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1 w y wz 8«( 3y) 137~142, 2005 J. of the Korean Society for Environmental Analysis sw n w Polychlorinated Biphenyls»y Áwx Á yá w w yw Analysis of Polychlorinated Biphenyls from Pohang and Gangseo, Busan Area Gi Ho Jeong, Hye-Sook Ha, Eun-Hwa Lee, and Ji Yong Moon Department of Chemistry, Graduate School, Pusan National University, Busan , Korea PCBs levels in the sediment collected from Po-hang and Gang-seo in Busan were determined. Quantification was performed by using Agilent 6890 gas chromatography equipped with a 5973 series mass selective detector. We used BP-MS for the calibration standard, MBP-CG for a surrogate and perylene-d12 for an internal standard. The total PCBs levels ranged from 2.9 to 35 ng/g. The highest level was obtained from the site P2 located inside the breakwater. Total PCBs and TOC contents did not show any correlation. This may imply that total PCBs in the sediments from these two area are not dependent only on TOC. Key words : Polychlorinated biphenyls (PCBs), TOC, Sediment 1. sww» j ƒ ü w š. ü ü w w y,,,, w» j wyw f. ü 1) y y g ƒ» w w e» ƒ š. ü 2,3) wù PCBs(polychlorinated biphenyls) 19» Schmidt Schulz w w. 4) yƒ w w 70 PCBs ƒ wš k r. ù 1979 PCBs w š y ³ wš ù, y 5). PCBsƒ š w» ƒ š». PCBs 6) ƒ f m, y e m w š2) l ƒ w ƒ w. k - 7),, w w Áyw w. PCBs 8) w w» w, t š t. 9) m w PCBs PCBs dw k. 10) sw w y n, ù m PCBs d w. To whom correspondence should be addressed.

2 138»yÁwx Á yá n sw w n P1~P4, y n P5(Fig. 1) w 6 ù G1~G4(Fig. 2) (grab)» w t n (0~10 cm) w. sw w n P4 n š ƒ û. n ƒ š ƒ j e (silt). w n s p w k n Fig. 1. Sampling sites in Po-hang area. Fig. 2. Sampling sites in Gangseo-gu, Busan w w z 1 mm m g yww. Ÿ w yw» w þ w. y» 11,12) w w yw y ƒ yw» w œ» s jš headspace y g w. 13) 2.2. x»» wš, k m n-x 3z w» w. ƒ w»,» w z, w.» e w š, z œ»(buchi R-114) š» (99.999%) w. PCBs w w t 62 congener swwš yw t BP-MS(Wellington Lab, Canada) w. t BP-MS n-x w 1, 10, 20, 50, 100 ng/ml w. ü t MBP-CG(Wellington Lab, Canada) w š, ƒ ü t perylene-d12(aldrich, U.S.A) w. n-x (Merck, Germany)», m (Merck, Germany) w š, 130æ 9 k y ùp (Yakuri, 1 ) w. w w» w y (Matsunden Chemical Ltd.) w š, y w» w ˆ ( mesh, Aldrich) w. e (Wakogel S-1, Wako Pure Chemical Ltd.) 130 o C 9 y y g,» z w m š, v j ƒƒ 100 ml m n-x 4 w z, ³ y k m š, t MBP-CG w. m n- x ƒƒ 150 ml w 60æ 16 w. w» w y ù p m g 1 ml w z, y w n-x 50 ml ƒw 1 ml w. w» w 1 ml

