KS I 3226-2009 Method for determination of tetra-through octa-chlorodibenzo-p-dioxins tetra-though octa-chlorodibenzofurans and coplanar polychlorobiphenyls in industrial water and.pdf

1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I 3226 (PCDDs/PCDFs co-PCBs) KS I 3226 :2009 2009 12 18 http:/www.kats.go.krKS I 3226:2009 : ( ) ( ) () ( ) : (ISO/TC147) ( ) () () KS I 3226:2009 : (http:/www.standard.go.kr) ： ：2004 9 30 ：2009 12 18 2009-0830 ： ： (ISO/TC147) ( 02-509-7266) (http:/www.k

2、ats.go.kr). 10 5 , . KS I 3226:2009 (PCDDs/PCDFs co-PCBs) Method for determination of tetra-through octa-chlorodibenzo-p-dioxins, tetra-though octa-chlorodibenzofurans and coplanar polychlorobiphenyls in industrial water and wastewater 1 ( GC/MS .) -p- - PCB( .) . GC/MS (GC) , 10 000 (MS) . , , 0.1

3、pg, 0.2 pg, 0.5 pg, PCB 0.2 pg . 2 . . ( ) . KS I 2202, KS I 3002, KS L 2301, KS L 2302, KS L 2303, KS L 2316, KS M 0027, KS M 0108, KS M 0124, ( ) KS M 0126, ( ) KS M 1030, KS M 1031, KS M 1125, KS M 8356, - KS M 8446, 2,2,4-() KS M 8450, - KS M 8458, () KS M 8510, ( PCB ) () KS I 3226:2009 2 KS M

4、8511, (99.5)( PCB )() KS M 8513, ( ) () KS M 8530, ( PCB ) () KS Q 5002, 1： 3 KS M 0108, KS M 0027, KS M 0126 KS M 0124 . 3.1 Polychloro-dibenzo-p-dioxins Polychloro-dibenzofurans PCB . 3.2 , . 3.3 , . 3.4 PCDDs Polychloro dibenzo-p-dioxins 3.5 PCDFs Polychloro dibenzofurans 3.6 TeCDDs Tetrachloro d

5、ibenzo-p-dioxins 3.7 PeCDDs Pentachloro dibenzo-p-dioxins 3.8 HxCDDs Hexachloro dibenzo-p-dioxins 3.9 HpCDDs Heptachloro dibenzo-p-dioxins 3.10 OCDD Octachloro dibenzo-p-dioxin KS I 3226:2009 3 3.11 TeCDFs Tetrachloro dibenzofurans 3.12 PeCDFs Pentachloro dibenzofurans 3.13 HxCDFs Hexachloro dibenzo

6、furans 3.14 HpCDFs Heptachloro dibenzofurans 3.15 OCDF Octachloro dibenzofuran 3.16 2,3,7,8- 2,3,7,8- TeCDD OCDD 7 TeCDF OCDF 9 16, . a) TeCDDOCDD(PCDDs) 2,3,7,8-Tetrachloro-dibenzo-p-dioxin(2,3,7,8-TeCDD) 1,2,3,7,8-Pentachloro-dibenzo-p-dioxin(2,3,7,8-PeCDD) 1,2,3,4,7,8-Hexachloro-dibenzo-p-dioxin(

7、1,2,3,4,7,8-HxCDD) 1,2,3,6,7,8-Hexachloro-dibenzo-p-dioxin(1,2,3,6,7,8-HxCDD) 1,2,3,7,8,9-Hexachloro-dibenzo-p-dioxin(1,2,3,7,8,9-HxCDD) 1,2,3,4,6,7,8-Heptachloro-dibenzo-p-dioxin(1,2,3,4,6,7,8-HpCDD) Octa chloro-dibenzo-p-dioxin(OCDD) b) TeCDFOCDF(PCDFs) 2,3,7,8-Tetra chloro-dibenzofuran(2,3,7,8-Te

8、CDF) 1,2,3,7,8-Penta chloro-dibenzofuran(1,2,3,7,8-PeCDF) 2,3,4,7,8-Penta chloro-dibenzofuran(2,3,4,7,8-PeCDF) 1,2,3,4,7,8-Hexa chloro-dibenzofuran(1,2,3,4,7,8-HxCDF) 1,2,3,6,7,8-Hexa chloro-dibenzofuran(1,2,3,6,7,8-HxCDF) 1,2,3,7,8,9-Hexa chloro-dibenzofuran(1,2,3,7,8,9-HxCDF) 2,3,4,6,7,8-Hexa chlo

