KS M ISO 17052-2012 Rubber raw-Determination of residual monomers and other volatile low-molecular-mass compounds by capillary gas chromatography- Thermal desorption(dynamic headsp.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M ISO 17052 ( ) KS M ISO 17052:2012 2012 12 10 http:/www.kats.go.krKS M ISO 17052:2012 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) ： ：2012 12 10 2012-0684 ： ： ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS M ISO 17052:2012 i ii 1 1 2 1 3 .2 4 2 5

2、 2 6 2 7 .2 8 3 9 4 10 5 11 .5 A( ) ( BR, SBR, NBR) .6 B( ) ( EPDM, EOM) 7 C( ) .8 13 KS M ISO 17052:2012 ii 2007 1 ISO 17052, Rubber, raw Determination of residual monomers and other volatile low-molecular-mass compounds by capillary gas chromatography Thermal desorption (dynamic headspace) method

3、. KS M ISO 17052:2012 ( ) Rubber, raw Determination of residual monomers and other volatile low-molecular-mass compounds by capillary gas chromatographyThermal desorption(dynamic headspace) method . . . . ( ) . 1 ( ) . , . , , . C4 C12 (monomers), , . 2 . . ( ) . KS M ISO 1795, KS M ISO 2393, , KS M

4、 ISO 17052:2012 2 KS M ISO 23529, 3 . 3.1 (relative response factor) RRF 4 (carrier gas) . , (trap) . , . . 5 . . 5.1 , , 6 . 6.1 2 , KS M ISO 2393 . 6.2 , , , , . 6.3 , 0.000 1 g . 6.4 20 mL , (septum) , (screw thread) . 6.5 (microvolume) , 1 L , “ (needle in needle)” , 0.01 L 7 7.1 . 7.2 A B . KS

5、M ISO 17052:2012 3 8 8.1 ( ) . , (1) . smmsRRFmAmA= (1) RRF ： ( ) Am： As： mm： 0.000 1 g (g) ms： 0.000 1 g (g) , ( 1, 2, 3 ). 8.2 (stock) , . 1 % / 5 % ( ) . . (1 100) ppm , 1 % . (100 1 000) ppm , 5 % . 100 ppm , 1 % 5 % . 20 mL (6.4) . 8.3 (working) . ( ) . 8.4 (dynamic headspace) , 5- . (linearity

6、) . ( ) 5 . . , (1 1 000) g/g “ (full)” . (6.5) (packing) 1 L , . 1 g . 5- . , 1- . KS M ISO 17052:2012 4 . 10 % . , 5 . . 9 9.1 . , (purge) . 9.2 KS M ISO 1795 (2505) g . (chip) , (package) . (mill) , . KS M ISO 1795 KS M ISO 2393 , (3.50.5) mm 6 , KS M ISO 23529 . 9.3 0.25 g . 0.5 mm , 0.000 1 g 0

7、.05 g . , 0.000 1 g 0.05 g . , . . , , , . . , ( ) . ( ) , . . , . 9.4 (2) . , . KS M ISO 17052:2012 5 mAVCAC=ccRRF(2) C ： (g/g) Cc： (g/mL) V ： (1 L) A ： Ac： m ： (g) RRF ： , 1 . 9.5 , , . 10 C . 11 . a) ： 1) , (bale), , 2) 9.2 b) , c) ： 1) 2) 3) d) ： 1) 2) ( .) 3) (duplicate) ： g/g(ppm) e) KS M ISO

8、17052:2012 6 A ( ) ( BR, SBR, NBR) A.1 . 34 . A.2 BR SBR NBR , 125 125 125 , 30 30 30 KS M ISO 17052:2012 7 B ( ) ( EPDM, EOM) B.1 . B.2 EPDM EOM (Ethylidene norbornene) (ENB)( ) (octene) ( ) ENB 1- , 200 150 , 10 10 KS M ISO 17052:2012 8 C ( ) C.1 (interlaboratory test programmes： ITPs) , 2003 , 2

