1、 KS I ISO 18287 KSKSKSKS SKSKSKS KSKSKS SKSKS KSKS SKS KS (PAH) (GCMS) KS I ISO 18287 : 2007 (2012 ) 2007 11 7 http:/www.kats.go.krKS I ISO 18287:2007 : ( ) ( ) ( ) () ( ) E&M / : (http:/www.standard.go.kr) : :2007 11 7 :2012 12 27 20120781 : : ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS I IS
2、O 18287:2007 .1 1 1 2 1 3 .2 4 .2 5 .5 6 , , 6 7 6 7.1 6 7.2 7 7.3 7 8 .9 9 (performance characteristics) .9 10 (quality assurance) .9 11 .10 A() GCMS .11 B() .14 18 i KS I ISO 18287 : 2007 (2012 ) (PAH) (GCMS) Soil quality Determination of polycyclic aromatic hydrocarbons(PAH) Gas chromatographic m
3、ethod with mass spectrometric detection(GC MS) 2006 1 ISO 18287, Soil qualityDetermination of polycyclic aromatic hydrocarbons(PAH)Gas chromatographic method with mass spectrometric detection(GCMS) . . , , . . 1 . 366 nm UV . . , (dust hazard) . ( , , ) . . . 1 (EPA, 1982) 16 (PAH) . ( ) . 0.01 mg/k
4、g( ) . 2 KS I ISO 18287:2007 . . ( ) . KS M ISO 103811, 1: KS M ISO 11465, () KS M ISO 14507, KS M ISO 16720, ISO 103818, Soil qualitySamplingPart 8:Guidance on sampling of stockpiles 3 (petroleum ether) . . , . 50 mL 50 mL ( ). 100 mL . . . A B, . A(2): 2 . 2 . . B(1): , , , . . (adsorption chromat
5、ography) . . . 4 . . 4.1 4.2 4.3 ( 4060 ) 4.4 (cyclohexane) 2 KS I ISO 18287:2007 4.5 (isooctane) 4.6 4.7 , 4.8 (magnesium perchlorate) 4.9 60 , 63200 m 4.10 60 :w(H 2 O)10 %() 450 3 (5.13) 60(4.9) . (5.14) 130 5 . 10 %() . 5 (5.3) 2 . . 4.11 (reference substance), . GCMS . . 1 (native) . 1) 1 CAS N
6、o. Naphthalene 91 20 3 Naphthalene-d 8Acenaphthene 83 32 9 Acenaphthene-d 10Acenaphthylene 208 96 8 Fluorene 86 73 7 Anthracene 120 12 7 Phenanthrene 85 01 8 Phenanthrene-d 81) , B 2440 Geel (Institute for Reference Materials and Managements, IRMM), D.C (National Science and Technology Office of Sta
7、ndard Ref. Data) . ISO . 3 KS I ISO 18287:2007 1 () CAS No. Fluoranthene 206 44 0 Pyrene 129 00 0 Benzaanthracene 56 55 3 Benzaanthracene-d 12Chrysene 218 01 9 Benzobfluoranthene 205 99 2 Benzoepyrene-d 12Benzokfluoranthene 207 08 9 Benzoapyrene 50 32 8 Indeno1,2,3-cdpyrene 193 39 5 Perylene-d 12Dib
8、enzahanthracene 53 70 3 Benzoghi perylene 191 24 2 4.12 GCMS (5.8) (4.4) (calibration solution) . 4.12.1 (single-substance stock solution) “ ” “ ”( 1 ) 10 mg( 0.1 mg ) 50 mL (4.4) (200 g/mL) . 1518 . 4.12.2 (4.12.1) 15 mL( .) 100 mL (210 g/mL). 4.12.3 (4.12.1) 5 mL 100 mL (10 g/mL). 4.12.2 4.12.3 4
9、. 1 . 4.12.4 (4.12.2) 1 5 mL (4.12.3) 1 mL 10 mL (0.205.0 g/mL) , . 4 KS I ISO 18287:2007 1.0 g/mL . 1 . 5 , . 5.1 1 L , PTFE ( ) 1 L . 5.2 5.3 ( 200300 ) 5.4 (kuderna Danish) (rotary evaporator) 5.5 100 . 5.6 5.7 (conical flask) PTFE ( ) 100 mL, 500 mL, 1 000 mL . 5.8 10 mL, 50 mL, 100 mL . 5.9 250
10、 mL, 500 mL, 1 000 mL . 5.10 1 mL, 2 mL, 5 mL, 10 mL , (Pasteur pipettes) 5.11 100 L L . 5.12 100 mL . 5.13 5.14 150 . 5 KS I ISO 18287:2007 5.15 (glass wool) (silane) . 5.16 (storage tank) PTFE , 250 mm 10 mm . 5.17 (gas chromatograph) , , (GCMS) . 5.18 (capillary column) , 30 m, (polysiloxane) 0.2
11、2 mm . benzoapyrene benzoepyrene . 6 , , KS M ISO 103811, ISO 103818 . 10 () 7 . ISO 103818 1 kg . KS M ISO 14507 ( 8.4, 8.3 ) . KS M ISO 16720 . 2 mm 2 mm . KS M ISO 11465 . 7 7.1 7.1.1 A(2) 1025 g (5.7) 100 mL ( ) (5.12) . (4.12.3) 1 mL( 10 g) (4.2) 50 mL PTFE (5.3) 1 . (4.3) 50 mL , 50 mL . . (4.
