1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 23631, - (GC- ECD / GC-MS) KS I ISO 23631 ：2007 (2012 ) 2007 12 7 http:/www.kats.go.krKS I ISO 23631：2007 : ( ) ( ) ( ) () ( ) () : (http:/www.standard.go.kr) ： ：2007 12 7 ：2012 12 27 20120787 ： ： (ISO/TC147) ( 02-509-7270) (http:/www.kats.go.kr).
2、10 5 , . KS I ISO 23631：2007 .1 1 1 2 2 3 2 4 2 4.1 2 4.2 2 5 3 6 6 7 .8 8 .8 8.1 .8 8.2 9 8.3 .9 8.4 10 9 11 9.1 .11 9.2 .12 GC 9.3 .12 9.4 .12 9.5 13 10 14 10.1 .14 10.2 14 11 .15 12 .15 A() .16 B() .21 C() .25 27 i KS I ISO 23631：2007 (2012 ) , - (GC- ECD / GC-MS) Water qualityDetermination of da
3、lapon, trichloroacetic acid and selected haloacetic acidsMethod using gas chromatography(GC-ECD and/or GC-MS detection) after liquid-liquid extraction and derivatization 2006 1 Water qualityDetermination of dalapon, trichloroacetic acid and selected haloacetic acidsMethod using gas chromatography(GC
4、-ECD and/or GC-MS detection) after liquid-liquid extraction and derivatization , . . . . , . , . . . 1 , (GC-ECD / GC-MS ) , (TCA) ( 1 ) . , 0.510 g/L . TCA 0.05 g/L( C.1 ). (ECD) . (MS) . 1 . . KS I ISO 23631：2007 2 . . ( ) . KS M ISO 3696, KS M ISO 56671, 1： KS M ISO 56672, 2： KS M ISO 56673, 3： 1
5、 CAS (bromochloroacetic acid) C 2 H 2 BrClO 2173.4 5589968 a (dalapon) C 3 H 4 Cl 2 O 2143.0 75990 (dibromoacetic acid) C 2 H 2 Br 2 O 2217.8 631641 (dichloroacetic acid) C 2 H 2 Cl 2 O 2128.9 79436 (monobromoacetic acid) C 2 H 3 BrO 2138.9 79083 (monochloroacetic acid) C 2 H 3 ClO 294.5 79118 (tric
6、hloroacetic acid)(TCA) C 2 HCl 3 O 2163.4 76039 a2,2-(2,2-dichloropropionic acid) 3 , (TCA) - (Methyl-Tert- Butyl Ether)(MTBE) . . . (GC-ECD) / (GC-MS) . 4 4.1 . , (6.15) . 4.2 . . . GC . 2 KS I ISO 23631：2007 (5.6) (5.10) . ECD . (5.19 ). 5 . “ ” . . 5.1 KS M ISO 3696 1 5.2 / 5.3 , 99.999 %, 5.4 (d
7、iethylether), C 4 H 10 O . 5.5 , C 2 H 5 OH 5.6 (C 4 H 8 O 2 ), (C 3 H 6 O) 5.7 -(methyl-Tert-Butyl Ether)(MTBE), C 5 H 12 O 5.8 (benzoic acid) , c(C 7 H 6 O 2 ) 0.2 mol/L 5.9 N-N-4-(N-methyl-N-nitroso-4-toluenesulfonamide), C 8 H 10 N 2 O 3 S5.10 550 4 . 5.11 w(KOH)60 % 5.12 c(NaOH) 0.1 mol/L 5.13
8、5 (sodium thiosulfate pentahydrate), Na 2 S 2 O 3 5H 2 O5.14 (phenolphthalein), C 20 H 14 O 45.15 w(CH 3 COOH)10 % 3 KS I ISO 23631：2007 5.16 , w(HCl)25 % 5.17 (9.2) ( 1 ) 5.17.1 , 50 mg 100 mL , MTBE(5.7) , MTBE . 18 . 1 . 5.17.2 (multiple-substance) , (5.17.1) 2 mL 100 mL MTBE(5.7) . 18 . 1 . 5.17
9、.3 (multipoint) ( ) . (5.17.2) MTBE(5.7) . 10 (： ) . 6 . 5.18 5.18.1 (spiking water) ( , 1 ). (9.3 9.4) , (9.5) (spike). 5.18.2 , 50 mg 100 mL , MTBE(5.7) , MTBE . 18 . 1 . 5.18.3 -(multiple-substance) , (5.18.2) 2 mL 100 mL MTBE(5.7) . 4 KS I ISO 23631：2007 18 . 1 . 5.18.4 (multipoint) . (5.18.3) M
