two 467.2.3.4.1 peak separation is at least 0.90 (peak separation defined in this annex, Figure 8).
Figure 8 the peak separation if the required separation is not achieved, use more efficient column or the regulation of the composition of the mobile phase, to ensure compliance with requirements. 467.2.3.4.2. All the resulting peak asymmetry factor As is 0.9-1.5 (peak asymmetry factor defined in this annex, Figure 9). To record the chromatogram for the determination of the asymmetry factor a chart speed recommended is at least 2 cm per minute.
Figure 9 peak asymmetry factor 467.2.3.4.3. Obtain a stable baseline. 468. the concentration of the Acid preservatives in the sample solution calculated by peak height of preservatives against the 2-metoksibenzoskāb (internal standard) peak height and the calibration curve. Calculate the benzoic acid, 4-Hydroxybenzoic acid, sorbic acid or salicylic acid content of the sample, in percentage by mass (xi), using the formula: xi% (m/m) = (100 × 20 × b)/(106 × a) = (b)/(500 × a), where the a-test (467.1.2) mass (in grams); b – the preservative concentration (µ g/ml) in the sample extract (467.1.2), read from the calibration curve. 469. Atkārtojamība4:469.1. From one sample with 0.40% 4-Hydroxybenzoic acid content, the difference between the results of two determinations in parallel should not exceed an absolute value of 0.035%. 469.2. From the same sample of benzoic acid content of 0.50% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.050%. 469.3. Out on the same sample of salicylic acid content of 0.50% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.045%. 469.4. Out on the same sample of sorbic acid content of 0.60% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.035%. * Notes. 1. Methods of coarse test results show that the amount of sulfuric acid added to extract the acids from the sample is critical, and the limits of the amount of sample should be kept within. 2. If desired, an appropriate guard column can be used. 36.3. the quantitative determination of propionic acid With 470. propionic acid carried out a quantitative detection method in the determination of quantitative propionsk the best in cosmetics if the concentration does not exceed 2%. 471. Propionic acid concentration is a cosmetic product as a percentage by mass (% m/m). 472. when propionic acid is extracted from the cosmetic, the quantum of tatīv is determined by gas chromatography as the internal standard with 2-metilpr-pionskāb. 473. the quantitative determination of propionic acid method uses the following reaģentus3:473.1. Ethanol, 96% (v/v). 473.2. Propionic acid. 473.3 2-metilpropionskāb. 473.4. Orthophosphoric acid, 10% (m/v). 473.5. Propionic acid solution: weigh accurately approximately 1.00 g (p gram) of propionic acid into a 50 ml graduated flask and make up to the mark with 96% ethanol. 473.6. Internal standard solution: weigh accurately approximately 1.00 g (e grams) of 2-metilpropionskāb 50 ml graduated flask and make up to the mark with 96% ethanol. 474. the quantitative determination of propionic acid method uses the following equipment: 474.1. Usual laboratory equipment. 474.2. Gas Chromatograph with a flame ionization detector. 474.3. glass tube (20 × 150 mm) with screw cap. 474.4. Water bath, set at 60 ° C. 474.5.10 ml glass syringe with a membrane filter (0.45 µm pore diameter). 475. the quantitative determination of propionic acid is carried out in the following order: 475.1. sample preparation: 475.1.1. sample preparation without internal standard: 475.1.1.1. Glass tube weigh approximately 1 g of sample. 475.1.1.2. Add 0.5 ml of phosphoric acid and 9.5 ml of ethanol. 475.1.1.3. Close the tube and shake vigorously. If you need to completely dissolve the lipid phase, place the tube for five minutes in a water bath, which is 60 ° c. Cool quickly under running water. 475.1.1.4. Filter part solution with membrane filter. 475.1.1.5. Filtrate chromatographed on the same day. 475.1.2. sample preparation, adding an internal standard: 475.1.2.1. To three decimal places of a glass tube, weigh 1 ± 0,1 g (a grams) of the sample. 475.1.2.2. Add 0.5 ml of phosphoric acid and 0.50 ml of the internal standard solution and 9 ml of ethanol. 475.1.2.3. Close the tube and shake vigorously. If you need to completely dissolve the lipid phase, place the tube for five minutes in a water bath, which is 60 ° c. Cool quickly under running water. 475.1.2.4. Filter part solution with membrane filter. 475.1.2.5. Filtrate chromatography performed on the same day. 475.2. gas chromatography, it is recommended that the following working conditions: 475.2.1.1.475.2.1. Column: stainless steel. 475.2.1.2. Length 2 m. 475.2.1.3.1/8 '' diameter. 475.2.1.4. Filling 10% sptm 1000 (or equivalent) + 1% H3PO4 on Chromosorb WAW 100 to 120 475.2.2. Temperature: 475.2.2.1. Injector: 200 ° C. 475.2.2.2. Column: 120 ° c. 475.2.2.3. Detector: 200 ° C. 475.2.2.4. Carrier gas: nitrogen. 475.2.2.5. Flow: 25 ml/min: 475.3.1. analytical 475.3. Calibration: 475.3.1.1. To calibrate the 20 ml flasks transfer by pipette 0.25, 0.50 respectively, 1.00, 2.00 and 4.00 ml propionic acid solution (473.5). 