9、ro-dibenzofuran(2,3,4,6,7,8-HxCDF) 1,2,3,4,6,7,8-Hepta chloro-dibenzofuran(1,2,3,4,6,7,8-HpCDF) Octa chloro-dibenzofuran(OCDF) 3.17 PCBs Polychlorobiphenyl 3.18 TeCBs Tetrachlorobiphenyl KS I 3226:2009 4 3.19 PeCBs Pentachlorobiphenyl 3.20 HxCBs Hexachlorobiphenyl 3.21 HpCBs Heptachlorobiphenyl 3.22

10、 PCB (DL-PCB) Polychloro biphenyl ortho (2,2 ,6 6 ) (non-ortho), ortho 1 (mono-ortho) . Coplanar-PCB . a) non-ortho 3,4,4 ,5-Tetrachlorobiphenyl3,4,4 ,5-TeCB(IUPAC No.81) 3,3 ,4,4 -Tetrachlorobiphenyl3,3 ,4,4 -TeCB(IUPAC No.77) 3,3 ,4,4 ,5-Pentachlorobiphenyl3,3 ,4,4 ,5-PeCB(IUPAC No.126) 3,3 ,4,4 ,

11、5,5 -Hexachlorobiphenyl3,3 ,4,4 ,5,5 -HxCB(IUPAC No.169) IUPAC：International Union of Pure and Applied Chemistry b) mono-ortho 2,3,3 ,4,4 -Pentachlorobiphenyl2,3,3 ,4,4 -PeCB(IUPAC No.105) 2,3,4,4 ,5-Pentachlorobiphenyl2,3,4,4 ,5-PeCB(IUPAC No.114) 2,3 ,4,4 ,5-Pentachlorobiphenyl2,3 ,4,4 ,5-PeCB(IUP

12、AC No.118) 2 ,3,4,4 ,5-Pentachlorobiphenyl2 ,3,4,4 ,5-PeCB(IUPAC No.123) 2,3,3 ,4,4 ,5-Hexachlorobiphenyl2,3,3 ,4,4 ,5-HxCB(IUPAC No.156) 2,3,3 ,4,4 ,5 -Hexachlorobiphenyl2,3,3 ,4,4 ,5 -HxCB(IUPAC No.157) 2,3 ,4,4 ,5,5 -Hexachlorobiphenyl2,3 ,4,4 ,5,5 -HxCB(IUPAC No.167) 2,3,3 ,4,4 ,5,5 -Heptachloro

13、biphenyl2,3,3 ,4,4 ,5,5 -HpCB(IUPAC No.189) 3.23 3.24 3.25 3.26 KS I 3226:2009 5 3.27 , , , 3 . 3.28 3.29 TEF 2,3,7,8-TeCDD (2,3,7,8-TeCDD toxicity equivalent factor) 3.30 TEQ 2,3,7,8-TeCDD (2,3,7,8-TeCDD toxic equivalents) 3.31 RRF (Relative response factor) 4 , GC/MS , . A . , , , . , . KS I 3226:

14、2009 6 1 5 5.1 , KS M 0108 . , GC , (R) 10 000 , SIM Calibration S/N , , GC/MS (CS) ( ) GC/MS ( ) , KS I 3226:2009 7 5.2 . , KS M 0108 . 5.2.1 . a) , ( ) ( ) . . , . . b) . 5.2.2 KS M 0108 . 5.2.3 KS M 0108 . , . 1 mg/L ( ) 7.0 mg/L . ( A ). 5.2.4 . a) . b) a) 1/30 . c) . DL E E DL 1 C V V x y Q V V

15、 ： (L) Q DL ： (pg) y ： ( L) x ：GC/MS ( L) V E ：(mL) V E ： (mL) C DL ： (pg/L) d) . 5.3 . KS I 3226:2009 8 a) b) c) d) e) f) ( . , ) g) h) , i) ( , ), , pH, . , . 5.4 , . , 0 10 . 6 6.1 ( ) , . - 1) , , . . . 1 . 2 . . 5 5 25 . a) 90 % . b) GC/MS 7.3.1 a) 50450 . c) 7.3.3 . 1) - .KS I 3226:2009 9 1 -

