KS M ISO 10638-2012 Rubber－Identification of antidegradants by gas chromatography mass spectrometry《橡胶 气相色谱法 根据质谱法确认抗氧化剂》.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M ISO 10638 / KS M ISO 10638:2012 2012 12 10 http:/www.kats.go.krKS M ISO 10638:2012 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) ： ：2012 12 10 2012-0684 ： ： ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS M ISO 10638:2012 i ii 1 1 2 1 3 1 4 .2 4.1

2、 2 4.2 .2 4.3 2 4.4 .3 5 - .3 5.1 3 5.2 .3 5.3 3 5.4 .3 6 .4 7 4 8 .4 A( ) .5 B( ) 8 C( ) 40 43 KS M ISO 10638:2012 ii 2010 1 ISO 10638, Rubber Identification of antidegradants by gas chromatography/mass spectrometry . KS M ISO 10638:2012 / Rubber Identification of antidegradants by gas chromatograp

3、hy/mass spectrometry . . . . ( ) . 1 , , , / . A 31 . . / . , / , . . 2 . . ( ) . KS M ISO 123, KS M ISO 124, , KS M ISO 1407, KS M ISO 1795, KS M ISO 4661 2, 2： 3 KS M ISO 10638:2012 2 (desorption) . , . (retention index) . 4 4.1 4.1.1 (Trap coolant), , , . 4.1.2 (Gas chromatograph carrier gas)： 4.

4、2 4.2.1 , , 340 . (pyrolyser) . 4.2.2 (Trap apparatus), . 4.2.3 / ： ： (25 60) m ： (0.25 0.35) mm ： 5 % -, 95 % ： (0.20 0.35) m A C , (： 100 % ) . ： (1.0 2.0) mL/min ： (300 350) ： 40 , 20 /min 320 , 320 10 (quadrupole) , - (magnetic-sector-type) . ： 300 ： (electron ionization) (ion source) ： (230 300

5、) ： 70 eV (scan range)： / (charge) (m/z)： 50 600 4.3 KS M ISO 10638:2012 3 4.3.1 , KS M ISO 123 KS M ISO 124 . 4.3.2 , KS M ISO 1795 KS M ISO 4661 2 . 4.4 4.4.1 (1 2) mg ( ) . 4.4.2 340 , / . , 340 1 . , , / . 5 - 5.1 5.1.1 , 5.1.2 ： 5.2 5.2.1 , KS M ISO 1407 . 5.2.2 / , 4.2.3 . 5.3 4.3 5.4 5.4.1 2

6、mm 2 g , 8 . 2 g , . 5.4.2 (10 20) mL , / 1 L . . , . KS M ISO 10638:2012 4 6 C 7 B.1 B.31 , . , / (m/z) , A.1 . , , B . . , . . , 1 . (peak ratio) . (decomposition product) . , . . 8 . a) (origin) b) ： 1) , 2) ( ) c) ： 1) 2) d) , (identity) e) KS M ISO 10638:2012 5 A ( ) , , , CAS , , / A.1 . A.1 a

7、 (ISO 6472 ) CAS a / m/z B1-12,2,4-trimethyl-1,2-dihydroquinoline 158 173 1 466B1-2 158 331 2 725B1 polymerized 2,2,4- trimethyl-1,2-dihydroquinoline TMQ 26780-96-1 B1-3 174 519 3 823B2 6-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline ETMQ 91-53-2 B2-16-ethoxy-1,2-dihydro-2,2,4-trimethylquinoline 202 2

8、17 1 762B3-1 diphenylamine 169 1 645B3-2 isopropyl diphenylamine 196 211 1 911B3-3 9,9-dimethylacridane 194 209 1 963B3 acetone-diphenylamine ADPA 68412-48-6 B3-4 236 251 2 175B4-1 diphenylamine 169 1 644B4-2 9,9-dimethylacridane 194 209 1 963B4-3 331 348 2 722B4 diphenylamine, aniline, acetone B4-4

