1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 18856/ KS I ISO 18856 :2010 2010 8 31 http:/www.kats.go.krKS I ISO 18856:2010 : ( ) ( ) ( ) ( ) : (http:/www.standard.go.kr) ： ：2005 12 14 ：2010 8 31 2010-0347 ： ： ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 18856:2010 i .1 1 1 2 2 3 2
2、 4 3 5 4 6 6 7 .8 8 9 9 12 10 14 11 .16 12 16 13 .16 A() 17 B() .19 C() .20 D() () .22 E() 25 F() 29 G() 30 32 KS I ISO 18856:2010 / Water qualityDetermination of selected phthalates using gas chromatography/mass spectrometry 2004 1 ISO 18856, Water qualityDetermination of selected phthalates using
3、gas chromatography/mass spectrometry , . . . . . 1 / . 0.02 g/L , 0.150 g/L , , ( 1 ) . 1 . ( A ) . B . KS I ISO 18856:2010 2 1 g/mol CAS a 1 C 10 H 10 O 4DMP 194.2 131113 2 C 12 H 14 O 4DEP 222.24 84662 3 C 14 H 18 O 4DPP 250.3 131168 4 C 16 H 22 O 4DiBP 278.4 84695 5 C 16 H 22 O 4DBP 278.4 84742 6
4、 C 19 H 20 O 4BBzP 312.4 85687 7 C 20 H 26 O 4DCHP 330.4 84617 8 (2) C 24 H 38 O 4DEHP 390.6 117817 9 (n) C 24 H 38 O 4DOP 390.6 117840 10 C 28 H 46 O 4DDcP 446.7 84775 11 C 30 H 50 O 4DUP 474.4 3648202 a CAS：Chemical Abstracts System 2 . . ( ) . KS I ISO 56671, ( ) KS I ISO 56672, 2： KS I ISO 56673
5、, 3： 3 . , . 1 . KS I ISO 18856:2010 3 1 4 , . 4.1 (cross-contamination) , ( ) . 4.2 (enrichment) . (batch-to-batch) . . , . . . . KS I ISO 18856:2010 4 . . . 80 ng/L( C ). 4.3 (septa) . . . . 5 . . (blank) . , . 5.1 , , (9.3). . 5.2 N 2 , 99.9 % 5.3 He, 99.999 % 5.4 / , . 5.5 , C 4 H 8 O 2 5.6 CH 3
6、 OH 5.7 C 8 H 18 (2,2,4-trimethypentene) 5.8 (quartz-wool) KS I ISO 18856:2010 5 4 400 . 5.9 C18(RPC18) , , 4.2 . (break-through rates) RPC18 . 5.10 , Al 2 O 3 , (50 200 ) m, 4 400 6 . . (baking) 5 . Florisil 1) . , 4.2 . 5.11 (diallyl phthalate), DAIP, C 14 H 14 O 4 ：D4-ring-deuterated dibutyl phth
7、alate, “D4DBP”, D4C 16 H 22 O 4 ：D4-ring-deuterated di(n-octyl) phthalate, “D4DOP”, D4C 24 H 38 O 4 , 13 C (6 12) - labelled () 5.12 1 . 5.13 (single substances) 10 mL (6.15), (5.5) 10 mg , ( 1 g/L). 18 . 3 . 5.14 (stock-solution) 10 mL (6.15) (100 500 ) L , (10 50 ) mg/L. 18 . 3 . 5.15 (5.14) (5.17
8、) (5.5) . 1) Florisil . ISO . KS I ISO 18856:2010 6 18 . 3 . 5.16 (5.5) (5.14) . 5.17 ( D ) 5.17.1 D4-ring-deuterated-di(n-octyl) phthalate(D4-ring-DOP) 5 mL (5.5) 10 mL (6.15) 0.1 g D4DOP (5.11) , . 5.17.2 D4-ring-deuterated-dibutyl phthalate(D4-ringDBP) 5 mL (5.5) 10 mL (6.15) 0.1 g D4DBP (5.11) ,
9、 . 5.17.3 I 5 mL 10 mL 0.1 mL 1 ：100 , (5.17.1 5.17.2) . . 5.17.4 II I(5.17.3), 250 L 250 mL (6.15) (5.5) . D4DBP D4DOP 0.1 mg/L . 5.17.5 III 5 mL 10 mL (6.15) I(5.17.3) 1 mL , (5.5) . D4DBP D4DOP 10 mg/L . 5.18 (5.13) (5.5), 1 ：1 000 . , D 6 . (8.1 ). E . 6.1 KS I ISO 18856:2010 7 , 1 000 mL 2 000