16、, , , , , , , , , , , PCDDs PCDFs, PCB PCDDs PCDFs, PCB (DMSO) 2 6.2 . . a) KS I 3002 A4( A3) b) , . c) KS M 8510 , . d) , . e) KS M 8513 , . , ( ) ( ) KS I 3226:2009 10 f) KS M 8530 , . g) , . h) KS M 1031 , . i) KS M 1030 , . j) 2,2,4- , . k) , . l) KS M 8356 , . m) KS M 8450 , . n) , . o) , . p)

17、a) f) . q) 13 C 37 Cl , . 2 . 1) , , . 2) GC/MS , . . r) 0.063 mm0.200 mm( 63 m212 m) , . 10 mm , 130 18 , 30 . , , . s) 2 %() KOH r) 100 g KOH (50 g/L) 40 mL , 50 , 50 80 1 . , . t) 22 %() r) 100 g m) 28.2 g , . , . u) 44 %() r) 100 g m) 78.6 g , . , . v) 10 %() r) 100 g (400 g/L) 28 mL , . . , . w

18、) (, 1) . , 10 mm 130 18 , 5 mm 500 8 , 30 , . . x) (graphite carbon) . Hypersil Hypercarb( 4.6 mm, 100 mm) . y) . , , . z) 0.5 m . . aa) (ODS) KS I 3226:2009 11 . ab) KS M 1125 2 2 13 C 12 -1,2,3,4-TeCDD13 C 12 -2,3,7,8-TeCDD 37 C1 4 -2,3,7,8-TeCDD 13 C 12 -1,2,3,7,8-PeCDD13 C 12 -1,2,3,4,7,8-HxCDD

19、13 C 12 -1,2,3,6,7,8-HxCDD 13 C 12 -1,2,3,7,8,9-HxCDD 13 C 12 -1,2,3,4,6,7,8-HpCDDPCDD 13 C 12 -1,2,3,4,6,7,8,9-OCDD13 C 12 -2,3,7,8-TeCDF 13 C 12 -1,2,7,8-TeCDF 13 C 12 -1,2,3,7,8-PeCDF 13 C 12 -2,3,4,7,8-PeCDF 13 C 12 -1,2,3,4,7,8-HxCDF 13 C 12 -1,2,3,6,7,8-HxCDF 13 C 12 -1,2,3,7,8,9-HxCDF 13 C 12

20、 -2,3,4,6,7,8-HxCDF 13 C 12 -1,2,3,4,6,7,8-HpCDF 13 C 12 -1,2,3,4,7,8,9-HpCDF PCDF 13 C 12 -1,2,3,4,6,7,8,9-OCDF 13 C 12 -2,3 ,4 ,5-TeCB(#70)13 C 12 -3,3 ,4,4 -TeCB(#77)* 13 C 12 -3,4,4 ,5-TeCB(#81)* 13 C 12 -2,3,3 ,4,4 -PeCB(#105)* 13 C 12 -2,3,4,4 ,5-PeCB(#114)* 13 C 12 -2,3 ,4,4 ,5-PeCB(#118)* 13

21、 C 12 -2 ,3,4,4 ,5-PeCB(#123)* 13 C 12 -3,3 ,4,4 ,5-PeCB(#126)* 13 C 12 -2,3,3 ,4,4 ,5-HxCB(#156)* 13 C 12 -2,3,3 ,4,4 ,5 -HxCB(#157)* 13 C 12 -2,3 ,4,4 ,5,5 -HxCB(#167)* 13 C 12 -3,3 ,4,4 ,5,5 -HxCB(#169)* 13 C 12 -2,2 ,3,3 ,4,4 ,5-HpCB(#170) 13 C 12 -2,2 ,3,4,4 ,5,5 -HpCB(#180) PCB* 13 C 12 -2,3,3

22、 ,4,4 ,5,5 -HpCB(#189)* * IUPAC No. . * DL-PCB . KS I 3226:2009 12 6.3 (, ) (, ) , . a) KS L 2302 KS L 2303 . . b) , , , , , , , , . 3 . c) KS L 2303 . d) , . e) 10 mm, 300 mm( 15 mm, 300 mm) , f) g) 3 () 6.4 6.4.1 . , , . 6.4.2 ( ) KS I 3226:2009 13 , 2) . 0.1 ng2 ng, 0.2 ng4 ng, DL-PCB 0.1 ng2 ng. , . . 6.4.3 , , . a) ( 0.5 m) 3) . . b) . 1) , , . 4)