KS I ISO 15009-2009 Soil quality-Gas chromatographic determination of the content of volatile aromatic hydrocarbons naphthalene and volatile halogenated hydrocarbons-Purge-and-trap.pdf

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1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 15009 , , KS I ISO 15009 :2009 2009 12 18 http:/www.kats.go.krKS I ISO 15009:2009 : ( ) ( ) ( ) :(ISO/TC190) () ( ) () : (http:/www.standard.go.kr) : :2004 9 30 :2009 12 18 2009-0830 : : (ISO/TC190) ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . K

2、S I ISO 15009:2009 , , Soil qualityGas chromatographic determination of the content of volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbonsPurge-and-trap method with thermal desorption 2002 1 ISO 15009, Soil qualityGas chromatographic determination of the content of vola

3、tile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons Purge-and-trap method with thermal desorption , . 1 , , . . ( ). :0.1 mg/kg :0.01 mg/kg . 2 . . ( ) . KS I ISO 103811, 1: KS I ISO 103812, 2: KS I ISO 11465, () KS L ISO 4799, - KS I ISO 15009:2009 2 3 . . , . . . . (FID)

4、. (ECD) . . (effluent splitter) . , ( ) . . . . . () . 4 . . 4.1 , 80 . 10 mL/min 30 . . 4.2 4.2.1 . . -D8(Toluene-D8)(CAS No. 2037265) -D10(Ethylbenzene-D10)(CAS No. 25837052) 4.2.2 . KS I ISO 15009:2009 3 . 1,4-(1.4-dichlorobutane)(CAS No. 110565) , , -( , , -trifluorotoluene)(CAN No. 98088) 2-(2-

5、bromofluorobenzene)(CAS No. 1072851) 4.3 CAS No. (benzene) 71432 (toluene) 108883 (ethylbenzene) 100414 o-(o-xylene) 95476 m-(m-xylene) 108383 p-(p-xylene) 106423 (stylene) 100425 (naphthalene) 91203 4.4 CAS No. (dichloromethane) 75092 (trichloromethane) 67663 (tetrachloromethane) 56235 1,1-(1,1-dic

6、hloromethane) 75343 1,2-(1,2-dichloromethane) 107062 1,1,1-(1,1,1-trichloroethane) 79016 1,1,2-(1,1,2-trichloroethane) 79005 1,2-(1,2-dichloropropane) 78875 1,2,3-(1,2,3-trichloropropane) 98184 cis-1,3-(cis-1,3-dichloropropane) 10061015 trans-1,3-(trans-1,3-dichloropropane) 10061026 cis-1,2-(cis-1,2

7、-dichloroethane) 156592 trans-1,2-(trans-1,2-dichloroethane) 156605 3-(3-chloropropene) 107051 (trichloroethene) 79016 (tetrachloroethene) 127184 (monochlorobenzene) 108907 1,2-(1,2-dichlorobenzene) 95501 4.5 (CAS No. 67561) 100 g/L 10 g/L . 4.6 KS I ISO 15009:2009 4 2,6-diphenyl-p-phenoxide 1) (406

8、0 mesh) . . 4.7 (6.1) . 10 . . 4.8 4.9 5 5.1 4 g/L (4.3 4.4) 100 mg 0.1 mg 25 mL (septum flask) . . 5.2 4 g/L (4.2.1 4.2.2) 100 mg 0.1 mg 25 mL . . 5.3 0200 mg/L (5.1) 200 mg/L (5.2) . 5.1 5.2 1 (4.5) 100 mL . 1) Tenax TA . KS . KS I ISO 15009:2009 5 1 (5.2) mL 1 (5.2) mL mg/L 100 mL() 5 L g 5.3.1 5

9、 0 0 0 5.3.2 5 1 40 0.2 5.3.3 5 2 80 0.4 5.3.4 5 3 120 0.6 5.3.5 5 4 160 0.8 5.3.6 5 5 200 1.0 6 . . 6.1 (off-line) 1 . KS I ISO 15009:2009 6 1 , 100 mL(6.1.1) 2 (6.1.5) 3 4 (6.1.2) 5 , PTFE ISO 641 (6.1.3). 6 , 14/23, KS L ISO 383 . 7 (6.1.6) 8 (6.1.7) 9 (6.1.8) 10 , 14/23, KS L ISO 383 . 1 (off-li

