1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 21458 / AMPA KS I ISO 21458:2011 2011 9 2 http:/www.kats.go.krKS I ISO 21458:2011 : ( ) ( ) ( ) : (http:/www.standard.go.kr) : :2011 9 2 2011-0308 : : ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS I ISO 21458:2011 i . ii 1 1 2 1 3 1 4 2 5 2 6 4
2、 7 .5 8 5 8.1 .5 8.2 .6 8.3 (HPLC).7 8.4 7 8.5 .7 9 8 9.1 .8 9.2 .8 10 9 10.1 .9 10.2 .9 10.3 .9 11 .9 12 .10 A( ) 11 B( ) .12 C( ) .14 16 KS I ISO 21458:2011 ii 2008 1 ISO 21458, Water quality Determination of glyphosate and AMPA Method using high performance liquid chromatography (HPLC) and fluoro
3、metric detection , . KS I ISO 21458:2011 / AMPA Water quality Determination of glyphosate and AMPA Method using high performance liquid chromatography (HPLC) and fluorometric detection . . . . , . 1 , (AMPA) . 0.05 g/L . . 2 . . ( ) . KS I ISO 6058, (EDTA ) KS I SO 6059, EDTA KS I ISO 8466 1, (1 ) K
4、S M ISO 3696, 3 9- (FMOCCl) AMPA( 1 ) . KS I ISO 21458:2011 2 . . 1 g/mol CAS No. N-(phosphonomethyl)glycine C3H8NO5P 169.1 1071-83-6 AMPA Aminomethylphosphonic acid CH6NO3P 111.0 1066-51-9 4 . . , , 2 AMPA , (8.1 ). , (7. ). 5 , HPLC . . 5.1 , KS M ISO 3696 1 . 5.2 , Na2S2O3, CAS No.: 7772-98-7 5.3
5、 , CH3CN, HPLC , CAS No.: 75-05-8 5.4 , C4H10O, CAS No.: 60-29-7 5.5 ( 1 ) 5.5.1 , 97 %, CAS No.: 1071-83-6 5.5.2 AMPA, 97 %, CAS No.: 1066-51-9 5.5.3 , 97 % ( A ) (10 g/mL, ) . KS I ISO 21458:2011 3 5.5.4 AMPA , 1.0 g/L (5.5.1) AMPA(5.5.2) , 20 mL (6.8) (5.1) 20 mg , (5.1) 1.0 g/L . (4 3) 1 . 5.5.5
6、 AMPA , 30 g/L 30 g/L AMPA (5.5.4) . (6.8) 20 mL (5.1) 200 L (5.5.4) . 60 L (6.8) (5.1) 20 mL . (4 3) 1 . 5.5.6 , 30 g/L (5.5.3) (5.1) (6.8) 30 g/L . (4 3) 1 . 5.6 , c(KOH) 3 mol/L, CAS No.: 1310-58-3 100 mL (6.8) 16.8 g 70 mL 80 mL (5.1) . (4 3) 3 . 5.7 , c(HCl) 4 mol/L, CAS No.: 7647-01-0 500 mL (
7、6.8) 340 mL (5.1) 160 mL HCl( 37 %) . (4 3) 3 . 5.8 2 , c(KH2PO4) 0.05 mol/L, pH 5.4, CAS No.: 7778-77-0 (6.8 0.05) g 2 1 000 mL . (5.6) pH 5.4 0.05 . 1 . 5.9 2 , (C2H2O4 2H2O) 100 g/L, CAS No.: 6153-56-6 KS I ISO 21458:2011 4 (50 0.05) g 2 500 mL . (4 3) 2 . 5.10 (5.3) 300 mL 2 (5.8) 700 mL . 1 . 5
8、.11 10 , c(Na2B4O7 10H2O) 0.05 mol/L, CAS No.: 1303-96-4 (19 0.1) g 10 1 000 mL . (4 3) 1 . 5.12 9- , (C15H11ClO2) 1 mg/mL, CAS No.: 28920-43-6 50 mL 9- (FMOCCl: 97 %) 50 mL (5.3) . (4 3) 2 . 5.13 , 85 %( ), CAS No.: 7664-38-2 6 . . , (6.1 6.2 ) 1 . , HPLC . 6.1 1 , 20 mL 6.2 , 50 mL 6.3 , 30 g/L AM
9、PA (5.5.5) 30 g/L (5.5.6) 6.4 , , NH2 , 3 m 5 m, 2 mm 4.6 mm, 250 mm . . 3 m 5 m, 2 mm 4.6 mm, 250 mm C18 . C18 C.2 . KS I ISO 21458:2011 5 6.5 , 2 mL . 6.6 (HPLC), 6.6.1 , (5.10) 6.6.2 6.6.3 HPLC , 35 6.6.4 , exc 260 nm, em 310 nm 6.7 pH 6.8 , KS L ISO 104210 A, 20 mL, 100 mL, 500 mL . 7 (6.2) . ,
10、100 mL 2 mg (5.2) . 4 2 1 (6.2) 1 . 20 . 8 8.1 KS I ISO 6058 / KS I ISO 6059 . c(CaCO3) 3 mmol/L , 2 ( 9) . (8.1.1 8.1.2), . 3 (8.1.3) . 8.1.1 200 L (5.7) 3 mL pH 1 . 1 . (5.6) pH 6 7 . 8.2 . 8.1.2 KS I ISO 21458:2011 6 30 mL 300 L 2 (5.9) . pH 2 3 . 1 . (5.6) . 8.2 . 8.1.3 4 mL 0.625 mL 10 (5.11) 5
