KS I ISO 17353-2010 Water quality－Determination of selected organotin compounds－Gas chromatographic method《水质 选择的有机化合物的测定 气体色谱法》.pdf

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1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 17353 KS I ISO 17353 :2010 2010 8 24 http:/www.kats.go.krKS I ISO 17353:2010 : ( ) ( ) ( ) : (http:/www.standard.go.kr) ： ：2005 12 14 ：2010 8 24 2010-0334 ： ： ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 17353:2010 i .1 1 1 2 2 3 .2 4 2

2、 5 (Interferences).2 6 2 7 7 8 10 8.1 .10 8.2 .11 8.3 12 8.4 .12 9 13 9.1 .13 9.2 13 10 15 11 17 11.1 17 11.2 18 12 18 13 .18 A() 20 B() .30 32 KS I ISO 17353:2010 Water qualityDetermination of selected organotin compounds Gas chromatographic method 2004 ISO 17353, Water qualityDetermination of sele

3、cted organotin compoundsGas chromatographic method , . . . . . 1 2 g/L , , 1 . (10 1 000 ) ng/L. . R , n12 R , n12 . . 1 R n Sn (4n) R n BuSn 3 1 MBT Bu 2 Sn 2 2 DBT Bu 3 Sn 3 TBT Bu 4 Sn 4 TTBT OcSn 3 1 MOT Oc 2 Sn 2 2 DOT Ph 3 Sn 3 TPhT Cy 3 Sn 3 TCyT KS I ISO 17353:2010 2 2 . . ( ) . KS I ISO 566

4、71, 1： KS I ISO 56672, 2： KS I ISO 56673, 3： KS M ISO 3696, 3 . 3.1 OTC (Sn)(C) . 3.2 OC ( ) OC . OC MBT, DBT, TBT, TTBT, MOT, DOT, TCyT, TPhT . 4 . () . 4 OTC , MS(), FPD(), AED( ) . . 5 (Interferences) . (A.4.6 ). 6 . 6.1 , KS M ISO 3696 1 KS I ISO 17353:2010 3 6.2 , (HNO 3 )1.4 g/mL 6.3 , CH 3 CO

5、OH, (glacial) 6.4 , c(NaOH)1 mol/L 6.5 , CH 3 COONa, 6.6 , Na 2 SO 4 , 6.7 , (0.2 0.063 ) mm(200 63 ) 6.8 , C 4 H 8 O, . 6.9 (), (CH 3 ) 2 CO 6.10 , CH 3 OH 6.11 , C 6 H 146.12 , NaB(C 2 H 5 ) 46.13 , MBTCI, C 4 H 9 SnCl 36.14 , DBTCl, (C 4 H 9 ) 2 SnCl 26.15 , TBTCl, (C 4 H 9 ) 3 SnCl 6.16 , TTBT,

6、(C 4 H 9 ) 4 Sn 6.17 , MOTCl, C 8 H 17 SnCl 36.18 , DOTCl, (C 8 H 17 ) 2 SnCl 26.19 , TPhTCl, (C 6 H 5 ) 3 SnCl 6.20 , TCyTCl, (C 6 H 11 ) 3 SnCl 6.21 , MHTCl, C 7 H 15 SnCl 3 () 6.22 , DHTCl, (C 7 H 15 ) 2 SnCl 2 () 6.23 , TPTCl, (C 3 H 7 ) 3 SnCl() 6.24 , TTPT, (C 3 H 7 ) 4 Sn() 6.25 /( , , , , 4

7、) KS I ISO 17353:2010 4 . . 6.25.1 , A 1 mg/mL 100 mL 2 0.1 mg . (6.10). . 4 , 1 . 6.25.2 , B 100 mL 0.1 mg , 120 mg 150 mg 115 mg 100 mg . . 2 1 mg/mL OC 122.4 mg, 148.8 mg, 114.3 mg, 100 mg 100 mL . 4 3 . 2 ( 100 % ) a bmg c 0.623 160.5 A 0.767 130.4 A 0.891 112.2 A 1.000 100.0 A 0.686 145.8 A 0.8

8、30 120.5 A 0.908 110.1 A 0.912 109.6 A 0.672 148.8 B 0.817 122.4 B 0.875 114.3 B 1.000 100.0 B a (OC)/ (OTC) b , OTC . c A B KS I ISO 17353:2010 5 6.25.3 3 . 100 mL 3 . . (10 1 000 ) ng/mL . 1： 100 . 3 OC ng/mL mL mL OC ng/mL A 1 000 000 10 100 100 000 A1 A1 100 000 10 100 10 000 A2 A1 100 000 15 10

9、0 15 000 A3 A2 10 000 20 50 4 000 A4 A2 10 000 5 100 500 A5 A2A3 10 000/15 000 16 100 1 000 AH6 A2A3 10 000/15 000 15 100 850 AH5 A2A3 10 000/15 000 14 100 700 AH4 A2A3 10 000/15 000 13 100 550 AH3 A2A3 10 000/15 000 12 100 400 AH2 A2A3 10 000/15 000 11 100 250 AH1 A4 4 000 6 100 240 AM6 A4 4 000 5

10、100 200 AM5 A4 4 000 4 100 160 AM4 A4 4 000 3 100 120 AM3 A4 4 000 2 100 80 AM2 A4 4 000 1 100 40 AM1 A5 500 7 100 35 AL6 A5 500 6 100 30 AL5 A5 500 5 100 25 AL4 A5 500 4 100 20 AL3 A5 500 3 100 15 AL2 A5 500 2 100 10 AL1 AH1AH6 AH ( ). AM1AM6 AM ( ). AL1AL6 AL ( ). AH1AH6 A2 A3 . 6.25.4 1：100 . 100

