KS I ISO 22032-2007 Water quality-Determination of selected polybrominated diphenyl ethers in sediment and sewage sludge-Method using extraction and gas chromatography mass spectro.pdf

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1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 22032 / KS I ISO 22032 ：2007 (2012 ) 2007 12 7 http:/www.kats.go.krKS I ISO 22032：2007 : ( ) ( ) ( ) () ( ) () : (http:/www.standard.go.kr) ： ：2007 12 7 ：2012 12 27 20120787 ： ： (ISO/TC147) ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS I ISO 2

2、2032：2007 .1 1 1 2 2 3 2 4 2 5 3 6 5 7 .6 8 6 8.1 .6 8.2 .7 8.3 .7 8.4 7 8.5 .7 9 8 9.1 8 9.2 9 9.3 10 9.4 11 9.5 .11 9.6 12 10 .12 A() (clean-up) 13 B() 17 C() 19 D() 20 E() .25 26 i KS I ISO 22032：2007 (2012 ) / Water qualityDetermination of selected polybrominated diphenyl ethers in sediment and

3、sewage sludgeMethod using extraction and gas chromatography/mass spectrometry 2006 1 ISO 22032, Water qualityDetermination of selected polybrominated diphenyl ethers in sediment and sewage sludgeMethod using extraction and gas chromatography/mass spectrometry , . . . . . 1 (EI) (NCI) / (GCMS) (polyb

4、rominated diphenyl ethers)(PBDE)( 1 1 ) . GCEIMS 0.0525 g/kg (tetrabromo), (octabromo) 0.3100 g/kg (decabromo diphenyl ether)(BDE209) . 10 GCNCIMS . (misinterpretation) EI . , . KS I ISO 22032：2007 1 1 PBDE a g/mol 1 2,2,4,4 (2,2,4,4 Tetrabromodiphenyl ether) C 12 H 6 Br 4 O BDE47 485.795 0 2 2,2,4,

5、4,5 (2,2,4,4,5 pentabromodiphenyl ether) C 12 H 5 Br 5 O BDE99 564.691 1 3 2,2,4,4,6 (2,2,4,4,6 Pentabromodiphenyl ether) C 12 H 5 Br 5 O BDE100 564.691 1 4 2,2,4,4,5,6 2,2,4,4,5,6 Hexabromodiphenyl ether C 12 H 4 Br 6 O BDE154 643.587 2 5 2,2,4,4,5,5 (2,2,4,4,5,5 Hexabromodiphenyl ether) C 12 H 4 B

6、r 6 O BDE153 643.587 2 6 2,2,3,4,4,5,6 (2,2,3,4,4,5,6 Heptabromodiphenyl ether) C 12 H 3 Br 7 O BDE183 722.483 2 7 (Decabromodiphenyl ether) C 12 Br 10 O BDE209 959.171 4 aPCB IUPAC 2 . . ( ) . KS M ISO 566713, 13： KS M ISO 84661, (1 ) 3 . . , (EI) (NCI) . . 4 2 KS I ISO 22032：2007 GCNCIMS , 2,2,4,4

7、,5,5 (BB153) A(tetrabromobisphenol A) BDE154 BDE153 (coelute) m/z79 m/z81 , BDE . (halogenated bipyrrols) (brominated phenoxyanisols) . ： . , , (filler) . 5 . ( 18 ). 5.1 , . , (C 7 H 8 ) (, C 3 H 6 O), (, C 3 H 6 O) (C 6 H 14 ) (C 7 H 16 ), (2,2,4-trimethylpentane, C 8 H 18 ), (C 9 H 20 ), (CH 2 Cl

8、 2 ). 5.2 1 . 5.3 ( 2, 1 5 ) ( 2, 6, 7, 8 ) . 2 g/mol GCMS 1 2,2,4,4 13 C 12 (2,2,4,4 Tetrabromo 13 C 12 diphenyl ether) 13 C 12 H 6 Br 4 O 13 CBDE47 497.703 5 2 2,2,4,4,5 13 C 12 (2,2,4,4,5 Pentabromo 13 C 12 diphenyl ether) 13 C 12 H 5 Br 5 O 13 CBDE99 576.599 5 3 2,2,4,4,5,5 13 C 12 (2,2,4,4,5,5

9、Hexabromo 13 C 12 diphenyl ether) 13 C 12 H 4 Br 6 O 13 CBDE153 655.495 5 4 2,2,3,4,4,5,6 13 C 12 (2,2,3,4,4,5,6Heptabromo 13 C 12 diphenyl ether) 13 C 12 H 3 Br 7 O 13 CBDE183 734.391 6 5 13 C 12 (Decabromo 13 C 12 diphenyl ether) 13 C 12 Br 10 O 13 CBDE209 971.079 7 GCMS a3 KS I ISO 22032：2007 2 (

10、) g/mol 6 3,3,4,4 (3,3,4,4 Tetrabromodiphenyl ether) C 12 H 6 Br 4 O BDE 77 485.795 0 7 2,2,3,4,4,5,6 (2,2,3,4,4,5,6 Heptabromodiphenyl ether) C 12 H 3 Br 7 O BDE 181 722.483 2 8 13 C 12 (Decabromo 13 C 12 diphenyl ether) 13 C 12 Br 10 O 13 CBDE209 971.079 7 a PBDE . , BDE140 , BDE . 5.4 Na 2 SO 4 ,

