KS I ISO 9377-2-2006 Water quality-Determination of hydrocarbon oil index《水质 烃油指数 第2部分 使用溶剂提取和气相色谱法》.pdf

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1、 KSKSKSKS SKSKSKS KSKSKS SKSKS KSKS SKS KS 2006 9 29 http:/www.kats.go.krKS I ISO 93772 KS I ISO 9377 2: 2006 (2011 )I ISO 9377 2: 2006 : ( ) ( ) KIST ( ) : (http:/www.standard.go.kr) : :2001 12 26 :2006 9 29 :2011 12 26 2011-0622 : : ( 02- 509-7270) (http:/www.kats.go.kr). 10 5 , . ICS 13.060.50 KS

2、 I ISO 9377 2: 2006(2011 ) Water qualityDetermination of hydrocarbon oil index 2000 1 Water quality Determination of hydrocarbon oil index Part 2:Method using solvent extraction and gas chromatography . 1. . , , , 0.1 mg/L . . . 1. ISO/TR 11046 . 2. , 150 mg/L . 3. , . 2. . . . IEC ISO . KS M ISO 84

3、66 1: 2003 (1 ) ISO 5667 3: 1994 Water quality Sampling Part 3: Guidance on the preservation and handling of samples 3. . 3.1 GCFID 3669 , (1) , n (C10H22) n (C40H82) (1) . , ISO . , , , . I ISO 9377 2: 2006 2 4. (: ) . . 5. (extracting agent) . . (FID) (capillary chromatography) . n n . , . . , . 6

4、 . . 6.1 ( ) . 6.2 3669 . 6.3 6.4 6.5 : , c(HCl) 12 mol/L( 1.19 g/mL) 6.6 C3H6O 6.7 16 140 150250 m(60100 mesh) 6.8 6.8.1 (2) , ISO . ( A B) , 10 mg/mL (6.11.2) . A . . EN 590 . B A . , 325460 . (2) . Fachgruppe I.2 Bundesanstalt fr Materialforschung und-prfung Richard-Willsttter-Strasse 11 D-12489

5、 Berlin, Germany 6.8.2 (6.11.2) (6.8.1) , 5 . . 0( ), 0.2 mg/mL, 0.4 mg/mL, 0.6 mg/mL, 0.8 mg/mL, 1.0 mg/mL I ISO 9377 2: 2006 3 . (48 ) . 6 . 6.8.3 6.8.1 (6.6 ) 1 mg/mL . 1 000 . , 10 (6.2) . , (48 ) . 6 . 6.9 n ( ) n 50 g/mL (6.2) (C20, C40 n ) n . , . (6.2) . , (48 ) . 6 . 1. n . 2. n . 6.10 6.10

6、1 n C10H226.10.2 n C40H826.10.3 n C20H426.11 6.11.1 (6.2) n (6.10.2) 20 mg . n (6.10.1) 20 L 1 000 mL . , (4 8 ) . 6 . n . . 6.11.2 10 (6.11.1) . 6.12 , C36H72O2100 mL (6.11.2) (stearyl stearate) 200 mg . . (48 ) . 6 . 7. 7.1 ( ). (6.2) . 7.2 . 7.3 (fused silica) , 100 % DMPS(dimethylpolysiloxane),

7、 95 % /5 % (diphenylpoly-siloxane) (siloxane) I ISO 9377 2: 2006 4 : 530 m : 0.250.53 mm : 0.251.2 m B . ( , 2 m, 0.53 mm .) 7.4 , . 7.5 2501 000 mL , PTFE(polytetrafluoroethene) . . 7.6 7.7 100 mL . 7.8 ( ) A.2 7.9 (sinter porosity) 2 . A.1 7.10 Kuderna Danish 250 mL . (rotary evaporator) 7.11 . 8.

8、 ISO 5667 3 . (7.5) 90 % (m1). 4 . 4 . (6.5) pH 2 . . , pH . 150 , 250 mL . 9. 9.1 9.3 . 9.2 1.0 mL (6.8.3) 900 mL (6.1) . 9.3 . 80110 % . 9.3 10 . (6.5) pH 2 . 900 mL (6.4) 80 g . 1. . (6.11.2) 50 mL (7.11) 30 . I ISO 9377 2: 2006 5 (7.8) . (6.1) , (7.9) 9.4 . (organic phase) , . (7.8)( A.2 ) . , .