9、 363 378 3 738B5 N-phenyl-naphthylamine PAN 90-30-2 B5-1 phenyl-1-naphthylamine 219 2 205B6-1 diphenylamine 169 1 645B6-2 4,4-dibutyl-diphenylamine 210 281 2 326B6 alkylated diphenylamine 68921-45-9 B6-3 4,4-dioctyl-diphenylamine 322 393 3 004B7 octylated diphenylamine ODPA 106-67-7 B7-1 4,4-dioctyl

10、-diphenylamine 322 393 3 009B8 4,4-bis(,-dimethylbenzyl)-diphenylamine 10081-67-1 B8-14,4-bis(,-dimethylbenzyl)-diphenylamine 390 405 3 655B9-1N-phenyl-p-phenylenediamine 184 1 986B9 p-(p-toluenesulfonylamido)-diphenylamine 100-93-6 B9-2p-(p-toluenesulfonylamido)-diphenylamine 183 338 3 337KS M ISO

11、10638:2012 6 A.1 ( ) a (ISO 6472 ) CAS a / m/z B10 N,N-di-2-naphthyl-p-phenylenediamine DNPD 93-46-9 B10-1N,N-di-2-naphthyl-p-phenylenediamine 360 4 124B11 N,N-diphenyl-p-phenylenediamine DPPD 74-31-7 B11-1N,N-diphenyl-p-phenylenediamine 260 2 736B12 N-isopropyl-N-phenyl-p-phenylenediamine IPPD 101-

12、72-4 B12-1N-phenyl-N-isopropyl-p-phenylenediamine 211 226 2 153B13 N-1,3-dimethylbutyl-N-phenyl-p-phenylenediamine 6PPD 793-24-8 B13-1N-phenyl-N-(1,3-dimethylbutyl)-p-phenylenediamine 211 268 2 391B14 N-(1-methylheptyl)-N-phenyl-p-phenylenediamine 15233-47-3 B14-1N-(1-methylheptyl)-N-phenyl-p-phenyl

13、enediamine 211 296 2 657B15-1N,N-diphenyl-p-phenylenediamine 260 2 728B15-2N,N-dimethylphenyl-p-phenylenediamine 288 2 810B15 diaryl-p-phenylenediamine 68953-84-4 B15-3N,N-dimethylphenyl-p-phenylenediamine( ) 288 2 880B16 2,6-di-tert-butyl-4-methylphenol BHT 128-37-0 B16-12,6-di-tert-butyl-4-methylp

14、henol 205 220 1 528B17 2,6-di-tert-butyl-4-ethylphenol 4130-42-1 B17-12,6-di-tert-butyl-4-ethylphenol 219 234 1 577B18-1 -methylbenzylphenol 183 198 1 744B18-2 di-methylbenzylphenol 287 302 2 530B18 styrenated phenol SPH 61788-44-1 B18-3 tri-methylbenzylphenol 391 406 3 082B19 n-octadecyl-3-(4-hydro

15、xy-3,5-di-tert-butylphenyl)propionate 2082-79-3 B19-1n-octadecyl-3-(4-hydroxy-3,5-di-t-butylphenyl)propionate 515 530 3 628B20 2-t-butyl-6-(3-t-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenyl acrylate 61167-58-6 B20-12-t-butyl-6-(3-t-butyl-2-hydroxy-5-methylbenzyl)-4-methylphenyl acrylate 361 394 2 6

16、08B21 2,2-methylene-bis(4-ethyl-6-tert-butylphenol) o-MBp24 88-24-4 B21-12,2-methylene-bis(4-ethyl-6-tert-butylphenol) 191 368 2 549B22 2,2-methylene-bis(4-methyl-6-tert-butylphenol) o-MBp14119-47-1 B22-12,2-methylene-bis(4-methyl-6-tert-butylphenol) 177 340 2 457B23 4,4-butylidene-bis(6-tert-butyl-

17、m-cresol) p-BBp14 85-60-9 B23-14,4-butylidene bis(3-methyl-6-tert-butylphenol) 339 382 2 736B24 4,4-thio-bis(2-tert-butyl-m-cresol) p-TBp14 96-69-5 B24-14,4-thio-bis(3-methyl-6-tert-butylphenol) 343 358 2 820KS M ISO 10638:2012 7 A.1 ( ) a (ISO 6472 ) CAS a / m/z B25 p-cresol dicydopentadiene 68610-