475.3.1.2. To each volumetric flask transfer by pipette 1.00 ml internal standard solution (473.6), make up to the mark with ethanol and mix. It prepared solutions are e mg/ml in 2-metilpropionskāb, which is an internal standard (i.e., 1 mg/ml if e = 1000) and p/4 p/2 p, 2 p, 4 p, mg/ml propionic acid (i.e., 0.25, 0.50, 1.00, 2.00, 4.00 mg/ml If p = 1000). 475.3.1.3. Enter 1 µ l of this solution each and, noting the propionic acid/2-metilpropionskāb-mass relation on x axis and the peak area ratio on the y axis, the calibration curve is obtained. 475.3.1.4. Every solution is administered three times and calculate the average peak area ratio. 475.3.2. Identification: 475.3.2.1. Enter 1 µ l sample of the filtrate (475.1.1). 475.3.2.2. Compare the chromatogram with one standard solution of chromium togramm (475.3.1). If a retention time of the peak is approximately equal to 2-metilpropionskāb corresponding to the retention time, the replacement of the internal standard. If no interference factor µ l sample 1 enter the filtrate (475.1.2) and the size of the propionic acid peak and the internal standard peak area. 475.3.2.3. Every solution is administered three times and calculate the average peak area ratio. 476. the calculation shall be effected in the following order: 476.1. From the calibration curve obtained in accordance with this subparagraph, annex 475.3.1. read weight (K) corresponding to the peak area ratio calculated in accordance with 475.3.2. of this annex. 476.2. mass derived from it for the calculation of the propionic acid content of the sample (X) as a percentage by mass using the formula: x% (m/m) = K ((0.5 × 100 × e)/(50 × a)) (e/a) = K, where K-ratio, calculated in accordance with this subparagraph annex 476.1.; (e) in accordance with this annex, point weighted 473.6. internal standard mass (in grams); (a) in accordance with 475.1.2. of this annex) (weighted sample mass (in grams). Rounds the result to one decimal place. 477. One sample with 2% (m/m) propionic acid content, the difference between the results of two determinations in parallel should not exceed 0.12% 4.37. Hydroquinone, hydroquinone monomethylether, hydroquinone monoethylether and hydroquinone monobenzylether qualitative and quantitative determination of Hydroquinone in cosmetic products, 37.1. hydroquinone monomethylether, hydroquinone monoethylether and hydroquinone monobenzylether in cosmetic products quality in 478. With hydroquinone, hydroquinone monomethylether, hydroquinone monoetil ether and hydroquinone monobenzylether qualitative method for detection of qualitatively and quantitatively hydroquinone , hydroquinone monomethylether, hydroquinone monoethylether and hydroquinone monobenzylether (monobenzone) in cosmetic products for lightening the skin. 479. hydroquinone and its ethers are determined by the thin-layer chromatography. 480. Hydroquinone and its ethers in quality detection method uses the following reaģentus1:480.1. Ethanol, 96% (v/v). 480.2. Chloroform. 480.3. diethyl ether. 480.4. Developing solvent: chloroform/diethyl ether: 66:33 (v/v). 480.5. Ammonia, 25% (m/m) (= 0.91 g/ml). 480.6. Ascorbic acid. 480.7. hydroquinone. 480.8. hydroquinone monomethylether 480.9. Hydroquinone monoethylether 480.10. Hydroquinone monobenzylether (monobenzone) Standard solution: solution of 480.11. should be prepared immediately before use, and they are stable in one day: Weigh 0.05 g hydroquinone 480.11.1.10 ml test tube with a section. Add 0.250 g of Ascorbic acid and 5 ml of ethanol. Add ammonia (480.5. bottom) until the pH is 10 and make up to a volume of 10 ml with ethanol. Weigh 0.05 g 480.11.2. hydroquinone monomethylether 10 ml test tube with a section. Add 0.250 g of Ascorbic acid and 5 ml of ethanol. Add ammonia (480.5) until the pH is 10 and make up to a volume of 10 ml with ethanol. Weigh 0.05 g 480.11.3. hydroquinone monoethylether 10 ml test tube with a section. Add 0.250 g of Ascorbic acid and 5 ml of ethanol. Add ammonia (480.5) until the pH is 10 and make up to a volume of 10 ml with ethanol. Weigh 0.05 g 480.11.4. hydroquinone monobenzylether 10 ml test tube with a section. Add 0.250 g of Ascorbic acid and 5 ml of ethanol. Add ammonia (480.5) until the pH is 10 and make up to a volume of 10 ml with ethanol. 480.12. Silver nitrate. 480.13.12-molybdophosphoric acid 480.14. Potassium ferricyanide hexahydrate 480.15. iron (iii) chloride hexahydrate. 480.16. Spray reagents: 480.16.1. Add 5% (m/v) aqueous solution of silver nitrate to ammonia (480.5) until the precipitate dissolves forming. The solution becomes explosively unstable on standing and should be discarded after use. 480.16.2.10% (m/v) solution of 12-molybdophosphoric acid in ethanol. 480.16.3. Prepare a 1% (m/v) aqueous solution of potassium ferricyanide and 2% (w/v) iron (iii) chloride aqueous solution. Immediately before use, mix the two solutions in equal shares. 481. Hydroquinone and its ethers in quality detection method uses the following equipment: 481.1. Normal laboratory equipment. 481.2. Usual TLC equipment. 481.3. ready to Use 20 × 20 cm of silica gel GHR/UV254 (Machery, Nagel or equivalent) thin-layer hromatogrāfijasplat. Layer thickness 0.25 mm. 481.4. ultrasonic bath. 481.5. Centrifuge. 