9、 100 mL (7.7) . . 2. 1015 . , . 9.4 2 g (6.7) 2 g (6.3) ( A.1 ) (extracting-agent phase)(9.3 ) . 1. (6.2) . 10 mL (6.2) (7.10) . 10 mL (6.2) . 2. , 30 2 g , (alternative) . 9.5 (7.10) 6 mL . 1 mL . (6.2) 1.0 mL , . (septum vial) . “ (large-volume injection system)” 1.0 mL . , ( 50, 100 mL) . , (6.8)

10、 n (6.9) . 5 . 1 g (m2) . 9.6 . (stearyl stearate)(6.12) (6.8) . 10 mL (9.4) , 25 mL (6.11.2) . , (9.7) . . 0.5 mL 25 mL (6.11.2) , . . 1 . 6.7 . 2 mg/mL (6.8) 10 mL (9.4) , (6.11.2) I ISO 9377 2: 2006 6 25 mL . . C10 C40 . 80 % . , 6.7 . . 9.7 9.7.1 (stationary phase)(7.3 B ) . . n (6.9) . n (C40H8

11、2) n (C20H42) 0.8 . , . 9.7.2 9.7.2.1 (initial calibration) , . KS M ISO 8466 1 , . . , (working range) (routine calibration) . , , , . . . ( ) , . 9.7.2.2 (6.8) . KS M ISO 8466 1 . 9.7.2.3 . . . 9.7.2.4 . 40 % 80 % . 10 % . , 9.7.2.3 . , . 9.7.3 , . . . . 9.7.4 n (C10H22) n (C40H82) . ( B.3 S) n ,

12、n ( B.3 E) . . S EI ISO 9377 2: 2006 7 . . B . n . . n . . n n . C . 9.8 . )()(21mmmawVfbA= (1) : a: Am: ( ) f: m1: (g) m2: (g) w: ( 1.00 g/mL ) V: b: y 9.9 , mg/L 2 . 15 mg/L 2.9 mg/L 10. , . a) b) c) d) , (qualitative) . e) (retention time) n f) g) I ISO 9377 2: 2006 8 11. 1999 1 . 1 No. L n NAP %

13、 x mg/L xsoil mg/L WFR % sR mg/L CVR % sr mg/L CVr % 1 35 127 15.3 3.04 2.99 101.6(1) 0.291 9.6 0.092 3.0 2 35 134 13.6 0.57 0.70 82.0(2) 0.192 33.5 0.037 6.5 3 38 142 10.1 3.61 4.00 90.3(2) 0.763 21.1 0.210 5.8 4 41 156 0.6 0.74 1.04 71.1(3) 0.300 40.5 0.105 14.1 L (outlier) n NAP x xsoll WFR sR CV

14、R sr CVr (1) . (2) 10 . (3) C12 . I ISO 9377 2: 2006 9 A() : mm 1 2 A.1 NS 14.5/231 221.82 50 150 91.5 I ISO 9377 2: 2006 10 : mm 1 , PTFE A.2 NS14/23 32 4NS19,PTFE 8 40 20 30 32 37 200 23 50 70 70 23 50 80 35 1 40 NS10/19NS14/23NS29/32I ISO 9377 2: 2006 11 B() . programmed temperature vaporization

15、PTV) 50300 1 L 30 m 0.25 mm DB 5 MS 0.25 m 0.8 bar 40 5 , 300 10 / , 300 20 300 25 mL I ISO 9377 2: 2006 12 1 n 2 n B.1 (0.5 mg/L) 0 5 10 15 20 25 30 35 40 45 50 55 60 (min) 514 512 510 508 506 504 502 500 E 2 S 1 I ISO 9377 2: 2006 13 1 n 2 n B.2 0 5 10 15 20 25 30 35 40 45 50 55 60 514 512 510 50

16、8 506 504 502 500 E 2 1 S (min) I ISO 9377 2: 2006 14 1 n 2 n B.3 0 5 10 15 20 25 30 35 40 45 50 55 60 514 512 510 508 506 504 502 500 E 2 S 1 (min) I ISO 9377 2: 2006 15 1 n 2 n B.4 (min) 0 5 10 15 20 25 30 35 40 45 50 55 60 514 512 510 508 506 504 502 500 E 2 S 1 I ISO 9377 2: 2006 16 C() C.1 2 44 n . n . C.1 n 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 89 42 0 36 69 98 126 151 174 196 216 235 253 271 287 302 317 331 344 356 369 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 380 391 402 412 422 432 441 450 459 468 476 483 491 498 505 512 51

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