11、 mL 1 mL B( 4 ) . (6.10) ( B1). 100 mL B1 1 mL . ( B2). KS I ISO 17353:2010 6 B2 . B2 6.25.1( 2) 100 ng/mL . 4 OC ng/mL mL mL OC ng/mL B 1 000 000 1 100 10 000 B1 B1 10 000 1 100 100 B2 6.25.5 1 000 mL (6.1) 1 L . 6.25.6 ( ) 6 . 10 . 6 1 000 mL 1 000 mL . , (AH1 AH6, AM1 AM6, AL1 AL2, 3 ) 1 mL . 20

12、. , OC . ：1 000 ng/L, 850 ng/L, 700 ng/L, 550 ng/L, 400 ng/L, 250 ng/L ：240 ng/L, 200 ng/L, 160 ng/L, 120 ng/L, 80 ng/L, 40 ng/L ：35 ng/L, 30 ng/L, 25 ng/L, 20 ng/L, 15 ng/L, 10 ng/L 6.25.7 1 000 mL 500 mL (6.1) 1 (82 g ) . (6.3) pH 4.5 . (4.5) . 6.25.8 A( 2 %) 10 mL 200 mg (6.12) (6.1) . . 6.25.9 B

13、( 20 %) 10 mL (6.12) 2 g (6.8) . 3 . . KS I ISO 17353:2010 7 6.25.10 (250 300 ) g (6.6) 180 4 . . . 6.25.11 (column) 120 g . ( 520 .) 12 (50020) . 200 , . 3 % . 2 (shaker) . . 0.1 % . 6.25.12 . (7.6 ) 5 g (6.25.11) 3 g (6.25.10) . 30 mL (6.11) . . (pre-packed) . 6.25.13 n . n . 100 mL (6.9) . (6.11)

14、 . 7 (A.4.5 ). 7.1 10 mL, 50 mL, 100 mL, 1 000 mL . 7.2 1 mL, 2 mL, 3 mL, 4 mL, 5 mL, 6 mL, 7 mL, 10 mL, 15 mL, 20 mL, 50 mL . KS I ISO 17353:2010 8 7.3 10 L, 250 L . 7.4 1 000 mL , . 7.5 1 000 mL 7.6 15 cm , 1 cm , frit . 7.7 150 mL 5 L . 7.8 (shaker) 7.9 (magnetic stirrer) 1 200 min 1 . 60 mm4.5 m

15、m . 7.10 100 mL, 250 mL . 7.11 7.12 (50020) . 7.13 180 . 7.14 12 cm . 7.15 7.16 KS I ISO 17353:2010 9 Schultze ( 1 ) 7.17 (7.19 ) . 7.18 (split or splitless), . 7.19 . 7.19.1 (FPD) 590 nm 610 nm 610 nm 390 nm . 7.19.2 (EI) . 7.19.3 KS I ISO 17353:2010 10 ：mm 1 2 (ground glass joint) 1 Schultze 8 8.1

16、 KS I ISO 56671, KS I ISO 56672, KS I ISO 56673 . KS I ISO 17353:2010 11 , , 1 000 mL (7.4) . (8.2.1 ) . 1 L 1 000 mL . . 24 (8.2 ). . 8.2 8.2.1 , . (10 1 000 ) ng/L (6.1) . . 1 L 1 L . . . . , , (6.25.6) (6.25.5) . 10 mL (6.25.7) 1 . pH (6.3) (6.4) pH 4.5 . ( 1 200 min 1 ) (7.9) B2(6.25.4) 1 mL . 2

17、0 . . . 8.2.2 (8.2.1) 5 mL A(6.25.8) 0.5 mL B(6.25.9) . (6.11) 20 mL 1 . pH (6.3) (6.4) pH 4.5 . 20 . (6.1) (7.16) . 100 mL 2 g (6.6) . (7.11) 1 mL , . 1 mL . KS I ISO 17353:2010 12 , (40 50 ) (30 45 ) kPa . . , , , . ( ) , . 8.3 , . . (6.25.12) . , 1 mL (6.25.13) . , (6.25.13) , 100 mL . (7.11) 1 m

18、L , . 1 mL . , (40 50 ) (30 45 ) kPa . . , , , . ( ) , . 8.4 . . ( ), . . . () , 6 () . , . . KS I ISO 17353:2010 13 9 9.1 . 0.05 min , 0.2 % . 9.2 9.2.1 . , . . , . (9.2.2 ) . 9.2.2 . 6(A Mh1 , A Mh2 , A Ml1 , A Ml2 ) . F h ( ) F l ( ) . 2 Mh 1 Mh h A A F (1) 2 Ml 1 Ml l A A F (2) F h ： ( h) F l ：

19、( l) A Mh1 ： ( h) ( 1) A Mh2 ： ( h) ( 2) A Ml1 ： ( l) ( 1) A Ml2 ： ( l) ( 2) KS I ISO 17353:2010 14 5 a1/a2 b1/b2 c1/c2 235.1/233.0 179.0/177.0 151.0/149.0 263.1/261.1 179.0/177.0 151.0/149.0 291.1/289.1 263.1/261.1 179.0/177.0 291.1/289.1 235.1/233.0 179.0/177.0 291.1/289.1 179.0/177.0 151.0/149.0 375.2/373.2 263.1/261.1 151.0/149.0 351.0/349.0 197.0/195.0 233.0/231.0 315.1/313.1 369.2/367.2 277.1/275.1 179.0/177.0 151.0/149.0 347.2/345.2 249.1/247.1 151.0/149.0 249.1/247.1 235.1/233.0 193.0/191.0 249.1/247.1 165.0/163.0 207.0/205.0 (a, b, c) ,