3 sw n w Polychlorinated Biphenyls 139 1:1 y 1 ml w š, 1 w z, d ƒ w ¾ e k. d ƒ y d wš, y 1 ml x d ¾ w. x d, x d Áòw»š, y d û x 1 ml š z, d ƒ ù x d x d ww. y w» w w ˆ q w z, û wš m wš» g w. y w 2 g š 1, e ƒ ¾». óù vr ü Á òw»š ƒ ¾ w. e y ùp 1 g, e 2 g wš y ùp 1 g w. y e z w e f š, x 250 ml 1 g. z œ» w,» 1 ml w GC-MS w GC-MS w GC-MS(Agilent 6890 GC, 5973 MSD) w k w. w f HP-5MS(5% phenyl methyl siloxane, 30 m 0.25 mm I.D 0.25 µm) š, GC-MS Table 1 ùkü. ü t t ƒƒ ƒw w ü t» w yw» w (response factor, RF) w. A s A is RF = A s =t d v j A is = ü t d v j = t ü t (ng) C s = t t (ng) 9 w 3z d w Table 1. GC-MS operating parameters for PCBs analysis Carrier gas : He at 40 cm/s Injection mode : Splitless Purge time : 1.5 min Gas Injection volume : 2 µl Chromatography Injection port temp : 250 o C Oven Temp. program : 70 o C(2 min) Oven Temp. program : 30 o C/min o C Oven Temp. progra m : 5 o C/min o C(10 min) Ionization : electron ionization Mass Ion source temp. : 220 o C Selective Ionization energy : 70 ev Detector Detector mode : Selected Ion Monitoring(SIM) y wš w w. w y v jƒ Û5 ü ù kùš, y v j ƒ» Û20% w PCBs w. A s A is (ng) = RF A s = d v j A is = ü t d v j = ƒw ü t (ng) w l PCBs w. PCBs (ng/g) k( ng) = ˆn Gt ( g) 2.5.»k m,» n, s» w»k d w Walkley-Black y w n w PCBs» w 2). 1 g 250 ml ƒv j š, M j e 10 ml w y 30 ml ƒw 30 yww z, v j 30 e g þƒw. 85% 10 ml v y ùp 0.2 g ƒw z r ƒw 0.5 M Fe(II) w. k w w

4 140»yÁwx Á yá w»k r p w w. Walkley-Black y d»k y ƒ w»k (OXC) w»» k (TOC) y w. 14) ( B S) ( M of Fe %OXC 2+ ) = ( W 4000) TOC = 1.23 OXC B k Fe(II) v (ml) š S Fe(II) v(ml). W, 12/ g w k. 3. š 3.1. PCBs x z d w» w t m SRM 1939a w w x 3 z xw. SRM 1939a sw congener IUPAC No. 28, 52, 66, 153, 105, 187, 128, 156, 180, congener w z 75.0~130% x ƒ. Fig. 3 t w GC-MS w j m. t BP-MS 5, GC-MS w ƒ w 62 congener w. š congener s ³ RF, t r (SD), t r (RSD) wš, s ³ RF w w. sw (P1~P5) (G1~G4) w Table 2 ùkü. 9 w PCBs 2.9 ng/g(p5)~35 ng/g(p2) ù kû. sw sw Fig. 3. Total ion chromatogram for BP-MS standard (100 ppb). Table 2. Total PCBs concentrations of sediment Site Total Concentration (ng/g) RSD(%) P P P P P G G G G œ w š,. PCBs ƒ ƒ ùkù P2 Fig. 1 q Á yw w ù ùƒ wš n ƒ ùkù. P2 w PCBs P1 G4 8.5 ng/g, G3 6.7 ng/g, P3 G2 4.9 ng/g, P4 3.5 ng/g, G1 3.3 ng/g PCBs w. sw n PCBs x w w n PCBs 10) û ùkû, y PCBs w w» 1000 ng/g w { û. ù n w» š, m w PCBs 1996 m y œ Á w» 12 ppm,» 30 ppm w š. ƒ 4 w PCBs ƒ š,»k l» w w j. ù 5 y š PCBs w š w» 5 y š PCBsƒ w. Fig. 4 5 s r sw ey 4 7 sƒ ùkû. 3.2.» k PCBs w w

5 sw n w Polychlorinated Biphenyls 141 Table 3. Total organic carbons in the sediment from Pohang and Gangseo-gu, Busan Sites OXC Average(%) TOC STD Fig. 4. PCBs concentrations by homolog in the sediment from Po-hang. P P P P P G G G G w PCBs ƒ ƒ. 4. Fig. 5. PCBs concentrations by homolog in the sediment from Gangseou, Busan.» w, t, t ƒ PCBs»k (TOC) w w Ì d w. TOC w G3 0.87% ƒ û, G4 3.1% ƒ ùkûš, ù w s. sw n» sw n TOC w ùkù. PCBs TOC w ƒ ùkù, ƒ ùkûš, TOC w w Table 3 ùkü. PCBs» w k, œ», l w w,» w sw w ù n PCBs w. yw t BP-MS 62 congener w PCBs, homolog PCBs w. š n PCBs» w w» w y w»k d w. sw 5 4 PCBs w 2.9~35 ng/g ùkû. s w sw w š, PCBs ƒ ƒ ùkù P2 q Á œ ùkû. PCBs sw P2 w ù w s. e y s 4 y 7 y sƒ ùkû. PCBs» k (TOC) r, ùkû PCBs w. w 2 w,.

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