KS I ISO 17858-2009 Water quality－Determination of dioxin-like polychlorinated biphenyls－Method using gas chromatography mass spectrometry《水质 测定类似二氧(杂)芑的多氯联苯 使用气相色谱 质谱测量法》.pdf

1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 17858 / KS I ISO 17858 :2009 2009 12 18 http:/www.kats.go.krKS I ISO 17858:2009 : ( ) ( ) ( ) : (ISO/TC147) () ( ) () () : (http:/www.standard.go.kr) ： ：2009 12 18 2009-0831 ： ：(ISO/TC147) ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 17

2、858:2009 / Water qualityDetermination of dioxin-like polychlorinated biphenyls Method using gas chromatography/mass spectrometry 2007 1 ISO 17858, Water qualityDetermination of dioxin-like polychlorinated biphenylsMethod using gas chromatography/mass spectrometry , . . . , . . non-ortho mono-ortho P

3、CBs co-planar , . PCBs . . . 1 / (HRGC/HRMS) (1 % ) - -(PCBs) . PCBs , (PCDDs/PCDFs) (PCNs) co-planar . ( , , , ) PCBs , . (World Health Organozation) 12 non- mono-ortho PCBs PCBS co-planar . . 2 (ML) PCBs . . , . KS I ISO 17858:2009 2 9.2 . 2 . . ( ) . KS I ISO 56671, 1： KS I ISO 56672, 2： KS M ISO

4、 3696, 3 , 3.1 . 3.1.1 (analyte) 1 3.1.2 (calibration standard) 2 / , 3.1.3 (calibration verification standard) VER 3.1.4 (certified reference material) CRM 3.1.5 (congener) , 209 PCBs 3.1.6 (critical pair) ( , 25 % valley) KS I ISO 17858:2009 3 3.1.7 (dioxin-like isomer) , PCB 3.1.8 (homologue grou

5、p) (tetrachlorobiphenyls) 3.1.9 (isotope dilution) , ( 13 C 12 ) 3.1.10 (keeper solvent) 3.1.11 (method blank) , , 3.1.12 (operational performance characteristics) , , , , , 3.1.13 (pattern) PCB 3.1.14 (profile) PCBs 3.1.15 (spiking) 13 C 12 PCB . 3.1.16 (statistical performance characteristics) 3.1

6、.17 (toxic equivalent factor) TEF 2,3,7,8-p-(TCDD)(2,3,7,8-tetrachlorodibenzo-p-dioxin) KS I ISO 17858:2009 4 3.1.18 (toxic equivalent quantity) TEQ 3.2 CRM GC/MS / GPC HPLC HRGC HRMS IPR LRMS MDL ML ( 2 ) PAR PCB (polychlorinated biphenyl) PCDD/PCDF -p-/ (polychlorinated dibenzo-p-dioxin/dibenzofur

7、an) PCN (polychlorinated naphthalene) PFK (perfluorokerosene) SIM SPE TEF TEQ VER 4 4.1 PCBs ( ) 1 L ( 1 % ) . 4.1 a), 4.1 b), 4.1 c) . , 1 % . a) 6.4 f) . . b) . 6.4 f) . . c) (SPE) . . . . KS I ISO 17858:2009 5 4.2 , . / , , , , 1) , . co-planar (HPLC) . , 2 GC PCB . 4.3 , . . GC . 2 . 10 000 . 10

8、 000 / 13 C 12 . (PCDD/Fs, PCBs, PCNs) 10 000 . 10 000 13 C 12 PCDFs PCBs PCDDs . (PCBs, PCNs) 10 000 . 4.4 PCB GC 2 . . 3 PCBs(：CB, CB 77) . 4.5 (SIM) . a) (4.1) PCBs , GC/MS . b) PCBs , GC/MS . 4.6 , , GC/MS . , , , (CRM), (SMS) . (QC) (CRM, SMS) . 1) (Florisil) . ISO . KS I ISO 17858:2009 6 5 5.1

9、 , , , / ( PCBs PCBs A ). . , , PCB118, PCB105 . 5.2 9.5.3 . a) c) . a) , . , . 30 . b) . , 6.4 f) . /. c) 20 . 6.4 f) / 2 , 6.4 f) 2 . . . . 5.3 (12 20 ) . 9.5, 15.5 5.4 . . . PCBs PCBs . -p-, , (diphenyl ethers), (methoxy biphenyls), (hydroxy- diphenyl), (benzyphenyl ethers), , , . PCBs . 13. 2 PC