9、2005 , ISO/TR 9272:2005 . C.2 ITP 1 (2003 ) C.2.1 2003 ITP . . 1 1 ppm 7 ( “ ” ) . 1 2 NBR, EPDM, EOM . 2 1 ppm . , . 1： 1 NBR-1, 2 NBR-2, 3 SBR, 4 EPDM-1, 5 EPDM-2, 6 EOM-1, 7 EOM-2, 2： 1 NBR-1, 2 NBR-2, 3 SBR, 8 SBC, 8 SBC, 8 2003 ITP 1 . 3 . C.2.2 2003 ITP . KS M ISO 17052:2012 9 C.2.3 ITP 1 (200

10、3) C.1 A, B, C . A 1 . A ISO/TR 9272:2005 (outliers) . . r R (r) (R) ( ). C.1 B C 2 . A 2003 ITP . ： (local domain) C.1 A . ( ) r (r) , , . . ： (global domain) C.1 A . ( ) R (R) , . . C.2.4 2003 ITP C.1 A , . (7 ), r 0.56 ( r/ r) . , R 0.66 ( R/ R) ( C.2 ). . r ITP . , 1/(r) (negative) . R ( ITP ) .

11、 , 150 ppm , R . (R) , . 2003 ITP 2005 ITP( ) (r) (R) (numerical) . r R . C.3 ITP 2 (2005 ) C.3.1 2003 ITP , . (scatter) . , ITP . SBR NBR KS M ISO 17052:2012 10 1 ITP . SBR , , NBR , ACN . NBR 2005 2004 . . NBR . , . . SBR (bulk) . , . , . 7 SBR , 5 NBR . 3 . (3 ) 3 . . 2003 2005 ITP . C.3.2 2005 I

12、TP . C.3.3 ITP 2 (2005) ( ) , C.3 . ISO/TR 9272:2005 (outliers) . . r R (r) (R) . 2005 ITP . ： (local domain) C.3 . ( ) r (r) , . . ： (global domain) C.3 . ( ) R (R) , . . C.4 (Bias) . , . KS M ISO 17052:2012 11 C.1 1 , ITP 1 (2003 ) A ： 1 ppm (：ppm) ( ) ppm srr (r) sRR (R) a1: NBR-1(ACN) 14 1.77 5.

13、0 36.6 10.9 30.5 225 5 2: NBR-2(ACN) 1.7 0.43 1.2 68.6 1.50 4.2 240 7 3: SBR( ) 0.84 0.37 1.0 121.7 0.78 2.2 258 5 4: EPDM-1(ENB) 113 6.20 17.4 15.4 37.4 105 92.7 6 5: EPDM-2(ENB) 120 5.86 16.4 13.6 56.5 158 131 7 6: EOM-1( ) 727 30.4 85 11.7 105 293 40.3 6 7: EOM-2( ) 23 1.53 4.3 18.4 12.1 34.0 146

14、 6 B ： (：ppm) 1: NBR-1( ) 1 1 1 1 1 1 1 8 2: NBR-2( ) 1 1 1 1 1 1 1 8 3: SBR( ) 1 1 1 1 1 1 1 8 8: SBC ( ) 1 1 1 1 1 1 1 8 , . C ：SBC (：ppm) 8: SBC ( ) 1 1 1 1 1 1 1 8 , . sr ( ), (ppm) r ( ) (r) ( ) sR ( ) R ( ) (R) ( ) a h k (ITP 8 ) 1 . KS M ISO 17052:2012 12 C.2 ( ) (2003 ) ( ) r r a r r 1: NBR-

15、1(ACN) 14 20.10 5.0 0.25 68.0 30.5 2: NBR-2(ACN) 1.7 1.12 1.2 1.06 5.73 4.2 3: SBR-3(styrene) 0.84 2.14 1.0 0.48 7.94 2.2 4: EPDM-5(ENB) 113 20.60 17.4 0.84 129.4 105 5: EPDM-6(ENB) 120 69.20 16.4 0.24 174.8 158 6: EOM-7(octene) 727 152.6 85 0.56 712 293 7: EOM-8(octene) 23 9.11 4.3 0.47 32.2 34.0 142.8 39.3 18.6 0.56 161.41 89.5 a / C.3 1 , ITP 2 (2005 ) ( ) ppm srr (r) sRR (R) aNBR (ACN)(2005 ) 42.7 2.01 5.6 13.2 7.21 20.2 47.9 4 NBR (ACN)(2004 ) 38.1 2.40 6.7 17.6 9.47 26.5 69.6 5 SBR( ) (2005 )