KS I ISO 18073-2010 Water quality－Determination of tetra- to octa-chlorinated dioxins and furans－Method using isotope dilution HRGC HRMS《水质 三氯至八氯二氧杂环乙烯和呋喃的测定 同位素稀释HRGC HRMS法》.pdf

1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 180734- 8- HRGC/HRMS KS I ISO 18073 :2010 2010 8 31 http:/www.kats.go.krKS I ISO 18073:2010 : ( ) ( ) ( ) ( ) : (http:/www.standard.go.kr) ： ：2005 12 14 ：2010 8 31 2010-0347 ： ： ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 18073:2010 i

2、.1 1 1 2 1 3 .2 4 4 5 6 6 8 7 .14 8 , , , .19 9 /.19 10 22 11 30 12 .31 13 35 14 HRGC/HRMS 38 15 (laboratory performance).39 16 (qualitative determination) .40 17 (quantitative determination) .40 18 44 19 .44 A() HRGC/HRMS 46 B() .51 C() .54 D() 55 59 KS I ISO 18073:2010 4- 8- HRGC/HRMS Water qualit

3、yDetermination of tetra- to octa-chlorinated dioxins and furansMethod using isotope dilution HRGC/HRMS 2004 1 ISO 18073, Water qualityDetermination of tetra- to octa- chlorinated dioxins and furansMethod using isotope dilution HRGC/HRMS , . . . . . 2,3,7,8 PCDDs/PCDFs . PCDDs/PCDFs . . 1 ( 1 % ) 4 8

4、 p(PCDDs) (PCDFs) / (HRGC/HRMS) . 1 17 2,3,7,8 PCDDs/PCDFs . . 2 (MLs) PCDDs/PCDFs . 2,3,7,8TCDD (MDL) 1 L 4.4 pg/L . . “ (peformance based)”. . 2 . KS I ISO 18073:2010 2 . ( ) . KS I 2003(ISO 6879), KS I ISO 56671, ( ) KS I ISO 56672, 2： KS M ISO 3696, 3 3.1 , KS I 2003(ISO 6879) . 3.1.1 PCDD PCDF

5、1 . 3.1.2 . . 3.1.3 3.1.4 congener 210 PCDDs/PCDFs 3.1.5 PCDDs PCDFs 13 C 12 (labelled) 2,3,7,8PCDD/ PCDF 3.1.6 (keeper) 3.1.7 , , , 3.1.8 (operational peformance characteristics) , KS I ISO 18073:2010 3 , , , , KS I 2003(ISO 6879) 3.1.9 PCDD/PCDF 3.1.10 PCDD/PCDF PCDDs/PCDFs 3.1.11 (profile) PCDDs

6、PCDFs 3.1.12 (recovery standard) GC 13 C 12 2,3,7,8 PCDD/PCDF 3.1.13 (spiking) 13 C 12 PCDD/PCDF . 3.1.14 KS I 2003(ISO 6879) 3.2 DCDPE GC/MS / GPC HpCDD p HpCDF HpCDPE HPLC HRGC HRMS HxCDD p HxCDF HxCDPE MDL ML ( 2 ) NCDPE OCDD p OCDF KS I ISO 18073:2010 4 OCDPE PCDD/PCDF p/ PeCDD p PeCDF PTFE SIM

7、TCDD p TCDF TEF (toxic equivalent factor) TEQ (toxic equivalent) 4 4.1 ( 2,3,7,8 PCDDs/PCDFs ) 1 % 1 L . . 4.1 a) 4.1 b) . a) . . . b) . (soxhlet) , . . . 4.2 . , , , , 1) (Florisil) . 4.3 . , . GC , . . 10 000 . 13 C 12 10 000 / . 6 000 10 000 . PCDD/PCDF 10 000 . 10 000 13 C 12 PCDFs PCDDs . 1) Fl

8、orisil . , ISO . KS I ISO 18073:2010 5 1 PCDDs PCDFs PDDDs/PCDFs CAS CAS 2,3,7,8TCDD 1746016 13 C 12 2,3,7,8TCDD 13 C 12 1,2,3,4TCDD 76523405 Total TCDD 41903575 2,3,7,8TCDF 51207319 13 C 12 2,3,7,8TCDF 89059461 Total TCDF 55722275 1,2,3,7,8PeCDD 40321764 13 C 12 1,2,3,7,8PeCDD 109719791 Total PeCDD