10、Bs . 5.5 , (6.7) . 5.6 (, , ) KS I ISO 17858:2009 7 . . 6 , . 6.1 , KS M ISO 3696 3 . 6.2 pH 6.2.1 (KOH) 20 g 100 mL . 6.2.2 , H 2 SO 4 , 1.84 g/mL 6.2.3 1 mol/L (6.2.2) 56 mL (6.1) 1 L . 6.2.4 5 g 100 mL . 6.2.5 , Na 2 S 2 O 36.3 6.3.1 , Na 2 SO 4 , , 300 24 , . ( .) , . (g) 6.4 f) 20 mL 6.4 f) . 6

11、.3.2 , N 2 , 99.999 % 6.4 , . a) , C 3 H 6 O b) , C 7 H 8 c) , C 6 H 12 d) , C 6 H 14 e) , CH 3 OH KS I ISO 17858:2009 8 f) , CH 2 Cl 2 g) , C 4 H 10 O h) , C 2 H 6 O i) , C 9 H 20 6.5 GPC 300 mg/mL, (2-) (C 24 H 38 O 4 ) 15 mg/mL, (C 6 Cl 5 OH) 1.4 mg/mL, (C 20 H 12 ) 0.1 mg/mL, (S) 0.5 mg/mL 6.4 f

12、) . . . 6.6 6.6.1 , 70 m230 m 6.6.1.1 , 180 1 , . 2 . 6.6.1.2 , 30 % (6.2.2) 44.0 g 100 g . . . 22 % 44 % 100 g 20 g 80 g . 2 . 6.6.1.3 1 mol/L c(NAOH)1 mol/L 30 g 100 g . . . 2 . 6.6.1.4 , 36 % 6.4 e) 300 mL (6.2.1) 56 g 750 mL1 000 mL . (6.6.1) 100 g 60 70 1 2 . 100 mL , 6.4 f) 100 mL . 2 4 . 200

13、250 . . 2 . 6.6.2 6.6.2.1 , 9.4 . (9.2) . a) , 130 12 b) , 600 24 KS I ISO 17858:2009 9 6.6.2.2 650 700 (tube furnace) 400 mL/min . 700 . 130 . 5 . ICN Alumina Super I 2) . 6.6.3 6.6.3.1 , Carbopak C 3) (Supelco 1-0258 .) Celite 545 4) (Supelco 2-0199 .) Carbopak C 9.0 g Celite 545 41.0 g 18 % . 130

14、 6 . . 2 . Active carbon-impregnated silica 5) (Wako Pure Chemical Industries 019-11941) active carbon- disperded silica gel 6) (Kanto Chemical Co. 01875-43) . 6.6.3.2 , ：Amoco PX21 7)PX21 0.30 g (6.6.1.1) 5.7 g . 2 . 300 60 . . 6.6.4 , 70 m250 m 130 24 . . . . 6.6.5 / (Ag), (10 % ) (AgNO 3 ) (6.6.1

15、) . (AgNO 3 ) 10 g 40 mL 90 g . 30 . 70 2 70 125 . 125 10 . . . 2) ICN Alumina Super I . ISO . 3) Carbopak C . ISO . 4) Celite 545 . ISO . 5) Wako Pure Chemical Industries Active carbon-impregnated silica(019-11941) . ISO . 6) Kanto Chemical Company Active carbon-dispersed silica gel(01875-43) . ISO

16、 . 7) Amoco PX21 . ISO .KS I ISO 17858:2009 10 6.7 PCBs . , , , HPLC . 6.8 , / . . 98 % , . . . . (6.8 6.16) 2, 3 4 . (4.1 ). . . . 6.9 (PAR) PAR 4 PCBs . PAR (6.13) . . (6.12) (6.10) . 6.10 4 PCBs . 6.4 a) . 1.0 mL , 1 . 6.11 4 13 C 12 - . 6.12 6.9 6.11 3 5 . KS I ISO 17858:2009 11 ( ) . 5 . 3 10 . (VER) . 6.13 . (6.9) 6.4 a) 2.0 mL . . 6.14 GC PCBs GC