1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 11369 ( ) KS I ISO 11369:2008 2008 8 7 http:/www.kats.go.krKS I ISO 11369:2008 : ( ) ( ) ( ) : (http:/www.standard.go.kr) : : 1998 12 24 : 2008 8 7 2008-0411 : : ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 11369:2008 ( ) Water quality D
2、etermination of selected plant treatment agents Method using high performance liquid chromatography with UV detection after solid-liquid extraction 1997 1 ISO 11369, Water quality Determination of selected plant treatment agents Method using high performance liquid chromatography with UV detection a
3、fter solid-liquid extraction . 1 (HPLC) . 0.1 g/L ( ) . 0.05 g/L ( 1 ). . 1 (1992) . A . KS I ISO 11369:2008 2 1 CAS ab C8H14CIN5215.7 001912 24 9 T C10H13CIN2O 212.7 015545 48 9 H c9H13CIN6240.7 021725 46 2 T dC6H9CIN5186.6 006190 65 4 T C9H10Cl2N2O 233.1 000330 54 1 H c12H20N4O2252.3 051235 04 2 T
4、 C12H18N2O 206.3 034123 59 6 H C9H10CI2N2O2249.1 000330 55 2 H C14H16CIN2O3277.8 067129 08 2 A C10H11N3OS 221.3 018691 97 9 H cC9H11BrN2O2259.1 003060 89 7 H C15H22CINO2283.8 051218 45 2 A c10H13CIN2O2228.7 19937 59 8 H C9H11CIN2O2214.6 1746 81 2 H cC9H15CIN5228.7 00728 69 3 T C7H12CIN5201.7 000122
5、34 9 T C9H16CIN5229.7 005915 41 3 T aCAS : b T: , H: , A: c . d 2 2.1 RP( ) C 18 . . . 1 . . . . 2.2 HPLC . . 3 . . KS I ISO 11369:2008 3 KS M ISO 5667 1, ( ) KS M ISO 5667 2, 2: KS M ISO 5667 3, 3: KS M ISO 8466 1, (1 ) 4 RP C l8(RP ) , (HPLC) . 5 5.1 , ( HPLC ) , . 5.2 . 5.3 HPLC (6.13 ) . 5.4 c(H
6、3PO4) 1 mol/L 5.5 c(NaOH) 1 mol/L 5.6 RP C 18 . 2.1 . , 2.1 . 5.7 (CH3OH), (CH3CN) (C3H6O) . . 5.8 (reference standards)( 1 ) . 5.9 (5.8 ) 50 mg( ) 100 mL (5.7 ) . KS I ISO 11369:2008 4 (simazine) . 4 . 1 . . 5.10 (stock solution) (5.9 ) 1 mL 100 mL (5.7) . 4 . 1 . 5.11 (reference solutions) (5.10)
7、5 , i 20 ng/mL200 ng/mL . HPLC . 4 . 1 . 5.12 20 mmol/L (CH3COONH4), (CH3COONa) ( ) 0.45 m . . 2 . 6 6.1 . , (PTFE) . 6.2 9 mm, 8 cm RP C 18 6.3 PTFE 1 000 mL 2 000 mL . 6.4 10 mL 1 000 mL . KS I ISO 11369:2008 5 6.5 12 mL . 6.6 6.7 PTFE . 6.8 1 mL, 10 mL 100 mL . 6.9 HPLC , 25 L, 50 L, 100 L, 250 L
8、 1 000 L . 6.10 0.75 m1.5 m . 6.11 0.2 m0.45 m . 6.12 . 6.13 HPLC . 6.14 300 mm , 2 mm4.6 mm 3 m5 m RP C 18 . 1( ) . 6.15 . a) b) , c) 1 d) 200 nm350 nm , 2 e) 7 (6.3 ) . KS I ISO 11369:2008 6 . . . . KS M ISO 5667 1, KS M ISO 5667 2 KS M ISO 56673 . 4 . 4 1 . 8 8.1 . 1 ( , , , , ) . . C 18 . . A .
