KS M 1075-2008 Determination of organotin compounds(MBT DBT TBT) in ceramic powder－GC MS method《陶瓷粉末中有机锡化合物(MBT、DBT、TBT)含量测量方法 气相色谱 质谱法》.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M 1075 (MBT, DBT, TBT) / KS M 1075:2008 2008 12 19 http:/www.kats.go.krKS M 1075:2008 : ( ) ( ) ()MPT ( ) : (http:/www.standard.go.kr) ： ： 2008 12 19 2008-0929 ： ： ( 02-509-7301) (http:/www.kats.go.kr). 10 5 , . KS M 1075:2008 (MBT, DBT, TBT) / Determinat

2、ion of organotin compounds(MBT, DBT, TBT) in ceramic powder GC/MS method 1 / . 2 . . ( ) . KS A 5101 1, 1： KS I ISO 17353, KS I ISO 22892, KS M 0001, KS M 0027, KS M 0031, KS M 8001, KS M ISO 3696, KS M ISO 6353 1, 1： 3 . / . 4 , . KS M 1075:2008 2 4.1 (Na2SO4) 4.2 (acetic acid) 4.3 10 % (sodium tet

3、raethylborate) 2 g (4.13) 20 mL . 4.4 (MBTCl, C4H9SnCl3) 96 % d 1.693 4.5 DBTCl, (C4H9)2SnCl2 96 % d 1.371 4.6 TBTCl, (C4H9)3SnCl 95 % d 1.207 4.7 TeBT, (C4H9)4Sn 93 % d 1.054 4.8 (n-hexane) HPLC 4.9 (methanol) (99 % ) 4.10 (KOH) (99 %) 4.11 2 mol/L (4.10) 112 g 1 L (4.9) . 4.12 (THF) . 4.13 4.13.1

4、(10 000 mg/L) 1)(4.6) 79.6 mg 100 mL . 4.13.2 (10 000 mg/L) 1)(4.5) 68.6 mg 100 mL . 4.13.3 (10 000 mg/L) 1)(4.4) 56.1 mg 100 mL . 1) . KS M 1075:2008 3 4.13.4 (10 000 mg/L) 1),2)(4.7) 88.2 mg 100 mL . 4.14 1： 100 . 4.14.1 (1 000 g/L) (4.13.1) 1 000 g/L . 4.14.2 (1 000 g/L) (4.13.2) 1 000 g/L . 4.14

5、.3 (1 000 g/L) (4.13.3) 1 000g/L . 4.14.4 (1 000 mg/L) (4.13.4) 1 000 g/L . 5 5.1 150 mL 5.2 100 mL 5.3 250 mL 5.4 5.5 5.6 80 /min 5.7 30 40 . 5.8 pH 5.9 / , , (mass detector) . 2) . KS M 1075:2008 4 KS M 0027 . . 6 6.1 KS A 5101 1 325 . . 6.2 10 g (1105) 2 . 6.3 1 g 0.1 mg . 6.4 . 7 7.1 a) 1 g 0.1

6、mg 150 mL (5.1) (4.11) 20 mL 1 . b) a) (4.14.4) 1 mL pH 4.5 , (4.8) 20 mL 10 % (4.3) 100 L 5 . c) b) 250 mL (5.3) (5.6) 30 20 mL 1 , . d) c) (4.1) 1 g , (5.7) 1 mL . . 7.2 . 7.3 7.3.1 KS M 1075:2008 5 1, 10, 100 mL TBT( ) (4.14.1) 100 mL 1, 10, 100 g/L . DBT( ) (4.14.2) MBT( ) (4.14.3) TeBT( ) (4.14

7、.4) 1, 10, 100 g/L , 7.1.1 . 7.3.2 7.3.1 . 7.4 . . (7.2) 7.5 . . . . 7.6 RF(response factor) . AiCiCmAmRF = Am ： Ai ： Cm ： (g) Ci ： (g) SwAiCiRFAm 1ion(mg/kg)Concentrat = KS M 1075:2008 6 Am ： RF ： Response factor Ai ： Ci ： (g) Sw ： (g) 8 . a) b) c) d) , e) KS M 1075:2008 7 A ( ) / . , . A.1 A.1.1 5

8、0 m 0.32 mm 0.17 m A.1.2 50 1 1.20 / 200 2.5 / 280 280 5 A.1.3 1 mL/ , A.1.4 (splitless) A.1.5 280 A.2 A.2.1 (ionization mode) (E.I.) A.2.2 (ion source temperature) 250 KS M 1075:2008 8 A.2.3 (ionization voltage) 70 eV 10 ( A.1) . / , . 3 . ( A.2) . A.1 (amu) (%) 112Sn 111.9 1.0 114Sn 113.9 0.7 115S

9、n 114.9 0.4 116Sn 115.9 14.7 117Sn 116.9 7.7 118Sn 117.9 24.3 119Sn 118.9 8.6 120Sn 119.9 32.4 122Sn 121.9 4.6 124Sn 123.9 5.6 A.2 (m/z) (MBT) 149, 179, 235 (DBT) 121, 149, 179 (TBT) 151, 177, 205 A.3 A.1 . KS M 1075:2008 9 X ( ) Y A.1 A.4 A.2 , A.3 GC/MS library . A.3 . A.2 X m/z Y A.3 GC/MS librar

10、y MBTDBTTBTTeBT ( ) Y X KS M 1075:2008 10 A.3 MBT, DBT TeBT reference (MBT) A.4 A.5 (DBT) A.6 A.7 (TeBT) A.8 A.9 A.4 A.5 GC/MS library A.6 Abundance 900080007000600050004000300020001000020 40 60 80 100 120 140 160 180 200 220 240 260 m/zAbundance 900080007000600050004000300020001000020 40 60 80 100

11、120 140 160 180 200 220 240 260 m/zAbundance 9000800070006000500040003000200010000m/z110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 KS M 1075:2008 11 A.7 GC/MS library A.8 A.9 GC/MS library Abundance 9000800070006000500040003000200010000Abundance 90008000700060005000400030002000

12、10000m/z110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 Abundance 900080007000600050004000300020001000020 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 m/zm/z20 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400 (MBT, DBT, TBT) / 135513 7017 (02)60094114 (02)600948878 http:/ KS M 1075:2008 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Determination of organotin compounds(MBT, DBT, TBT) in ceramic powderGC/MS method ICS 71.040.40 Korean Agency for Technology and Standards http:/www.kats.go.kr