9、 36088229 1,2,3,7,8PeCDF 57117416 13 C 12 1,2,3,7,8PeCDF 109719779 2,3,4,7,8PeCDF 57117314 13 C 12 2,3,4,7,8PeCDF 116843028 Total PeCDF 30402154 1,2,3,4,7,8HxCDD 39227286 13 C 12 1,2,3,4,7,8HxCDD 109719804 1,2,3,6,7,8HxCDD 57653857 13 C 12 1,2,3,6,7,8HxCDD 109719815 1,2,3,7,8,9HxCDD 19408743 13 C 12

10、 1,2,3,7,8,9HxCDD 109719826 Total HxCDD 34465468 1,2,3,4,7,8HxCDF 70648269 13 C 12 1,2,3,4,7,8HxCDF 114423982 1,2,3,6,7,8HxCDF 57117449 13 C 12 1,2,3,6,7,8HxCDF 116843039 1,2,3,7,8,9HxCDF 72918219 13 C 12 1,2,3,7,8,9HxCDF 116843040 2,3,4,6,7,8HxCDF 60851345 13 C 12 2,3,4,6,7,8HxCDF 116843051 Total H

11、xCDF 55684941 1,2,3,4,6,7,8HpCDD 35822469 13 C 12 1,2,3,4,6,7,8HpCDD 109719837 Total HpCDD 37871004 1,2,3,4,6,7,8HpCDF 67562394 13 C 12 1,2,3,4,6,7,8HpCDF 109719848 1,2,3,4,7,8,9HpCDF 55673897 13 C 12 1,2,3,4,7,8,9HpCDF 109719940 Total HpCDF 38998753 OCDD 3268879 13 C 12 OCDD 114423971 OCDF 39001020

12、 13 C 12 OCDF 109719780 4.4 PCDD/PCDF GC (abundance) . 2,3,7,8 congener . 4.5 3 (SIM) . a) (labelled) 2,3,7,8 PCDDs/PCDFs , GC/MS . b) 2,3,7,8 PCDDs/PCDFs , GC/MS . KS I ISO 18073:2010 6 c) 2,3,7,8 PCDDs/PCDFs . 4.6 , , GC/MS . 5 5.1 , , , . . 5.2 (9.4.3) . 5.2 a) c) . a) , . , . 30 . b) , . c) 3 .

13、(80/20 ) 2 , 2 . . . 5.3 (12 20 ) (reference-matrix method blank) . 5.4 (reference matrix) . PCDDs/PCDFs . . KS I ISO 18073:2010 7 2 PCDDs/PCDFs PCDDs/PCDFs a abpg/L abpg/ L 2,3,7,8TCDF 13 C 12 2,3,7,8TCDF 0.9991.003 10 0.5 2,3,7,8TCDD 13 C 12 2,3,7,8TCDD 0.9991.002 10 0.5 1,2,3,7,8PeCDF 13 C 12 1,2

14、,3,7,8PeCDF 0.9991.002 50 2.5 2,3,4,7,8PeCDF 13 C 12 2,3,4,7,8PeCDF 0.9991.002 50 2.5 1,2,3,7,8PeCDD 13 C 12 1,2,3,7,8PeCDD 0.9991.002 50 2.5 13 C 12 2,3,7,8TCDF 13 C 12 1,2,3,4TCDD 0.9231.103 50 2.5 13 C 12 2,3,7,8TCDD 13 C 12 1,2,3,4TCDD 0.9761.043 50 2.5 13 C 12 1,2,3,7,8PeCDF 13 C 12 1,2,3,4TCDD

15、 1.0001.425 50 2.5 13 C 12 2,3,4,7,8PeCDF 13 C 12 1,2,3,4TCDD 1.0111.526 50 2.5 13 C 12 1,2,3,7,8PeCDD 13 C 12 1,2,3,4TCDD 1.0001.567 50 2.5 1,2,3,4,7,8HxCDF 13 C 12 1,2,3,4,7,8HxCDF 0.9991.001 50 2.5 1,2,3,6,7,8HxCDF 13 C 12 1,2,3,6,7,8HxCDF 0.9971.005 50 2.5 1,2,3,7,8,9HxCDF 13 C 12 1,2,3,7,8,9HxC

16、DF 0.9991.001 50 2.5 2,3,4,6,7,8HxCDF 13 C 12 2,3,4,6,7,8HxCDF 0.9991.001 50 2.5 1,2,3,4,7,8HxCDD 13 C 12 1,2,3,4,7,8HxCDD 0.9991.001 50 2.5 1,2,3,6,7,8HxCDD 13 C 12 1,2,3,6,7,8HxCDD 0.9981.004 50 2.5 1,2,3,7,8,9HxCDD c1.0001.019 50 2.5 1,2,3,4,6,7,8HpCDF 13 C 12 1,2,3,4,6,7,8HpCDF 0.9991.001 50 2.5