12、1) 400 mL 2 . . (4.7) , (5.4) (keeper) (4.5) 100 L . 40 (5.5) (5.4) 10 mL . . GCMS 1 g/mL . 6 KS I ISO 18287:2007 . , , , (PFE) . . 7.1.2 B(1) 1025 g 500 mL (5.7) . (4.12.3) 1 mL 50 mL(4.1), (NaCl) 40 g(4.6), 100 mL(4.2), (4.3) 50 mL PTFE (5.3) 6 . (4.7) 1 . (5.12) . (, 30 mL) (5.4) (4.5) 100 L . 40
13、 (5.5) (5.4) 2 mL . . GCMS 1 g/mL . . 7.2 . . . ( ) 80 % . . (5.15) (4.10) 4 g . (4.7) 1 cm , (4.3) 10 mL . (2 mL) (5.10) . 1 mL 2 . (4.3) 70 mL . (4.5) 100 L 0.5 mL . (4.4) 2 mL . GCMS 1 g/mL . 1 . 2 (ammonium oxide) . 7.3 7.3.1 (5.17) . 7 KS I ISO 18287:2007 . :, , 0.25 m, 30 m, 0.25 mm :60 2 30 /
14、 120 5 / 300 300 15 :260 (splitless injection):1 L, 1.8 (split) :, 0.81 mL/min 7.3.2 (MS) MS :295 :6 (mass number) : ( 2) (selected ion monitoring mode) . 2 (amu) Naphthalene-d 8 () 136 Naphthalene 128(129) Acenaphthylene 152(151) Acenaphthene-d 10 () 164 Acenaphthene 154(153) Fluorene 166(165) Phen
15、anthrene-d 10 () 188 Phenanthrene 178(179) Anthracene-d 10 () 188 Anthracene 178(89) Fluoranthene-d 10 () 212 Fluoranthene 202(101) Pyrene 202(101) Benzaanthracene-d 12 () 240 Benzaanthracene 228(114) Chrysene 228(114) Benzobfluoranthene-d 12 () 264 Benzobfluoranthene 252(253) Benzokfluoranthene 252
16、(253) Benzoapyrene 252(253) Benzoepyrene-d 12 () 264 Perylene-d 12 () 264 Indeno1,2,3-c,dpyrene 276(138) Dibenzahanthracene 278(139) Benzoghiperylene 276(138) 8 KS I ISO 18287:2007 7.3.3 , . , . (10 g) . . 4.12.4 GCMS . (1) ( ) . b s A A d n d n .(1) A n : A d : s : n : ( g/mL) d : (deuterated) ( g/
17、mL) b : y 8 (2) . V f w m s b A A w d s d n n ) / ( .(2) w n : (mg/kg, ) A d : A n : d : ( g/mL) m : (g) w s :KS M ISO 11465 (%, ) f : B (, 150 mL) (, 30 mL)( f5) V : (mL) s : b : y mg/kg . 9 (performance characteristics) B . 10 (quality assurance) 9 KS I ISO 18287:2007 . 11 . a) b) c) ( A B) d) e)
18、10 KS I ISO 18287:2007 A () GCMS A.1A.3 5 . X () Y (%) A.1 (GC MS ) X () Y (%) A.2 10 ng/L(20 ng/) (GC MS ) 11 KS I ISO 18287:2007 X () Y (%) A.3 ( B: 150 mL 10 mL, 1 mL) A.1 ( A.3 .) Naphthalene NP C 10 H 8128.18 6.96 Acenaphthylene ACY C 12 H 8152.20 13.00 Acenaphthene ACE C 12 H 10154.20 13.38 Fl
19、uorene FLN C 13 H 10166.23 15.87 Phenanthrene PHE C 14 H 10178.24 20.65 Anthracene ANT C 14 H 10178.24 20.84 Fluoranthene FLU C 16 H 10202.26 26.70 Pyrene PYR C 16 H 10202.26 27.63 Benzaanthracene BaA C 18 H 12228.30 33.99 Chrysene CHR C 18 H 12228.30 34.15 Benzobfluoranthene BbF C 20 H 12252.32 39.
20、22 Benzokfluoranthene BkF C 20 H 12252.32 39.35 Benzoapyrene BaP C 20 H 12252.32 40.52 Indeno1,2,3-cdpyrene IcdP C 22 H 12276.34 46.45 Dibenza,hanthracene DBahA C 22 H 14278.35 45.38 Benzoghiperylene BghiP C 22 H 12276.34 45.72 GC :CARLO ERBA MEGA 5300 :SPB1701, SUPELCO 30 m, 0.32 mm, 0.25 m :, 5.0 70 kPa :50 1 20 / 90 5 / 290 5 12 KS I ISO 18287:2007 :PTV(Programmable Temperature Vaporizati