10、mL . 6.2 (10510) . 6.3 400 60 L 6.4 (, , E.4 ) 6.5 (stainless steel cock) Luer 2) polytetrafluoroethane(PTFE) 6.6 5 L 6.7 (vial), , , PTFE , , 2 mL , GC . 6.8 KS L 2320(ISO 383), DN 14/23(E.1 ) Luer 2) . 6.9 , 4 cm 35 cm KS L 2320(ISO 383), DN 14/23(E.3 ) 6.10 PTFE-frits 6 mL 6.11 4.5 cm, (3.4 4.5 )
11、 cm (circular depression) Luer 2) 0.5 cm (E.2 ) . 6.12 (foil) 400 2) Luer . ISO .KS I ISO 18856:2010 8 6.13 (stainless steel reservoir) . 6.14 250 mL 500 mL 6.15 1 mL, 2 mL, 10 mL, 25 mL, 250 mL 6.16 Pasteur 2 mL 6.17 2 % 2 L, 5 L, 10 L, 50 L, 100 L 500 L 6.18 (GC) , 6.19 (fused silica capillary col
12、ums) ( F ) 0.32 mm, 30 m , (0.10 0.50 ) m . (5.16) . 6.20 (graduated) 10 mL 6.21 7 KS I ISO 56671, KS I ISO 56672 KS I ISO 56673 . (6.1 8.1) . . . , ( .) . , 5 . . . , 4 KS I ISO 18856:2010 9 4 . . , . . 8 8.1 105 (6.2) . (6.3) . 2.5 / 100 . 250 10 / . 400 75 . 12 . . (6.12) ( ) . () . , Pasteur (6.
13、16) (5.7) . . . . 8.2 8.2.1 (conditioning of the solid phase material and enrichment) . a) PTFE-frit(6.10) . b) RPC18 (5.9) 250 mg . c) (quartz wool)(5.8) . (6.8) (RPC18). (5.5) (one bed) . 10(5.2) . (5.6) (two bed) . , (6.5) . KS I ISO 18856:2010 10 (6.9 8.1) (6.8) . 250 mL (6.14) (6.9) . ( sam) V
14、sam . , (6.11) . . (6.4) (2 10 ) mL/min( 700 hPa) (6.8) . SPE (6.6) (6.4) . (6.4) 5 (5.2 6.21) , . (6.20) , (6.4) 2 mL (5.17.4) . 2 mL , . . GC (6.7) ( ex) V ex . , (6.12) , . 8.2.2 , . PTFE frit(6.10) , Al 2 O 3 (5.10) 1 g . (one bed) (5.5) Al 2 O 3 (5.10) . 1 (5.2) . (6.20) . GC (6.7) (6.12) , , .
15、 8.3 GC (6.18) . (6.19 G ) . , GC (6. ) 5 (5.5) . KS I ISO 18856:2010 11 8.4 (blank monitering) . , RPC18 (8.2.1) (7. ) . . . 8.2.18.3 . 8.5 8.5.1 . . . , . 8.5.2 (mass spectrometric detection) , . (ion-current) (t R ) t R 0.03 . , . , . ( 2 ) 20 % . KS I ISO 18856:2010 12 2 M 1 a M 2 a M 3 a1 DMP 1
16、63 194 135 2 DEP 149 177 222 3 DPP 149 209 191 4 DiBP 149 223 5 DBP 149 223 278 6 BBzP 149 206 312 7 DCHP 149 167 249 8 (2) DEHP 149 167 279 9 (n) DOP 149 279 207 10 DDcP 149 307 11 DUP 149 321 12 D4 D4DBP 153 13 D4(n) D4DOP 153 14 DalP 149 189 132 a M 1 . M 2 M 3 . 9 9.1 , . . 5 5 . . . , . , (5.15
17、 ). , . 9.2 , 5 (5.15) . , 1 . KS I ISO 18856:2010 13 . (5.13) . (5.15) (aliquot) . . , i ( std ) y i,std (, ) , i,std . . y i,std a i i,std b i (1) y i,std ： , i ( std) i,std a i ： (areaL/ g), i (substance-specific) i,std ： i( ) ( g/L) b i ： i , . . 9.3 (determination of the within-laboratory recovery) , , i . , 250 mL ( .) (spiking) (5.16) . . 9.2 , (2) (3) i (substance specific mean recovery) i . N k i N k i , 1 (2) ,def , rec , , , k i k i k i (3) i ： i N ： i,k i,k ： k i KS I ISO 18856:2010 14 i,k,rec ： (ng/L), k i