18、51-5 B25-12,2-cyclopentadiene-bis(4-methyl-6-tert-butyl-phenol) 445 460 3 746B26 2,2-methylene-bis6-(1-methylcyclohexyl)-p-cresol o-MBp1 (1C) 77-62-3 B26-12,2-methylene-bis6-(1-methylcyclohexyl-p-cresol) 217 420 3 327B27-1 205 220 1 483B27 2,5-di-tert-butyl-hydroquinone DBHQ 88-58-4B27-22,5-di-tert-

19、butyl-hydroquinone 207 222 1 814B28-12,5-di-pentyl-p-benzoquinone 177 248 1 680B28 2,5-di-tert-amyl-hydroquinone DAHQ 79-74-3B28-22,5-di-tert-amyl-hydroquinone 221 250 1 982B29-1 di-n-butylamine 86 129 960 B29 tributyl thiourea 2422-88-0 B29-2 butylisothiocyanate 72 115 1 003B30 dilauryl thiodipropi

20、onate DLTDP 123-28-4 B30-1 dilauryl thiodipropionate 329 514 3 629B31 butyl hydroxyanisole BHA 25013-16-5 B31-13-tert-butyl-4-hydroxyanisole 165 180 1 495a B KS M ISO 10638:2012 8 B ( ) B.1 B.31 . . a) ： Frontier-LAB PY-2020 iD ： 350 b) ： c) / ： Agilent 6890 Agilent 5973 ： 1.0 mL/min ： 300 mL/min (s

21、plit ratio) 1/300 ： 320 ： 40 , 20 /min 320 , 320 10 ： 300 ： ： 250 ： 70 eV ： / (m/z) 29600 d) ： Ultra ALLOY-5 (Frontier-LAB): ： 30 m ： 0.25 mm ： 5 % -, 95 % ： 0.25 m KS M ISO 10638:2012 9 t ( ) m/z / B.1 2,2,4-trimethyl-1,2-dihydroquinoline KS M ISO 10638:2012 10 t ( ) m/z / B.2 6-Ethoxy-1,2-dihydro-

22、2,2,4-trimethylquinoline KS M ISO 10638:2012 11 t ( ) m/z / B.3 Acetone-diphenylamine KS M ISO 10638:2012 12 t ( ) m/z / B.4 diphenylamine, aniline, acetone KS M ISO 10638:2012 13 t ( ) m/z / B.5 N-Phenyl-naphthylamine KS M ISO 10638:2012 14 t ( ) m/z / B.6 Alkylated diphenylamine KS M ISO 10638:201

23、2 15 t ( ) m/z / B.7 Octylated diphenylamine KS M ISO 10638:2012 16 t ( ) m/z / B.8 4,4-bis(,-Dimethylbenzyl)diphenylamine KS M ISO 10638:2012 17 t ( ) m/z / B.9 p-(p-Toluenesulfonylamido)diphenylamine KS M ISO 10638:2012 18 t ( ) m/z / B.10 N,N-Di-2-naphthyl-p-phenylenediamine KS M ISO 10638:2012 1

24、9 t ( ) m/z / B.11 N,N-Diphenyl-p-phenylenediamine KS M ISO 10638:2012 20 t ( ) m/z / B.12 N-Isopropyl-N-phenyl-p-phenylenediamine KS M ISO 10638:2012 21 t ( ) m/z / B.13 N-1,3-Dimethylbutyl-N-phenyl-p-phenylenediamine KS M ISO 10638:2012 22 t ( ) m/z / B.14 N-(1-Methylheptyl)-N-phenyl-p-phenylenediamine KS M ISO 10638:2012 23 t ( ) m/z / B.15 diaryl-p-phenylenediamine KS M ISO 10638:2012 24 t ( ) m/z / B.16 2,6-Di-tert-butyl-4-methylphenol KS M ISO 10638:2012 25 t ( ) m/z / B.17 2,6-Di-tert-butyl-4-ethylphenol KS M ISO 10638:2012 26 t ( ) m/z / B.18 Styrenated phenol