481.6. Uv lamp, 254 nm. 482. Hydroquinone and its ethers quality test is performed in the following order: 482.1. sample preparation: Weigh 3.0 g of sample 482.1.1.10 ml test tube with a section. 482.1.2. Add 0.250 g of Ascorbic acid and 5 ml of ethanol. 482.1.3. Adjust the pH of the solution to 10 with ammonia (480.5). 482.1.4. Make up to a volume of 10 ml with ethanol. 482.1.5. Close the tube with the stopper and homogenize the ultrasonic bath for 10 minutes. 482.1.6. Filter through a filter paper or centrifuge with a speed of 3000 rpm. 482.2. Thin layer chromatography: 482.2.1. Saturate the chromatography tank with developing solvent (480.4.). 482.2.2. Precipitates on the plate 2 µ l of the standard solution (480.11) and 2 µ l of the sample solution (482.1). Develop in the dark ambient tempera tour until the solvent front moves 15 cm from the starting line. 482.2.3. Remove the plate from the tank and allow to dry at room temperature. 482.3. Detection: 482.3.1. view the plate under UV light at 254 nm, and mark the spots. 482.3.2. Spray the plate with silver nitrate reagent (480.16.1 below) or with a 12-molybdophosphoric acid reagent (482.16.2) (heat to approximately 120 ° C), or with potassium ferricyanide solution and ferric chloride solution (482.16.3). 483. Qualitative determination calculations shall be carried out in the following order: 483.1. Calculate the Rf value of each spot. 483.2. Sample solution with the standard solution spots plank ating in the light of their Rf values, spots of colour under the influence of ultra-violet light and the colours of the spots after visualization with the spray reagent. 483.3. Take high resolution HPLC under this subsection and 37.2 of annex sample peak (s) with the retention time of the peak of the standard retention times. 483.4. by thin-layer hromatogrāfijasun high performance thin layer hromatogrāfijasrezultāt to determine the quality of hydroquinone and its ethers (or). 484. The conditions described are observed, the following Rf values: 484.1. hydroquinone: hydroquinone monomethylether 0.32.484.2.: 0.53.484.3. Hydroquinone monoethylether: 0.55. Hydroquinone monobenziletilēter 484.4.: 0.58.37.2. Hydroquinone, hydroquinone monomethylether, hydroquinone monoethylether and hydroquinone monobenzylether in cosmetic products quantitative * 485. With hydroquinone, hydroquinone monomethylether, hydroquinone monoetil ether and hydroquinone monobenzylether quantitative detection method of the light determines the kvantit of HYDROQUINONE, hydroquinone monomethylether, hydroquinone monoethylether and hydroquinone monobenzylether in cosmetic products for lightening the skin. 486. The sample is extracted with a water/methanol mixture, gently heating to melt any lipid substances. The resulting solution of the analyte in the determination of reverse phase liquid chromatography with UV detection. 487. Hydroquinone and its ethers quantitative detection method uses the following reaģentus3:487.1. Methanol. 487.2. hydroquinone. 487.3. hydroquinone monomethylether 487.4. Hydroquinone monoethylether 487.5. Hydroquinone monobenzylether (monobenzone) 487.6. Tetrahydrofuran, HPLC grade thin layer chromatography. 487.7. Water/methanol mixture 1:1 (v/v): Mix one volume of water and one volume of methanol. 487.8. Mobile phase: tetrahydrofuran/water mixture 45:55 (v/v). Mix 45 volumes of tetrahydrofuran and 55 volumes of water. 487.9. Solution: weigh 0.06 g 0.08 g hydroquinone, hydroquinone monomethylether, hydroquinone monoethylether and 0.10 g 0.12 g hydroquinone Mono benzilēter 50 ml volumetric flask. Dissolve and make up to the mark with methanol. Prepare the standard solutions by diluting 10.00 ml of this solution to 50.00 ml with water/methanol mixture (487.7.). These solutions must be freshly prepared before use. 488. Hydroquinone and its ethers in quality detection method uses the following equipment: 488.1. Normal laboratory equipment. 488.2. Water bath, capable of maintaining a temperature of 60 ° C. 488.3. High-performance liquid chromatograph with variable-wavelength UV detector and 10 µ l injection loop. 488.4. Analytical column: stainless steel chromatographic column, length is 250 mm, internal diameter 4.6 mm, packed with Zorbax phenyl (chemically related phenethylsilane on Zorbax SIL, who left with the end of the inactivated trimethylchlorosilane), particle size 6 µm or equivalent. Not used, except phenyl guard column or equivalent. 488.5. Filter paper, diameter 90 mm, Schleicher and Schull, Weissband & Of 5892, or equivalent 489. Hydroquinone and its ethers quality test is performed in the following order: 489.1. sample preparation: 489.1.1. To three decimal places of a 50-ml volumetric flask weigh 1 ± 0,1 g (a grams) of the sample. 489.1.2. Disperse the sample 25 ml water/methanol mixture (487.7.). 489.1.3. Close the flask and shake vigorously until a homogeneous suspension is obtained. Shake for at least one minute. 489.1.4. Place the flask in a water bath kept at 60 ° C to facilitate the extraction. 489.1.5. Cool the flask and make up to the mark with the water/methanol (487.7.). 489.1.6. Filter the extract using a filter paper. 489.1.7. preparation of extract After 24 hours set the equestrian high-performance thin-layer chromatography. 