10、ne) 1 . (on-line) . KS I ISO 15009:2009 7 . 6.1.16.1.9 . 2 . 6.1.1 3 100 mL . 6.1.2 . 6.1.3 PTFE 6.1.4 (402) mL/min . 6.1.5 (thermocouple) 6.1.6 KS L ISO 4799 Allin- Graham- 6.1.7 PTFE . 6.1.8 240 mg (4.6). (silanized glass fiber) . . . (: PTFE ) . 10 mL/min 3 250 . . , 1 ng . . . . KS I ISO 15009:2

11、009 8 . . 6.1.9 100 mL (thermocouple) . 6.2 2 0003 000 g 200 mL . 6.3 200 mL . 6.4 (Capillary column) (semipolar) . 8.4 A . 6.5 (flame ionization detector:FID), (electron capture detector: ECD, Ni63) 1 :10 1 :100 . (photo-ionization detector:PID) (mass selective detectors:MSD, ITD) . PID, MSD ITD .

12、6.6 . 250 /2 150 40 mL/min . 6.7 (Electronic integrator) (automatic recorder) 6.8 KS I ISO 15009:2009 9 0.1 L 5 L 1 L 50 L 6.9 7 , KS I ISO 103812 KS I ISO 103811 . . PTFE . (32) 4 . . 8 8.1 50 mL 5 50 L . . 8.2 KS I ISO 11465 . 8.3 . (6.3) 50 g . 50 mL (4.5) . (6.9) . 30 . . 10 2 000 g . 8.4 50 mL

13、(4.1) . 8.3 5 50 L (5.3.1) 5 L . 15 95 30 40 mL/min . (6.1.7). (6.1.8) . 15 600 mL . KS I ISO 15009:2009 10 8.5 8.5.1 . . : :25 m :50 m :0.32 mm :80 2.5 10 /min 280 280 10 . :300 : :2030 cm/s 0.53 mm 6.6 . . 90 % (R2). ethylbenzene ethylbenzene-D 10. . . . FID, ECD . 8.5.2 (5.3) . 50 mL (4.1) . 5 L

14、. 15 95 30 40 mL/min . 8.5.3 . . . . 5 % , . 5 % , . . , . (8.5.3) . . KS I ISO 15009:2009 11 y x t rel,x . y x x t t t IS , rel (1) t x :x t ISy : y -D10 (4.2.1) 1,4- (4.2.2) . y x R rel,x,y . R rel,x,y R x /R ISy c ISy /c x (2) R x :x R ISy : y c ISy : y c x : x 8.5.3 240 10 (8.3) . , . 8.5.2 0.5

15、% . . 5 L . 9 9.1 . . 2 . . , . RRR(relative response ratio) . , RRR 1.00. RRR1.000.05 . RRR 1.000.05 , . KS I ISO 15009:2009 12 . RRR . RRR 1.05 . , RRR . . . . , . 9.2 . 2(:-D10) 1,4- . . pe d te d .IS rel. IS e, IS e, e, ) 1 ( 1 V w m V w m R m R R w i i i (3) w i : i (mg/kg of dry matter) R e,i

16、: i R e,IS : m e,IS : (ng) R rel,i,IS : i m : portion (g) w d : V te : (mL) V pe : ( L) , . 10 kg mg 2 . 11 . B . 12 KS I ISO 15009:2009 13 . a) b) c) d) 10. e) KS I ISO 15009:2009 14 A () CP-Sil 5 CB CP-Sil 13 CB -D10(ethylbenzene-D10) :40 5 , 10 100 100 2 15 250 250 5 a) CP-Sil 5 CB column (dichlo

17、romethane) 0.212 29 trans-1,2-(trans-1,2-dichloroethene) 0.253 89 cis-1,2-(cis-1,2-dichloroethene) 0.312 39 (trichloromethane) 0.331 73 1,2-(1,2-dichloroethane) 0.385 69 1,1,1-(1,1,1-trichloroethane) 0.404 68 (benzene) 0.441 26 (tetrachloromethane) 0.453 19 1,2-(1,2-dichloropropane) 0.512 67 (trichloroethene) 0.536 20 cis-1,3-(cis-1,3-dicloropropene) 0.625 55 trans-1,3-(trans-1,3-dicloropropene) 0.68

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