11、 5.5 / . 5.6 , 99.999 % 5.7 / (, ), (5.2, 5.3) 10 mg 10 mL (5.1) 10 mL (： 1 mg/mL). 18 . 5.8 10 mL (5.7) 100500 L . , (5.1) 10 mL ( 1050 g/mL ). 5.9 7 . , (5.1) ( 5 ) (5.8) , (5.10), (5.12) . . . GCMS . . 5.10 (2,2,4-trimethylpentane) . 5 . 4 KS I ISO 22032：2007 5.11 (clean-up) A . 5.12 (dibromoocta

12、fluorobiphenyl)(C 12 Br 2 F 8 ) . 5.13 8 400 . 6 ()(5.1) . 400 . . 6.1 (wide-necked) 1 0005 000 mL 6.2 6.3 6.4 , (grinding mill) 6.5 , 100400 6.6 ( ) , 2 mm 6.7 6.8 (：250 mL), (thimbles)(：27 mm100 mm), (：300 mm) . 6.9 , , 6.10 6.11 250500 mL 5 KS I ISO 22032：2007 6.12 1 mL, 2 mL, 10 mL, 25 mL 6.13 ,

13、 2 mL 6.14 2 L, 5 L, 10 L, 50 L, 2 % 6.15 . 6.16 (：CH 4 ) (GCMS) (on-column) . 6.17 (low bleed) ( B ), 0.25 mm , 15 m 30 m( ), 0.1 m . 7 KS M ISO 566713 (6.1) . 4 . , . (6.4) (6.6) . 8 8.1 (510 g) (thimble) . (5.10) 1001 000 L (thimble) . (thimble) . 5.1 16 . , () , PDBE . , 16 . , (5.1) 100 mL . .

14、. . 16 . , (6.9) 6 KS I ISO 22032：2007 . (decabromo diphenyl ether)(C 12 Br 10 O) . BDE209 , PBDE . BDE209 . (keeper) . 8.2 . A . ( 9.3 9.5 ) 60 % . , A.1 A.2 . 8.3 , GCMS . B . GCMS . (5.12) GCMS . BDE209 300 BDE209 . BDE209 . 8.4 (baked sand)(5.13) (thimble) . PBDE PBDE . 8.5 . , ( 1 % 12 .) (quan

15、tification) (qualifier mass) 10 % 3 . 7 KS I ISO 22032：2007 3 BDE47 79 81 BDE99 79 81 BDE100 79 81 BDE154 79 81 BDE153 79 81 BDE183 79 81 BDE209 486.7 a484.7 BDE77 79 81 BDE181 79 81 13 CBDE209 494.7 496.7 a13 CBDE209 (fragment) 488.7 . ( 4 ) . (qualifier ion) (qualifier ion) . . . 4 BDE47 325.9 483

16、.7(69.5), 485.7(100) BDE99 405.7 563.6(100), 565.6(98) BDE100 405.7 563.6(100), 565.6(98) BDE153 485.7 641.5(100), 643.5(73.4) BDE154 485.7 641.5(100), 643.5(73.4) BDE183 563.6 721.4(100), 723.4(93.6) BDE209 799.3(100) 959.1(25), 797.3(81) 13 CBDE47 339.9 495.7(69.5), 497.7(100) 13 CBDE99 417.7 575.

17、6(100), 577.6(98) 13 CBDE153 497.7 653.5(100), 655.5(73.4) 13 CBDE209 811.3(100) 971.1(25), 809.3(81) . C . 9 9.1 8 KS I ISO 22032：2007 . . . 9.2 9.2.1 (5.9) 5 . (9.3 ) . , i y i / y is,i ( , ), i / is,i . KS M ISO 84661 . 5 1 2 3 4 5 6 7 ng/mL BDE47 5 12.5 25 50 100 150 250 BDE99 5 12.5 25 50 100 1

18、50 250 BDE100 5 12.5 25 50 100 150 250 BDE153 5 12.5 25 50 100 150 250 BDE154 5 12.5 25 50 100 150 250 BDE183 5 12.5 25 50 100 150 250 BDE209 25 50 100 200 500 700 1 000 NCI BDE77BDE47, BDE99, BDE100 100 100 100 100 100 100 100 BDE181BDE153, BDE154, BDE183 100 100 100 100 100 100 100 13 CBDE209 ( 13

19、 C 12 Br 10 O)BDE209 500 500 500 500 500 500 500 EI 13 CBDE47 200 200 200 200 200 200 200 13 CBDE99 200 200 200 200 200 200 200 13 CBDE153 200 200 200 200 200 200 200 13 CBDE183 400 400 400 400 400 400 400 13 CBDE209 500 500 500 500 500 500 500 9.2.2 2 2 (multi-injection) . 9.3 9 KS I ISO 22032：2007

20、 2 . (batch) GCMS . . 9.2.3 , 3 . i . 1 ) ( 1 2 N s N i i (1) s： . N ： . 9.2.4 ( , Eurachem Guide 1998 3 , ISO/TR 13530 4 , DIN 32645 2 ) . . 2 s 1/3 . 9.2.5 10 KS M ISO 84661 . 9.3 , . . . . (9.5 ) . PBDE 5 . . , 2 . 2 (multi-injection) , , ) 1 ( ) 1 ( , is i i y y , ) 2 ( ) 2 ( , is i i y y , ) 3 ( ) 3 ( , is i i y y . 10 KS I ISO 22032：2007 (2) 2 , i i y y , is i i , is . i i i i i i b a y y , is , is (2) y i： i , (： ) i： i ( ), ng/mL a i： i , (： , mL/ng). b i： y() , (： ). y is,i： i , (： ).