489.2. High-performance liquid chromatography: 489.2.1. Mobile phase (487.8.) to adjust the flow rate of 1.0 ml/min and set the detector wavelength to 295 nm. 489.2.2. Enter 10 µ l of the sample solution obtained in accordance with section 489.1. of this annex, and record the chromatogram. Measure the peak areas. Calibrated in accordance with 489.2.3. of this annex. Sample and standard solution chromatograms. After the peak area and the relative response factor (Rf), calculated in accordance with paragraph 489.2.3. of this annex at the bottom, calculate the analyte concentration in the sample solution. 489.2.3. Calibration: 489.2.3.1.10 µ l Type solution (487.9) and host hromatogram. Enter several times to obtain a constant peak area. 489.2.3.2. determine the relative response factor RFI: RFI = pi/pi-ci that hydroquinone, hydroquinone monomethylether, hydroquinone monoethylether or hydroquinone monobenzylether peak area; CI-hydroquinone, hydroquinone monomethylether, hydroquinone monoethylether or hydroquinone monobenzylether concentration (g/50 ml) solution (487.9.). 489.2.3.3. Determine whether the resulting solution and chromatogram of the sample solution meet the following requirements: minimum of two 489.2.3.3.1 peak separation is at least 0.90 (peak separation defined in this annex, Figure 10).
Figure 10 peak separation if the required separation is not achieved, either a more efficient column should be used, or the mobile phase composition, regulation, to achieve compliance with the requirements. 489.2.3.3.2. All the resulting peak asymmetry factor AS is 0.9-1.5 (peak asymmetry factor defined in this annex, Figure 11). To record the chromatogram for the determination of the asymmetry factor a chart speed recommended is at least 2 cm per minute.
Figure 11 peak asymmetry factor 489.2.3.3.3. Obtain a stable baseline. 490. at the analyte peak area calculation of the test substance (s) concentration in the sample. Calculate the concentration of the analyte in the sample, in percentage by mass (xi), using the formula: xi% (m/m) = (bi × 100)/(RF × a), where the a-sample mass (in grams); BI-sample analyte peak area i. 491. Repeatability assessed šādi4:491.1. From the same sample for a hydroquinone content of 2.0% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.13%. 491.2. Out on the same sample hydroquinone monomethylether content 1.0% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.1%. 491.3. Out on the same sample hydroquinone monoethylether content 1.0% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.11%. 491.4. From the same sample hydroquinone monobenzylether content 1.0% the difference between the results of two determinations in parallel should not exceed an absolute value of 0.11%. 492. The reproducibility shall šādi4:492.1. From one sample with hydroquinone content of 2.0% the two determinations carried different conditions (different laboratories, different operators, different apparatus and/or different time), the difference between the results obtained should not exceed an absolute value of 0.37%. 492.2. From one sample with 1.0% hydroquinone monomethylether content of two determinations carried different conditions (different laboratories, different operators, different apparatus and/or different time), the difference between the results obtained should not exceed an absolute value of 0.21%. 492.3. From one sample with 1.0% hydroquinone monoethylether content of two determinations carried different conditions (different laboratories, different operators, different apparatus and/or different time), the difference between the results obtained should not exceed an absolute value of 0.19%. 492.4. From one sample with 1.0% hydroquinone monobenzylether content of two determinations carried different conditions (different laboratories, different operators, different apparatus and/or different time), the difference between the results obtained should not exceed an absolute value of 0.11%. * Notes. 1. when a hydroquinone content turns out to be considerably higher than 2%, and its content must be accurately predicts, the sample extract (489.1) should be diluted to a concentration that is similar to the concentration, which is derived from a sample containing 2% hydroquinone, and the determination should be repeated (some plants absorption can be outside the linear range of the detector if the concentration of hydroquinone is high). 2. With the above method can quantify hydroquinone and its ethers in one izokrātisk in the analysis. Phenyl column assures sufficient retention for HYDROQUINONE, which can not be guaranteed using C18 column with the mobile phase. However, this method does not eliminate the interference caused by multiple parabens. In such a case the determination repeated with other mobile phase/stationary phase system. Appropriate methods are indicated in the following sources: 2.1 m. Herpol-Borreman et m.