17、 1,2,3,4,7,8,9HpCDF 13 C 12 1,2,3,4,7,8,9HpCDF 0.9991.001 50 2.5 1,2,3,4,6,7,8HpCDD 13 C 12 1,2,3,4,6,7,8HpCDD 0.9991.001 50 2.5 OCDD 13 C 12 OCDD 0.9991.001 100 5.0 OCDF 13 C 12 OCDD 0.9991.008 100 5.0 13 C 12 1,2,3,4,7,8HxCDF 13 C 12 1,2,3,7,8,9HxCDD 0.9440.970 13 C 12 1,2,3,6,7,8HxCDF 13 C 12 1,2

18、,3,7,8,9HxCDD 0.9490.975 13 C 12 1,2,3,7,8,9HxCDF 13 C 12 1,2,3,7,8,9HxCDD 0.9771.047 13 C 12 2,3,4,6,7,8HxCDF 13 C 12 1,2,3,7,8,9HxCDD 0.9591.021 13 C 12 1,2,3,4,7,8HxCDD 13 C 12 1,2,3,7,8,9HxCDD 0.9771.000 13 C 12 1,2,3,6,7,8HxCDD 13 C 12 1,2,3,7,8,9HxCDD 0.9811.003 13 C 12 1,2,3,4,6,7,8HpCDF 13 C

19、 12 1,2,3,7,8,9HxCDD 1.0431.085 13 C 12 1,2,3,4,7,8,9HpCDF 13 C 12 1,2,3,7,8,9HxCDD 1.0571.151 13 C 12 1,2,3,4,6,7,8HpCDD 13 C 12 1,2,3,7,8,9HxCDD 1.0861.110 13 C 12 OCDD 13 C 12 1,2,3,7,8,9HxCDD 1.0321.311 a . b (ML) . , , 1 L , . c1,2,3,7,8,9HxCDD 13 C 12 1,2,3,6,7,8HxCDD. 1,2,3,7,8,9HxCDD 13 C 12

20、 1,2,3,4,7,8HxCDD 13 C 12 1,2,3,6,7,8HxCDD . . PCDDs/PCDFs . , , , KS I ISO 18073:2010 8 , , . PCDDs/PCDFs , . 13. , 2 PCDDs/PCDFs . 5.5 , (6.1) . 5.6 . , , . 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 , c(HCl)6 mol/L 6.2.4 , , NaCl, 5 g 100 mL

21、 . 6.3 6.3.1 , Na 2 SO 4 , , , (20 mL/g) , 1 400 . ( ), . , . 6.3.2 , N 299.999 % 6.4 . a) Acetone, C 3 H 6 O b) Toluene, C 7 H 8 c) Cyclohexane, C 6 H 12 d) Hexane, C 6 H 14 e) Methanol, CH 3 OH KS I ISO 18073:2010 9 f) Dichloromethane, CH 2 Cl 2 g) Nonane, C 9 H 206.5 GPC 300 mg/mL , 15 mg/mL (2)

22、C 24 H 38 O 4 , 1.4 mg/mL C 6 Cl 5 OH, 0.1 mg/mL C 20 H 12 , 0.5 mg/mL S 6.6 6.6.1 6.6.1.1 (75 140 ) m , 1 180 . 6.6.1.2 30 % 44.0 g (6.2.2) 100 g . . . 6.6.1.3 30 g c(NaOH)1 mol/L 100 g . . . 6.6.1.4 56 g (KOH) 7501 000 mL 300 mL . 100 g (stirring bar) , (hotplate) (1 2 ) (60 70 ) . 100 mL , 100 mL

23、 . , (2 4 ) . (200 250 ) . 6.6.2 9.3 . . (9.2) . a) 12 130 . b) 24 600 . 130 . 5 . KS I ISO 18073:2010 10 ICN Alumina Super I 2) . 6.6.3 9.0 g Carbopak C 3) (Supelco 10258 ) 41.0 g Celite 545 4) (Supelco 20199 ) . 6 130 . . 5) (Wako Pure Chemical Industries 01911941) 6)(Kanto Chemical Co. 0187543) . 6.6.4 (Florisil) 1), (150 250 ) m, 24 500 g (7.5.2) . 1.5 g( 2 mL) , 1 mL (6.3.1) . 24 (130 150 ) , 30 . 90 . 6.7 (reference matrices) PCDDs/PCDFs . , (6.1) . 6.8 , , . . (6.96.15) 2, 3, 4, 5 . (spiking) (4.1 ). 98 % , . 2) ICN Alumina Super I . , ISO . 3) Carbopak C .