1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M ISO 16591 KS M ISO 16591:2012 2012 12 14 http:/www.kats.go.krKS M ISO 16591:2012 : ( ) ( ) GS () SK ( ) : (http:/www.standard.go.kr) : :2012 12 14 2012-0706 : : ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS M ISO 16591:2012 i ii 1 1 2 1 3 1 4 .2 5
2、3 6 5 7 .5 7.1 (titration cell) 5 7.2 .6 7.3 6 7.4 .6 8 6 9 7 10 8 11 .8 12 8 12.1 8 12.2 , r 9 12.3 , R.9 13 9 A( ) 1 mg/kg (standby technique) 10 B( ) 11 C( ) .13 15 KS M ISO 16591:2012 ii 2010 1 ISO 16591, Petroleum products Determination of sulfur content Oxidative microcoulometry method , . KS
3、M ISO 16591:2012 Petroleum products Determination of sulfur content Oxidative microcoulometry method 1 (final boiling point) 400 . (1 100) mg/kg . 100 mg/kg . 1 mg/kg A . (1 100) mg/kg . 0.1 %(m/m) 1.0 %(m/m) , (sodium azide) . 500 mg/kg . 1 (900 1 200) (26 274) , MS (motor spirit sample) . ( , ) .
4、2 - KS M ISO 4260 . 3 “%(m/m)” . 2 . . ( ) . KS M 2001, KS M 2002, KS M ISO 3171, KS M ISO 3696, KS M ISO 12185, U 3 . KS M ISO 16591:2012 2 , 3- . 3- , . . I3 SO2 H2O SO3 3I 2H+ (1) 3I I3 2e- (2) 4 , KS M ISO 3696 3 . 4.1 500 mL 1 000 mL , (KI) (0.50.01) g (NaN3) (0.60.01) g . (CH3COOH) 5 mL . . ,
5、. , , , , . 3 . 4.2 , 99.995 % . 4.3 , 99.995 % , . (baseline) . 4.4 , (resublimed) . 4.5 , , (0.5 mg/kg ) (5 mg/kg ) . , 2,2,4- , . 4.6 (stock solution) 4.6.1 (certified reference material, CRM) (200 500) mg/kg 4.6.2 ( ) . . 100 mL 0.1 mg . (4.5) , 0.1 mg . 0.000 1 %(m/m) (1 mg/kg) . KS M ISO 16591
6、:2012 3 . a) 38.103 %(m/m) (thiophene) b) 21.915 %(m/m) (dibutyl sulfide) c) 17.399 %(m/m) (dibenzothiophene) d) 23.89 %(m/m) (thionaphthene) KS M ISO 20846( ) 4.4.2 4.4.4 4.7 (4.5) (4.6) . 3 , 5 . 5 5.1 5.1.1 5.1.2 5.1.7 . 1 . 1 (septum) 5 2 6 3 7 4 8 a (O2) b 1 5.1.2 , 2 3 . . . KS M ISO 16591:201
7、2 4 . . 5.1.3 , . (syringe) . . (quartz wool) 20 mm . 2 . (scrubber) . (soot), , , . 230 (recovery) . a) TOT b) COT 1 a , O2bAr, He N2 2 5.1.4 , (seal) . 5.1.5 , 3- - 3- (generator) - . . (Faraday cage) , mg/kg . KS M ISO 16591:2012 5 , . . . . 5.1.6 , / (attenuation) (gain control) - (bias potentia
8、l) . (equivalent current) (titrant) . . 5.1.7 / , 0.1 mV/25 mm (10 20) mm/min . . PC/ . 5.1.8 , (30 60) W . (90 300) ( ). 5.2 ( ) , ( ). . . , . 5.3 , (4.2) (4.3) 2 . 5.4 , (single-pan) (two-pan) 0.1 mg . 5.5 , , , (100 1 000) mL (one-mark) 6 6.1 KS M 2001 KS M ISO 3171 . 6.2 (subsample) . 70 (cloud
9、 point) 15 . 7 7.1 (titration cell) 7.1.1 . . . . KS M ISO 16591:2012 6 7.1.2 (4.4) 2 g (4.1) . 50 mm . . . . . 7.1.3 . , . (5 8) mm . 7.1.4 , . . 7.1.5 . 7.2 ( ) , 1 . (furnace) ( ). 7.3 (5.1.8) . 7.4 , , , . . 8 8.1 (4.7) . 3 . 8.2 , . 8.3 . . 0.1 mg , . (0.1 1.0) L/s . (needle blank) . (plunger)
10、. . . KS M ISO 16591:2012 7 8.4 . 8.4.1 3 b) . 8.4.2 (tailing) 3 a) , (bias) . 8.4.3 (overshooting) 3 c) (bias) . 8.5 (5.1.7) . . 8.6 g . (SO2) 3 (SO3) , (4.5 4.7 ). 75 % , , . (7590) % . B . . 8.7 . 8.8 10 . (4.7) (8.1 ). a) b) c) 3 9 9.1 KS M 2002 KS M ISO 12185 0.1 kg/m3 KS M ISO 16591:2012 8 . 3
11、 KS M ISO 91 1 . 9.1.1 (5.2) 8.3 8.5 . 3 . 9.1.2 . 3 . 9.2 (8.6) . 10 10.1 (3) wS mg/kg . testtS,Smmw = (3) mS,t: (g) mtest: (g) (L) (kg/m3)10 6 . 10.2 (4) . test1testtS,Smmmw = (4) mtest1: mtest (g) 10.3 C . (SO2) . 11 10 mg/kg 0.1 mg/kg , (10 100) mg/kg 1 mg/kg . 12 12.1 (1 110) mg/kg KS M ISO 425
12、9 12.2 12.3 . KS M ISO 16591:2012 9 12.2 , r , 20 1 . r 0.063X X: 12.3 , R 2 , 20 1 . R 0.147X X: 13 . a) b) c) (11. ) d) , e) KS M ISO 16591:2012 10 A ( ) 1 mg/kg (standby technique) A.1 1 mg/kg SO2 . 1 mg/kg . A.2 A.2.1 , . A.2.2 25 L 10 L . “ ” ( . ). A.2.3 “ ” 10 L 0.3 L/s . . A.2.4 (30 60) . (1
13、 2) , , “ ” . . A.2.5 (4.7) , (4.5) A.2.2 A.2.4 . (“ ” ) . A.2.6 , . KS M ISO 16591:2012 11 B ( ) B.1 B.1.1 , . . . B.1.2 . B.1.3 , 2 . B.1.4 . “ ” . (FBP) . , . ( ) . . , (devitrification) “ ” . 50: 50( ) (HF) . . . . . . . HF( ) . . . . HF 1 . B.1.5 KS M ISO 16591:2012 12 . , (5.1.5, ) . . B.1.6 . B.1.7 ( ) . B.2 . 5A . B.3 . . . . . B.4 , . B.5 B.5.1 . . . . B.5.2 . . KS M ISO 16591:2012 13 C ( ) C.1 C.1.1 3- (2) . (3- ) , Q . C.1.2 . (: C/s) i T(: ) (Q iT)