-o. Masse, Identification et de l ' "hydroquinon et de ses in the méthyliqu of the benzyliqu éther et dans les produits cosmétiqu pour blanchir la of the pea. Int. j. Cosme. Sci. 8-203-214 (1986): 2.1.1. column: Zorbax ODS, 4.6 mm × 25 or equivalent; 2.1.2. temperature 36 ° C; 2.1.3. flow 1.5 ml/min; 2.1.4. mobile phase: hydroquinone: methanol/water 5:95 (v/v) for HYDROQUINONE, Mono-allylanisole – methanol/water 30:70 (v/v), hydroquinone monobenzylether – methanol/water 80:20 (v/v); 2.2. Conditions, suitable for HYDROQUINONE: j. Firth and i. Rix, Determination of skin toning cream in hydroquinon, analyst (1986), 111, p. 129: column: Spherisorb S5 2.2.1-ODS, or equivalent; 2.2.2. mobile phase: water/methanol 90:10 (v/v); 2.2.3. flow 1.5 ml/min 38.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate demonstration and in cosmetic products 38.1.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate demonstration 493. With the method set out in this chapter demonstrate the 2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, propyl 4-hydroxybenzoate, butyl 4-hydroxybenzoate and benzyl 4-hydroxybenzoate in cosmetic products. 494. Preservatives from the acidified cosmetic sample is extracted with acetone. After filtering the acetone solution is mixed with water and alkaline environment precipitated the calcium salts of fatty acids. Alkaline acetone/water mixture is extracted with diethylether to remove lipofil. After acidification konser Vantaa are extracted with diethyl ether. Diethyl ether an aliquot part of the extract spotted on the gel thin-layer plate silik. After developing the plates for the chromatogram under UV light and is made visible with Millon's reagent. 495.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate probative method uses the following reaģentus1, 3:495.1. Acetone. 495.2. diethyl ether. 495.3. n-pentane. 495.4. Methanol. 495.5. Glacial acetic acid. 495.6. Hydrochloric acid solution, c (HCl) = 4 mol/l 495.7. Potassium hydroxide solution, c (KOH) = 4 mol/l 495.8. Calcium chloride dihydrate (CaCl2 72h2o). 495.9. Discovery reagent: Millon's reagent (Millon's reagent (dzīvsud rab (II) nitrate) is sold ready-to-use solution (Fluka 69820)). 495.10.2-phenoxyethanol. 495.11.1-phenoxypropan-2-ol. 495.12. Methyl 4-hydroxybenzoate (methylparaben). 495.13. Ethyl 4-hydroxybenzoate (ethylparaben). 495.14. n-propyl 4-hydroxybenzoate (propylparaben). 495.15. n-butyl 4-hydroxybenzoate (butylparaben). 495.16. Benzyl 4-hydroxybenzoate (benzylparaben). 495.17. Standard solution: from each of the reference substances (495.11.,.,., 495.12 495.13 495.14.,., 495.16. and 495.15 495.17.) prepare 0.1% (m/v) solution in methanol. 495.18. Development solvent: mix 88 volumes of n-pentane with 12 volume units of glacial acetic acid. 496.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate method of proof, used laboratory equipment and such equipment: 496.1. Water bath, capable of maintaining 60 ° C. 496.2. Developing tank (not lined with filter paper). 496.3. light source, UV 254 nm. Thin-Layer plates, 496.4.20 × 20 cm, precoated with 0.25 mm silica gel 60F254, with concentrating zone (Merck No 11798, Darmstadt, or equivalent). 496.5. Oven, at 105 ° C can be maintained. 496.6. Hot air dryer. 496.7. Wool color wheel button, about 10 cm long, with an external diameter of about 3.5 cm. Fleece layer thickness is 2-3 mm. If necessary, the fur clipped. 496.8. glass tube, 50 ml, with screw cap. 496.9. Hotplate with thermostat for temperature control. Temperature setting: about 80 ° c. Electric stove cover with about 6 mm thick aluminum 20 × 20 cm wide, in order to ensure a smooth warming. 497.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate demonstration is carried out in the following order: 497.1. sample preparation: 497.1.1. Weigh approximately 1 g of sample in a 50-ml glass tube with screw cap. Add four drops of hydrochloric acid solution (495.7) and 40 ml of acetone. 497.1.2. Highly basic cosmetic products (such as toilet SOAP) add 20 drops of hydrochloric acid. 497.1.3. Into the tube, gently heat the mixture to approximately 60 ° C to facilitate the extraction of the preservatives into the acetone phase and shake vigorously for one minute. 497.1.4. The solution pH with indicator strips by hydrochloric acid solution and adjust the pH of the solution to 3.497.1.5. Again shake vigorously for one minute. 497.1.6. Cool the solution to room temperature and filter through a filter paper into a conical flask. 497.1.7. Transfer 20 ml of the filtrate into a 200-ml conical flask, add 60 ml of water and mix. 497.1.8. With potassium hydroxide (495.7.), using pH indicator paper, adjust the pH of the mixture to approximately 10.497 1.9. Add 1 g calcium chloride dihydrate and shake. 497.1.10. Filter the solution through a filter paper into a 250-ml separating funnel containing 75 ml diethylether and shake vigorously for one minute. 497.1.11. Allow the phases to separate and collect the aqueous layer in a 200 ml flask with a conical shape. 497.1.12. hydrochloric acid solution, using pH indicator paper, adjust the pH of the solution around to 2.497.1.13. Then add 10 ml diethylether and shake vigorously for one minute. 497.1.14. Allow the phases to separate and transfer approximately 2 ml of the diethylether layer into a 5-ml sample vial. 497.2. Thin layer chromatography (TLC): TLC plate to replace the 497.2.1. heated aluminium plate. 