11、0 L EDTA(1 g/L, pH 9 ) . . 4 3 24 . 3 mL . 8.2 . 8.2 (7. ) , 3 mL . 1 (6.1) . 0.5 g/L 50 L (5.5.6) . 0.5 mL 10 (5.11) 5 . 3 mL (5.4) , 2 15 . 1.5 mL 0.25 mL (5.3) , 0.25 mL FMOCCl(5.12) . 60 . 40 L (5.13) . 1 100 % 30 , 30 . . 2 , . . 18 . 40 L (5.13) . 2 mL (5.4) 2 , 1 , (6.5) . 4 3 2 ( 4 ) . , 2 1
12、 . 15 , . KS I ISO 21458:2011 7 2 1 (6.1) (0 g/L, 0,5 g/L 1 g/L) (5.11) 0.5 mL 0.5 mL 0.5 mL 3 mL 3 mL 3 mL AMPA , g/L(5.5.5) 0 L 50 L 100 L 8.3 (HPLC) 8.3.1 . . . 8.3.2 ( , 5.10, 6.4, C ) HPLC AMPA . ( , ) . 260 nm 310 nm . 8.4 , (5.1) . ( 10 % ) , . 8.5 . , 1 %(10 s) . , . , . , , NH2 C18 . AMPA 6
13、 . KS I ISO 21458:2011 8 9 9.1 . . , (5.5.5) (0.05 g/L 2.0 g/L) KS I ISO 8466 1 5 . ( , ) . . yie( ) , , ie . (ie, yie) , (1) . , i yie . iiiibay +=ee (1) ai i (g/L) bi i ie i (g/L) 9.2 AMPA , . . . yie/yint,ie , , ie/int,ie . (ie/int,ie, yie/yint,ie) , (2) . i,yie/yint,ie i , . iiiiiibayy+=eint,eei
14、nt,e(2) ai i KS I ISO 21458:2011 9 bi i ie i (g/L) int,ie i (g/L) 10 10.1 (3) i ig g/L . iiiiaby )(gg-= (3) ai i (g/L) bi i yig i 10.2 (4) i , ig g/L . gint,gint,gg)/(=iiiiiiabyy-(4) ai i bi i yig i yint,ig i int,ig i (g/L) 10.3 AMPA ig . . . c(CaCO3) 3 mmol/L . . 2 i , g/L . . i . 11 KS I ISO 21458
15、:2011 10 g/L . 0.15 g/L AMPA 1.2 g/L 12 . a) (KS I ISO 21458) b) c) d) 11. e) f) , KS I ISO 21458:2011 11 A ( ) A.1 L- 1 , C3H7NO5S H2O, CAS No.: 23537-25-9 . A.2 O- -L- , C3H8NO6P, CAS No.: 407-41-0 A.3 2- , C2H8NO3P, CAS No.: 2041-14-7 KS I ISO 21458:2011 12 B ( ) 2007 2/4 ( 8), B.1 . B.1 po pref
16、CV(r) sr CV(R) sR nl nm% g/L g/L % g/L % g/L 25 83 21 0.100 0.103 5.1 0.005 28.6 0.0291. , AMPA 25 85 17 0.116 0.118 5.0 0.006 30.0 0.035 25 85 0 0.816 0.803 4.1 0.033 29.8 0.2392. , AMPA 25 87 13 0.958 0.949 3.8 0.036 21.2 0.201 25 83 13 0.204 0.194 6.1 0.012 31.9 0.0623. , AMPA 25 85 4 0.240 0.209
17、 7.4 0.015 29.2 0.061 25 85 17 1.632 1.574 4.5 0.071 33.7 0.5314. , AMPA 25 87 21 1.917 1.932 3.7 0.071 17.0 0.329 25 83 21 0.510 0.558 3.6 0.020 29.9 0.1675. , AMPA 25 87 8 0.599 0.790 5.6 0.044 17.1 0.135 25 85 8 5.100 4.720 5.6 0.264 37.9 1.7906. , AMPA 25 83 8 5.990 6.180 3.8 0.235 24.3 1.504 B.
18、2 . KS I ISO 21458:2011 13 B.2 Na+ mg/L K+ mg/L Mg2+ mg/L Ca2+ mg/L 7.1 0.9 0.53 0.05 41 6 141 21 15 2 1.1 0.1 44 6 166 25 12 1 2.4 0.2 11 2 195 30 KS I ISO 21458:2011 14 C ( ) NH2 . AMPA . 150 . : NH2 : 3 m : 4.6 mm : 250 : 35 : 50 L : 2.5 pg : AMPA 15.268 : 5.115 : 260 nm, : 310 nm PMT ( ) 2 0.05
19、mol/L, pH 5.4 30 % 70 % 2 : 1 mL/min h t , aAMPA b C.1 NH2 ( AMPA 2.5 pg ) KS I ISO 21458:2011 15 : C18 : 5 m : 3 mm : 250 : 27 : 25 L : 0.25 ng : AMPA 10.707 , 14.214 : 260 nm, : 310 nm A: 2 ( 0.002 mol/L 2 pH 7.0 ) B: 0 25 93 % 43 % A 25 27 43 % 5 % A 27 35 5 % A 35 37 5 % 93 % A : 1 mL/min h t a bAMPA C.2 C18 ( AMPA 0.25 ng ) KS I ISO 21458:2011 16 1 ISO 6101 3, Rubber Determination of metal content by atomic absorption spectrometry Part 3:Determination of copper content 2 MILES, C.J., W