1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS H ISO 15303 GC/MS KS H ISO 15303:2008 2008 8 6 http:/www.kats.go.krKS H ISO 15303:2008 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) ： ： 2003 8 30 ： 2008 8 6 2008-0410 ： ： ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS H ISO 15303:2008 i .1 1 1 2 1
2、 3 2 4 2 4.1 .2 4.2 .2 4.3 2 4.4 .2 4.5 (RBD) 2 5 .2 5.1 .2 5.2 2 5.3 2 5.4 2 5.5 / 2 5.6 (vortex mixer).3 6 3 6.1 .3 6.2 3 6.3 .3 6.4 GC/MS .3 6.5 .4 7 .4 7.1 .4 7.2 5 8 5 8.1 .5 8.2 .5 8.3 .5 A( ) .6 A.1 .6 A.2 , 1993 6 A.3 , 19948 KS H ISO 15303:2008 GC/MS Animal and vegetable fats and oils Detec
3、tion and identification of a volatile organic contaminant by GC/MS 2001 1 ISO 15303, Animal and vegetable fats and oils Detection and identification of a volatile organic contaminant by GC/MS , . ISO 15303 ISO/TC 34 (SC 11) . A . 1 . . . . . . . , , , , , 1 mg/kg 10 mg/kg . 2 . . ( ) . KS H ISO 1530
4、3:2008 2 KS H ISO 661, 3 GC . GC/MS . . 160 GC/MS . 4 , , . 4.1 ( 99 %). 4.2 . 4.3 , ( 99 %) 4.4 . 4.5 (RBD) 5 . 5.1 5.2 5.3 1)5.4 50 m, OV101( .) , 0.5 m 0.32 mm . 5.5 / . 1) Chrompack . ISO . KS H ISO 15303:2008 3 a) ( ) 160 40 5 40 160 . GC . 3 160 . b) GC 50 5 7.5 / 250 5 c) MS 1 / (source) 70 e
5、V, 200 , 100 A, 4 kV d) 1 mL/ (split during cold trapping) 5 mL/ 5.6 (vortex mixer) 6 6.1 6.1.1 (4.5) . 6.1.2 (6.1.1) ( 100 mg/kg) (4.1)( ) . . ( 1 mg/kg 10 mg/kg ). . 6.1.3 1.0 mg/kg 10 mg/kg (4.5) . 6.2 (4.2) 0.1 g/L(0.1 g/L) , (4.3) . GLC . 6.3 1.00 g . 6.2 (4.2) 5.0 L . (5.6) . , . . 6.4 GC/MS K
6、S H ISO 15303:2008 4 . 3 cm 4 cm . 10 mg . 10 mg 10 mg/kg 2.5 mg . 1 mg/kg 10 mg/kg(6.1.3 ) (6.1.1) . 20 40 . TCT TCT GC/MS . 6.5 GC mass . GC . . (co-elutants) . 7 7.1 R . isCCKR= K ： C ： Cis ： isSAMSAMCCKR= RSAM： R CSAM： Cis RSAM = F CSAM F isCKF = , R RSTD= F CSTD CSTD： KS H ISO 15303:2008 5 STDS
7、AMSTDSAMRRFCFC=STDSTDSAMSAMRCRC= 7.2 . 8.2 . 2 . 0.6 mg/kg , kg 1.0 mg 4 . . 8 8.1 A . . 8.2 2 0.6 mg/kg 5 % . 8.3 2 1.43 mg/kg 5 % . 1,1,1- (1,1,1-trichloroethane), 2- (2-ethyl hexyl acrylate), (dicylopentadiene), (tetrachloroethylene), N,N-(N,N-ethylmethylaniline), N,N- (N,N-dimethylaniline), -2-
8、(hexan-2-ol), (benzen), (cumene) (ethyl acrylate) (ring test) ( ). KS H ISO 15303:2008 6 A ( ) A.1 2 . 1993 , A.1 . 1994 , A.3 . 1996 4 ISO/TC 34/SC II , . ISO 5725 : 1986 KS A ISO 5725 1 . A.2 , 1993 ： 10 21 ( ) ： 5 7 ( ) A H 8 . 3 3 . A.1 . A.2 . . ISO . KS H ISO 15303:2008 7 A.1 a (spiked) mg/kg