497.2.2. Spotted 10 µl of each standard solution (495.17.) and 100 µ l of the sample solution (s) (497.1) on the starting line of the TLC plate focus area. After the elections the solvent evaporation can accelerate with the air flow. remove the TLC plate 497.2.3. from the stove and allow to cool to room temperature. Transfer 100 ml of the developing solvent (495.18.) on the developing tank. 497.2.4. Now TLC plate in the unsaturated Chamber and develop at room temperature until the solvent front has moved about 15 cm from the starting line. 497.2.5. Remove the plate from the developing tank and dried in hot air dryer. 497.2.6. view the plate under UV light and spots placed in you. 497.2.7. Heat plate 30 minutes oven 100 ° C to remove excess acetic acid. Preservatives in the chromatogram with Millon visualize reagent (495.9), dipping the paint roller (496.7) and drove it to the reagent on the TLC plate to plate is evenly moistened. Alternatively, the spots may be visualized, carefully a few drops each of Millon's reagent on ultraviolet light marked spots. 4-Hydroxybenzoic acid esters appears red spots, 2-phenoxyethanol and 1-phenoxypropan-2-ol-yellow spots. However, the same 4-Hydroxybenzoic acid, which can be as a preservative or decomposition product samples, also appears in the red spot. 497.3. Demonstration: 497.3.1. Calculates the value of each spot of the Rf. 497.3.2. Compare the results obtained from the sample solution spots with those obtained from the reference solutions by comparing their Rf values, their character and the influence of ultra-violet light color once they are made visible. 497.3.3. make preliminary conclusions about the identity of the preservatives. In the case of the presence of paraben should be made to this annex referred to in sub-section 38.2. HPLC procedure. Combining TLC and high-performance liquid chromatography (HPLC) to confirm the results of 2-phenoxyethanol, 1-fenoksipr-2-ol of pan and parabens. * Notes. 1. Whereas the Millon's reagent is toxic, it is better to use it in accordance with one of these procedures. Sprinkle is not recommended. 2. Other compounds containing hydroxyl groups may be painted to contact with Millon's reagent. Their color and Rf value obtained from the table a number of preservatives using this TLC procedure is found in the N. deKruijf, M.A.H. Rijk, L.A. pranato-soetardhi and a. Schouten (1987): Determination of cosmetic products in preservativ I: Thin-layer chromatographic procedure for the identification of preservativ in cosmetic products (j. Chomatography 410, 395-411). 3. the following table indicates the values of that Rf values can be obtained: compound hRf color 4-Hydroxybenzoic acid 11 Red, methylparaben, ethylparaben, 12 red 17 red propylparaben 21 red butylparaben 26 red benzylparaben 16 29 2-phenoxyethanol red yellow 1-phenoxypropan-2-ol 50 yellow 4. There is no difference between a 4-Hydroxybenzoic acid and methylparaben and ethylparaben benzylparaben or. Proof of this connection by this annex referred to in sub-section 38.2. HPLC method and comparison of the sample and of the standard retention time. 38.2. the 2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate * 498. With 2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate in cosmetic products detection method determines the 2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl 4-hydroxybenzoate, ethyl 4-hydroxybenzoate, propyl 4-hydroxybenzoate, butyl 4-hydroxybenzoate and benzyl 4-hydroxybenzoate. 499.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate (preservative) the quantity shall be expressed as a percentage by mass. 500. the sample is acidified by adding sulphuric acid, and then suspended in a mixture of ethanol and water. The mixture is gently heated to melt the lipid phase to promote quantitative extraction and, then the mixture is filtered. Preservatives the filtrate is determined by reverse phase HPLC, using the internal standard isopropyl-4-hydroxy benzoates. 501.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate method uses the following reaģentus1, 2, 3:501.1. Absolute ethanol. 501.2.2-phenoxyethanol. 501.3.1-phenoxypropan-2-ol. 501.4. Methyl 4-hydroxybenzoate (methylparaben). 501.5. Ethyl 4-hydroxybenzoate (ethylparaben). 501.6. n-propyl 4-hydroxybenzoate (propylparaben). 501.7. Isopropyl 4-hydroxybenzoate (isopropylparaben). 501.8. n-butyl 4-hydroxybenzoate (butylparaben). 501.9. Benzyl 4-hydroxybenzoate (benzylparaben). 501.10. Tetrahydrofuran. 501.11. Methanol. 501.12. Acetonitrile. 501.13. sulphuric acid solution, c (H2SO4) = 2 mol/l. 501.14. Ethanol/water mixture: mix nine volumes of ethanol and one volume of water. 501.15. Internal standard solution: weigh accurately approximately 0.25 g of pilparaben izopr, transfer to a 500 ml graduated flask, dissolve and make up to volume with ethanol/water mixture (501.14). 501.16. Mobile phase: tetrahydrofuran/water/methanol/acetonitrile mixture. Mix 5 volumes of tetrahydrofuran, 60 volumes of water, 10 volumes of methanol and 25 volumes of Acetonitrile. 