9、8.2 RP C 18 (conditioning) 1 000 mL RP C 18 (5.6 ) 1 g2 g . 1 L 1 g/L . RP C 18 (5.7 ) 5 . (5.1 )( 5 ) , . 8.3 , . (spiked sample) . 1 000 mL (5.4 ) (5.5 ) pH 68 . KS I ISO 11369:2008 7 3 mL/min15 mL/min 1 g . 2 g 25 mL/min . . ( 200 mL/min 45 ) . 8.4 RP C 18 (5.6 ) 500 mg (5.7 ) 1 mL . (conical bot
10、tom) . 15 . . . 35 30 , . HPLC , 1 mL . . . HPLC . 8.5 (HPLC) 8.5.1 . (signal noise) (drift) . 8.5.2 1 (6.14 ) . ( 1 2 ). 1 . . 2 (band broadening) . 4 mm 100 L . 8.5.2.1 1 a)c) KS I ISO 11369:2008 8 : 25 L( i 100 ng/mL) : 2 mmol(pH 6.5) : ODS 3 m(250 mm4 mm) : A 2 mmol(pH 6.5)/ /8: 2 B : 75 10 % B
11、45 % : B/10 % A 10 : 10 : 0.35 mL/min : 40 : d 10 nm, 640 ms 218 nm, 230 nm, 245 nm, 4 nm : 460 nm, 80 nm a) 218 nm 1 ( )218 nmKS I ISO 11369:2008 9 b) 230 nm c) 245 nm 1 ( ) ( )230 nm245 nm ( )KS I ISO 11369:2008 10 2 / 1 10 2 11 3 12 4 13 5 14 6 15 7 16 8 17 9 8.5.2.2 2 / : 50 L( i= 5-20 ng/L) : :
12、 120-3; 3 m(250 mm4 mm) : A 20 mmol, /; 75/25 B : 30 60 0 % B9.5 % B B 30 87 % : 5 : 15 : 1 mL/min : 40 ; 4.5 L, d 6 mm ( )KS I ISO 11369:2008 11 218 nm, 230 nm, 245 nm, 4 nm : 550 nm, 100 nm 1 10 2 11 3 12 4 13 5 14 6 15 7 16 8 17 9 8.5.3 ( 218 nm, 230 nm, 245 nm) ( ) . 200 nm350 nm . 8.6 (5.1 ) (8
13、.18.5) HPLC . ( 10 % .), . 8.7 1 . . . . (8.5.3 ). . . 1 % 10 . 2 . N- ( ) . . KS I ISO 11369:2008 12 . ( ) 10 % ( ) , . 2 ( ) (9.10.2 ) 10 % . ( .) . 3 (GC), GC (HPTLC) . 9 9.1 . 2 . a) HPLC (9.2 ) , . b) (spiked) (9.3 ) 5 . ( ) . (9.3 ) (9.4 ) (9.2 ) . mi mig 9.4 . . HPLC . 2 (10.1 ). 2 . 2 i e g
14、j 9.2 HPLC ( ) KS I ISO 11369:2008 13 5 . 1 . . (5.9 ) . (5.11 ) . . . i yie( , ) ie . ie yie . iieiiebmy += (1) yie : ie i . . ie : i ( )(g/L) mi : i ( ). (L/g) bi : 9.3 ( ) (5.11 ) 1 mL ( 5 ) (control) (5.1 ) ( , 1 000 mL) (5.11 ). . 9.2 yieg egi . yiegi iegi . igiegigiegbmy += (2) yieg: e i . . e
15、g : i (g/L) mig : i big : i 9.4 (5.1 ) . (mean specific recovery),iA . KS I ISO 11369:2008 14 , 1 000 mL (5.1 ) (5.11 ) 1 mL . (3) (4) i iA 10.1 10.2 . NAA=N1Nni, i (3) N: Ai nnomi,nfdi,ni, =A(4) Ai.n : n i i,nfd : n i , (1) (g/L) i,nnom : n i ( ) (g/L) 8. . . iA . 10 10.1 (5) i i . i iioi)(AVmVbVii=