9、A (Dichloromethane) 1,2- (1,2-Dibromoethane) 1,1,1- (1,1,1-TRICHLOROETHANE) 1.12 B 2- (2-ETHYL HEXYL ACRYLATE) (Methyl acrylate) (Dipentene) 1.25 C t- (Methyl t-butyl ether) (DICYCLOPENTADIENE) (Furfural) 1.29 D (Trichloroethylene) (TETRACHLOROETHYLENE) 2- (2-Furaldehyde) 1.03 E N,N- (N,N-ETHYLMETHY
10、LANILINE) 5- -2- (5-Ethyl-2-methylpyridine) N,N- (N,N-Dimethyl aniline) 1.04 F (Pyridine) N,N- (DIMETHYLANILINE) (Nitrotoluene) 1.10 G (Butanal) -2- (HEXAN-2-OL) (Di-isobutyl ketone) 1.04 H (Cumene) (Pyridine) (BENZENE) 1.04 a , . KS H ISO 15303:2008 8 A.2 A B C D E F G H (mg/kg) (mg/kg) 7 1.111.127
11、 1.321.257 1.531.297 1.051.037 1.58 1.04 7 1.18 1.10 7 0.83 1.04 7 0.911.04 sr(mg/kg) (%) r(2.83 sr) 2 0.1513.70.432 0.085.6 0.233 0.1215.90.622 0.086.6 0.213 0.13 19.4 0.51 2 0.04 3.5 0.11 2 0.11 14.3 0.31 3 0.044.0 0.11 sR(mg/kg) (%) R(2.83 sR) 7 0.6458.21.826 0.5742.21.617 1.0979.03.096 0.2929.70
12、.815 1.80 13.5 5.09 6 0.43 36.8 1.22 6 0.44 53.0 1.25 7 0.1819.60.51 (mg/kg) 0.58 2.500.58 2.100.57 3.500.68 1.300.40 4.73 0.4 1.7 0.17 1.37 0.6 1.10 r R . (r) 0.36 (R) 2.38 . A.3 , 1994 ： 7 16 ： 5 9 I K 3 . 3 3 . A.3 . A.4 . KS H ISO 15303:2008 9 A.3 a (mg/kg) I 2- (2-Ethyl hexyl acrylate) (ETHYL A
13、CRYLATE) (Vinyl acetate) 1.03 J N,N- (N,N-Dimethylaniline) (Epichlorhydrin) 1,3- (1,3-Dichloropropen) K (CUMENE) (Tetrachloroethylene) N,N- (N,N-ethlymethylaniline) 1.25 a , . A.4 ( m/z ) I(55) K(105) K(105) K(120) K(120) ( m/z ) (84) (98) (116) (98) (116) (mg/kg) 9 7 1.19 9 8 0.94 8 8 0.99 8 6 0.92
14、 8 7 0.97 sr(mg/kg) (%) r(2.83 sr) 0.48 40.0 1.3 0.07 7.7 0.2 0.08 8.5 0.24 0.04 4.15 0.11 0.08 8.7 0.24 sR(mg/kg) (%) R(2.83 sR) 0.50 42 1.4 0.50 53.25 1.4 0.51 51.2 1.4 0.52 56.8 1.47 0.52 53.5 1.47 (mg/kg) 0.5 2.75 0.16 1.69 0.15 1.66 0.1 1.47 0.09 1.67 r R . (r) 0.61 (R) 1.43 . KS H ISO 15303:20
15、08 10 1 ISO 5725： 1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests 2 KS A ISO 5725 1, ( ) 1： 3 Leatherhead Food Research Association. Research Reports, No.708(June 1993) 4 Leatherhead Food Research Association. Te
16、chnical Notes, No.110(April 1994) 5 Leatherhead Food Research Association. Research Reports, No.742(February 1997) GC/MS 135513 7017 (02)60094114 (02)600948878 http:/ Korean Agency for Technology and Standards http:/www.kats.go.kr KS H ISO 15303:2008 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Animal and vegetable fats and oils Detection and identification of a volatile organic contaminant by GC/MS ICS 67.200.10