10、TBE(5.7) . 10 (, ) . 6 . 5.19 ( ) N-N-4-(N-methyl-N-nitroso-4-toluenesulfonamide) . , 1 . 1 . , . , (5.15) . (KOH) (5.11) 8 mL (5.5) 10 mL 250 mL . N-N-4-(N-methyl-N-nitroso-4-toluenesulfonamide)(5.9) 5 g (5.4) MTBE(5.7) 45 mL -(equalizing) . ( ) 60 , 20 (equalizing) N-N-4-(N-methyl-N-nitroso-4-tolu
11、enesulfonamide) (dropwise) . MTBE , . ( / ) (trap) MTBE . , ( MTBE) 10 mL . , 18 . . (intensive) . 1 . . N-N-4-(N-methyl-N-nitroso-4-toluenesulfonamide) (5.15) . (equalizing) . (5.5) 50 mL . ( ) . , . 0.2 mol/L (ethanolic benzoic acid) (5.8) 3 mL 5 KS I ISO 23631：2007 . (etheric) ( MTBE) (phenolphth
12、alein)(5.14) 1 mL . 0.1 mol/L (5.12) . 5.20 2-(2-bromopropionic acid; C 3 H 5 BrO 2 2,3-(2,3- dichloropropionic acid; C 3 H 4 Cl 2 O 2 )(9.4) 6 . , (polytetrafluoroethene)(PTFE) . 6.1 , 250 mL, 6.2 250 mL 6.3 10 mL, 25 mL, 50 mL, 100 mL 6.4 150 mL 6.5 6.6 . PTFE . 6.7 PTFE . 6.8 (microseparator) 6.9
13、 250 mL, 500 mL 6.10 ( 1 ) . 6.10.1 , 250 mL 6 KS I ISO 23631：2007 6.10.2 (equalizing) 100 mL 6.10.3 , Vigreux 6.10.4 (head) 6.10.5 , Liebig 6.10.6 100 mL 6.10.7 250 mL 6.10.8 250 mL, 1 (w10 %) 1 6.11 (ECD) , (6.13) . 2 1 . 7 KS I ISO 23631：2007 . , . , , . 6.12 (MS) , , (6.13) . 6.13 GC / , (PTV) (
14、on-column) 6.14 ( A ) 50 m . 6.15 0.751.5 m, . 6.16 pH 6.17 5 L 10 L . 7 KS M ISO 56671, KS M ISO 56672, KS M ISO 56673 . 250 mL (6.1) . . . 25 mg 5 (sodium thiosulfate pentahydrate)(5.13) . , 4 . (3 ). 8 8.1 8.1.1 (6.2) (20010) mL . (5.20) . (5.16) pH 1.00.2 . 8 KS I ISO 23631：2007 (5.10) 20 g . 8.
15、1.2 8.1.3 . 8.1.2 (microseparator) ：250 mL (6.1) , MTBE(5.7) 20 mL , (6.7) 5 10 1 000 min 1 , 5 . (microseparator) . (microseparator) (6.8) , (5.1) . 8.1.3 20 MTBE(5.7) 20 mL (6.9) . . , . 8.2 (8.1.2 8.1.3) 0.80.9 mL： (400 hPa, 30 ) . MTBE . ( 100200 L) (5.19) . 15 . 0.8 mL . (9.3) , MTBE(5.7) ( 1 m
16、L). 8.3 8.3.1 (GC-ECD) (ECD) , (RT) . ECD (5.17.3) RT()0.02 min , (necessary assignment certainty) . . , . . 9 KS I ISO 23631：2007 1) . . (GC-MS) . (ECD) 1 . ECD . , . (ECD) . ( 2 ) 2 . 8.3.2 (GC-MS) . (RT) (RT) 0.02 min ( ) ( 2 ) . . ( 2 ) . . SIM( ) , . , ( 2 ). 8.4 . (5.1) 200 mL . 1) , ( A ). 10
17、 KS I ISO 23631：2007 , . 2 () m/z (bromochloroacetic acid)( ) 127, 129, 131 a (dalapon)( ) 61, 97, 99 (dibromoacetic acid)( ) 171, 173, 175 (dichloroacetic acid)( ) 83, 85, 87 (monobromoacetic acid)( ) 93, 95, 121, 123 (monochloroacetic acid)( ) 77, 79, 108, 110 (TCA)(trichloroacetic acid)( ) 117, 119, 121 () 2-(2,2- dibromopropionic acid)( ) 87, 107, 109 2,3-(2,3- dichloropropionic acid) ( ) 97, 99, 121 9 9.1 , . . GC-MS ( .) 9.2 . 5 ( 1 ). . . 2 . . (5.17.3, 5.18.4 ). ( ) (9.3 ) ( ) (9.4 ) (RT)