501.17. Preservative stock solution: weigh accurately approximately 0.2 g 2-phenoxyethanol, 0.2 g 1-phenoxypropan-2-ol, 0.05 g methylparaben, 0.05 g ethylparaben, 0.05 g propylparaben, 0.05 g butylparaben and 0.025, g benzilpar ben 100 ml volumetric flask, dissolve and make up to volume with ethanol/water mixture. Stored in the refrigerator, the solution remains stable for one week. 501.18. Standard preservative solutions: transfer respectively 20.00 5.00, 10.00, 2.00, 1.00 ml of the standard solution and (501.17) to a 50 ml volumetric flask. Each flask, add 10.00 ml internal standard solution (501.15.) and 1.0 ml sulfuric acid solution (501.13.) and make up to volume with ethanol/water mixture. These solutions should be freshly prepared before use. 502.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate method used in laboratory equipment and such equipment: 502.1. Water bath, capable of maintaining 60 ± 1 ° c. 502.2. High-performance liquid chromatograph with 280 nm ultraīsviļņ detector. 502.3. Chromatography column with the following conditions: 502.3.1. Stainless steel. 502.3.2. column length 25 cm, internal diameter 4.6 mm (or 12.5 cm and 4.6 mm). 502.3.3.5C18 or equivalent Nucleosil filling. 502.4. glass vials 100 ml, with screw cap. 502.5. Boiling chips, carborundum 2-4 mm, or equivalent. 503.2-phenoxyethanol, 1-phenoxypropan-2-ol, methyl, ethyl, propyl, butyl and benzyl 4-hydroxybenzoate shall be carried out in the following order: 503.1. sample preparation: 503.1.1. Sample preparation without addition of internal standard: 503.1.1.1. Weigh approximately 1.0 g of sample in a 100-ml glass tube with screw cap of the jam. 503.1.1.2. With the pipette tube pipette 1.0 ml sulfuric acid solution (501.13. below) and 50.0 ml ethanol/water mixture (501.14). 503.1.1.3. Add approximately 1 g of boiling chips, close the tube and shake vigorously until a homogeneous suspension is obtained. Shake for at least one minute. 503.1.1.4. Place the tube for five minutes in a water bath kept at 60 ± 1 ° C, in order to speed up the extraction of the preservatives into the ethanol phase. 503.1.1.5. immediately cool the tube in a stream of cold water and store the extract in the refrigerator for one hour. 503.1.1.6. Filter the extract using a filter paper. 503.1.1.7. Transfer approximately 2 ml of the filtrate into a 5-ml sample vial. 503.1.1.8. The extract in the refrigerator and perform the HPLC determination within 24 hours. 503.1.2. sample preparation, adding an internal standard: 503.1.2.1. Weigh to three decimal places 1,0 ± 0,1 g of the sample into a 100-ml glass tube with screw cap. 503.1.2.2. With the pipette tube pipette 1.0 ml sulfuric acid solution and 40.0 ml ethanol/water mixture. 503.1.2.3. Add approximately 1 g of boiling chips and exactly 10.00 ml internal standard solution. 503.1.2.4. Close the tube and shake vigorously until obtaining smooth suspension. Shake for at least one minute. 503.1.2.5. Place the tube for five minutes in a water bath kept at 60 ± 1 ° C, in order to speed up the extraction of the preservatives into the ethanol phase. 503.1.2.6. immediately cool the tube in a stream of cold water and store the extract in the refrigerator for one hour. 503.1.2.7. Filter the extract using a filter paper. 503.1.2.8. Transfer approximately 2 ml of the filtrate into a 5-ml sample vial (sample) 503.1.2.9. The extract in the refrigerator and perform the HPLC determination within 24 hours. 503.2. High performance liquid chromatography (HPLC): 503.2.1. Chromatographic conditions: 503.2.1.1. Mobile phase: tetrahydrofuran/water/methanol/acetonitrile mixture (501.16). 503.2.1.2. Flow rate: 1.5 ml/minute. 503.2.1.3. Detection wavelength: 280 nm. 503.2.2.503.2.2.1. Enter the Calibration: 10 µ l of the standard solution for each preservative (501.18. below). 503.2.2.2. After acquired the chromatogram of preservative solution peak Standart height relationship to the internal standard. 503.2.2.3. Designed curve of each of the preservative to extend that relationship to concentrations of the standard solution. 503.2.3.: 503.2.3.1. Enter 10 µ l of the sample solution without internal standard (503.1.1.) into the chromatograph and record the chromatogram. 503.2.3.2. Inject 10 µl of the standard solution of one preservative (501.18. bottom) and record the chromatogram. 503.2.3.3. Compare the resulting chromatogram is: If the sample extract (503.1.1.4) there are no peaks in the chromatogram, the retention time which is approximately equal to isopropylparaben (recommended internal standard) peak retention time, enter 10 µ l sample solution with internal standard (503.1.2). Record the chromatogram and measure the peak heights. If in the chromatogram of the sample solution is a troublesome peak retention time which is approximately equal to the retention time of the peak isopropylparaben, choose another internal standard. If a test does not show the preservative the sample hromat, the gramm these preservatives can be used as an alternative to the internal standard. 503.2.3.4. Calculation of the investigated preservatives to the peak height of the internal standard peak against height. 503.2.3.5. Make sure that the calibration standard solution used to form a straight line. 503.2.3.6. Make sure that the resulting solution and chromatogram of the sample solution meet the following conditions: 503.2.3.6.1. The worst separated pair separation of peaks is at least 0.90 (peak separation defined in this annex 12. the picture).
