1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 19739 KS I ISO 19739:2010 2010 7 13 http:/www.kats.go.krKS I ISO 19739:2010 : ( ) ( ) ( ) : (http:/www.standard.go.kr) : :2005 12 14 :2010 7 13 2010-0260 : : ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 19739:2010 i .1 1 1 2 1 3 .1 4 3 5
2、 4 6 4 6.1 .4 6.2 .5 6.3 .5 6.4 .5 6.5 5 6.6 .5 6.7 .6 6.8 .6 6.9 .6 6.10 6 7 7 8 7 9 7 10 8 A( ) ( ).9 B( ) .10 C( ) FPD GC 14 D( ) ED GC 20 E( ) MSD GC .26 F( ) AED GC 29 G( ) FPD GC .32 H( ) SCD GC 44 I( ) PFPD GC .50 54 KS I ISO 19739:2010 Natural gas Determination of sulfur compounds using gas
3、chromatography 2004 1 ISO 19739, Natural gas Determination of sulfur compounds using gas chromatography , . 1 , , C1 C4 , THT (tetrahydrothiophene) (GC) . , . 2 . . ( ) . KS A ISO 5725 2, ( ) 2: KS I ISO 6141, KS I ISO 6143, KS I ISO 6145 10, 10: KS I ISO 10715, KS I ISO 14532, 3 . 3.1 alkane thiol
4、(alkyl mercaptan) R SH , KS I ISO 19739:2010 2 . KS I ISO 14532, 2.5.3.3.1 Methanethiol(MeSH), ethanethiol(EtSH), 2-methylpropane-2-thiol(tert-butylmercaptan TBM) 3.2 (alkyl disulfide) R S S R(R and R are alkyl groups) KS I ISO 14532, 3.5.3.3.3 3.3 (alkyl sulfide) (thioether) R S R(R and R are alkyl
5、 groups) , KS I ISO 14532, 3.5.3.3.2 dimethyl sulfide(DMS), diethyl sulfide(DES) 3.4 (carbonyl sulfide) COS KS I ISO 14532, 3.5.3.3.4 3.5 (chromatographic resolution) KS I ISO 14532, 2.5.3.4.6 baseline . 3.6 cyclic sulfide (thioether) tetrahydrothiophene(thiophane or thiacyclopentane: THT), C4H8S( .
6、) KS I ISO 14532, 2.5.3.3.6 3.7 (hydrogen sulfide) H2S KS I ISO 19739:2010 3 KS I ISO 14532, 2.5.3.3.8 3.8 (normal reference conditions) , , ( ) 101 325 kPa, 273 15 K, . KS I ISO 14532, 2.6.1.3 3.9 (standard reference conditions) , , ( ) 101 325 kPa, 288 15 K, . KS I ISO 14532, 2.6.1.4 3.10 (total s
7、ulfur) KS I ISO 14532, 2.5.3.3.17 , . 3.11 (working reference gas mixture) WRM (working standard gas mixture) (CRM) KS I ISO 14532, 2.5.3.5.2.3 3.12 (secondary standard gas mixture) PSM KS I ISO 14532, 2.5.3.5.2.2 3.13 (primary standard gas mixture) PSM , KS I ISO 14532, 2.5.3.5.2.1 4 (GC) KS I ISO
8、19739:2010 4 . . 5 5.1 , , , 5.2 (6.4 ) 1.5 , 1 A . 2 COS H2S . 5.3 (sulfur-specific) (multi-specific) , B . 1 , . 2 (matrix effect) . 3 . 4 . . , . , , , , . 6 . . . . KS I ISO 10715 . . , . 6.1 KS I ISO 19739:2010 5 KS I ISO 10715 . . 6.2 , ( ) , 7 . . . ( 90 ). 6.3 , , . KS I ISO 10715 . 6.4 . ,
9、. , , . . KS I ISO 10715 . 6.5 . . KS I ISO 10715 A . 6.6 KS I ISO 10715 . , . . KS I ISO 19739:2010 6 , . . 10 % . , . (needle valve) . , . . 6.7 ( ) . KS I ISO 10715 . . , . 6.8 KS I ISO 10715 . 3.175 mm(1/8 in) (80100) mL/min . . (separation effects)( ) 10 mL/min . . . 6.9 . . 6.10 . . . . KS I I
10、SO 19739:2010 7 7 KS I ISO 6143 KS I ISO 6145 10 . (: ) . KS I ISO 6141 . 1 . , (matrix gas) . . . 2 . . , (mercaptan) (disulfide) . 8 KS I ISO 6143 . . . 9 7 . , IUPAC , ( ) . a) 1 (H2S): 3 mg/m3 (CH4): b) 2 (COS): 5 mg/m3 methanethiol(MeSH): 5 mg/m3 ethanethiol(EtSH): 5 mg/m3 2-methylpropane-2-thi
11、ol(TBM): 6 mg/m3 diethyl sulfide(DES): 10 mg/m3tetrahydrothiophene(THT): 25 mg/m3 methane(CH4): KS I ISO 19739:2010 8 7 . 1 . 1 (performance characteristics for sulfur analysis) ( ) mg/m3(norm.ref.cond.) () mg/m3(norm.ref.cond.) () % () % H2S 3 0.1 3 25 COS 5 0.1 2 15 MeSH 5 0.1 2 10 EtSH 5 0.2 4 30
12、 TBM 6 0.4 7 25 DES 10 0.2 2 20 THT 25 1.0 4 20 1 5(4.1, 4.2, 4.3 ) z , . THT 25 mg/m3 , 19 mg/m3 31 mg/m3 (255) mg/m3( 1 20 %)1 mg/m3( 1 4 %) . 1 .: n1 values(KS A ISO 5725 2 95 % ) , (KS A ISO 5725 2, 7.3.4.1 ), 5 10 . a) b) / ( ) c) d) WRM , e) f) , , KS I ISO 19739:2010 9 A ( ) ( ) df m . . 100
13、% 100 % - 5 % - 95 % 50 % 50 % 100 % 40 % 80 10080 10080 100KS I ISO 19739:2010 10 B ( ) B.1 B.1 . B.2 (Atomic Emission Detector: AED) , . . F B.3 (Electrochemical Detector: ED) , ( ). , . . D B.4 (Electron Capture Detector: ECD) . (DC voltage mode). . . B.5 (Flame Photometric Detector: FPD) FID . (
14、 .) . . ( , , , ). , . . . C G KS I ISO 19739:2010 11 B.6 (Pulsed Flame Photometric Detector: PFPD) FPD . . (FPD .), . . PFPD , . , 10 ms , . . 300 ms inlet tube GC . 3 . I B.7 (Hall-Electrolytic Conductivity Detector: ELCD HELCD) . . ( , , ), . B.8 (Mass Selective Detector: MSD) . . . . . E B.9 (Photoionization Detector: PID) . . , , H2S . B.10 (Thermoionization Detector: TID) . B.11 (Sulfur Chemiluminescence Detector: SCD) KS I ISO 19739:2010 12 . . H B.12 (Thermal Conducti