Peak separation (p) p = f/g figure 12 peak separation if the required separation is not achieved, should be used for more effective regulation of the column, or the mobile phase composition, to achieve the desired separation 503.2.3.6.2.: the asymmetry factor for all peaks is 0.9-1.5 (peak factor defined the asime threshing this annex 13 figure). To record the chromatogram for sharp metrij factor, we recommend a chart speed of at least 2 cm per minute.
Asymmetry factor (As) As = b/a figure 13 peak asymmetry factor 503.2.3.6.3. Obtained a steady base line. 504. the concentration of the preservatives in the sample solution calculated by calibrated horse curve (503.2.2) and peak heights of the investigated preservatives to the relationship to the internal standard. Calculate the 2-phenoxy-ethanol, 1-phenoxypropan-2-ol, methyl 4-hydroxybenzoate, ethyl 4-hidroksiben zoāt, propyl 4-hydroxybenzoate, butyl 4-hydroxybenzoate and benzyl 4-hydroxy benzoate content wi as a percentage by mass (% m/m), using the formula:% wi (m/m) = ((bi)/(200 × a)) where (i) the concentration of the preservatives, bi-(µ g/ml) sample solution, read from the calibration curve; a – the quantity test mass (in grams). 505. reproducējamības4 evaluation method and Atkārtojamības4 set out in paragraph 5 of the notes. * Notes. 1. Stationary phase. Withdrawal, setting the HPLC, largely depends on the nature of the stationary phase, the brand and origin. Whether the column can be used for the separation of the preservatives can be gleaned from the results obtained under the standard solutions (503.2.3. below). In addition to the ODS Hypersil column stuffing is also recognized as a suitable Zorbax ODS. Alternatively, you can optimize the recommended composition of the mobile phase in order to achieve the required separation. 2. Detection wavelength. This analysis during the pointer controlled carefully because about checking that the method has shown that small detection wavelength changes can significantly affect the detection results. 3. Interference. Under the conditions described in this method, elute also many others linking to you, such as preservatives and cosmetic additives. The retention time of the preservatives are included in n. deKruijf, M.A.H. Rijk, L.A. pranato-soetardhi and a. Schouten, (1989). Determination of cosmetic products in preservativ II. High-performance liquid chromatographic identification (j. chroma tography 469, 317-398). 4. analytical column an appropriate guard column can be fitted with. 5. the method is tested comparable tests with the participation of nine laboratories. Three samples were analysed. This table is included in the determination of the components in each sample average% m/m (m), the repeatability (r) and reproducibility (R): model 2-phenoxy-propan-2-ol 1-phenoxy-propan-2-ol Methyl paraben parabens propyl paraben in the Ethyl Butyl paraben is Benzyl as ben Vitaminizēt cream m 1.124 0.250 0.0628 0.031 0.0906 r R 0.176 0.030 0.0068 0.0111 0.0034 0.016 0.018 0.0035 0.0028 0.0044 cream that quickly absorbed into m r R 0.147 0.022 0.004 1.196 0.266 0.076 0.040 0.003 0.002 massage cream 0.806 0.180 0.148 0.152 m r R 0.112 0.078 0.012 0.016 0.067 0.034 0.013 0.015

The notes. 1 all reagents must be of analytical quality. 2 all reagents must be suitable for HPLC where appropriate. 3 the water used must be distilled water or water of at least equivalent quality. 4 the accuracy of methods is assessed according to the following standards: 1) EN ISO 5725-1:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 1: General principles and definitions. Registered 2003.07.29.; valid from 2003.07.29.; 2) EN ISO 5725-2:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 2: Vienmetod standartmērījum of the repeatability and reproducibility of the determination of the basic method. Registered 2003.07.29.; valid from 2003.07.29.; 3) EN ISO 5725-3:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 3: the standartmērījum of konverģentum of Vienmetod suffer. Registered 2003.07.29.; valid from 2003.07.29.; 4) EN ISO 5725-4:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 4: determination of the accuracy of standartmērījum of Vienmetod of basic methods. Registered 2003.07.29.; valid from 2003.07.29.; 5) EN ISO 5725-1:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 5: alternative methods of standard methods of measurement accuracy. Registered 2000.10.26.; valid from 2000.10.26. (2003.07.29. name change); 6) EN ISO 5725-1:2003 measurement precision of the methods (even the sum of results and konverģentum) – part 6: accuracy use values in practice. Registered 2003.07.29.; valid from 2003.07.29. "
Health Minister g. Smith