KS I ISO 17735-2012 Workplace atmostheres-Determination of total isocynate groups in air using 1-(9-anthracenylmethyl)piperazine(MAP) reagent and liquid chromatography《工作场所的环境 1-(9.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 17735 1-(9- ) (MAP) KS I ISO 17735:2012 2012 12 27 http:/www.kats.go.krKS I ISO 17735:2012 : ( ) ( ) ( ) : (ISO/TC146) () ( ) : (http:/www.standard.go.kr) ： ：2012 12 27 2012-0785 ： ： (ISO/TC146) ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS I I

2、SO 17735:2012 i . iii 1 1 2 1 3 1 4 .3 4.1 MAP .3 4.2 5 4.3 (standard matching solution).5 4.4 HPLC 7 5 8 5.1 8 5.2 .8 5.3 .8 5.4 .9 5.5 .9 5.6 .9 6 10 6.1 .10 6.2 10 6.3 .11 6.4 (negative control) 11 6.5 11 6.6 12 6.7 .12 6.8 .12 7 HPLC 13 7.1 13 7.2 HPLC 13 8 .14 8.1 .14 8.2 ( ) 15 9 15 9.1 (stand

3、ard matching solution).15 9.2 .15 9.3 .16 9.4 .16 9.5 16 10 16 10.1 .16 KS I ISO 17735:2012 ii 10.2 ( ) 17 11 17 12 , .18 12.1 .18 12.2 .19 A ( ) 26 A.1 26 A.2 27 A.3 27 28 KS I ISO 17735:2012 iii 2009 1 ISO 17735, Workplace atmostheres Determination of total isocyanate groups in air using 1-(9-anth

4、racenylmethyl)piperazine(MAP) reagent and liquid chromatography , . KS I ISO 17735:2012 1-(9- ) (MAP) Workplace atmostheres Determination of total isocynate groups in air using 1-(9-anthracenylmethyl)piperazine(MAP) reagent and liquid chromatography 1 . ( ), (1,6- (HDI), (TDI), 4,4- (MDI) (IPDI), (H

5、DI ) . HDI IPDI HDI- IPDI IPDI . 11010 2107 . 2 . . ( ) . KS A ISO 5725 2, ( ) 2： KS I ISO 16200 1, / 1： 3 1-(9- ) (MAP) , MAP KS I ISO 17735:2012 2 , MAP . ( 13). , (SPE) , (UV) (FL) (HPLC) . , . . HPLC/UV/FL . UV FL , . ( ) FL (standard matching solutions) FL . UV ( , ) UV . 1 . 1 2 3 4 4,4-MDI 5

6、2,6-TDI 6 HDI 7 2,4-TDI 8 IPDI 9 HMDI 1 KS I ISO 17735:2012 3 4 . , . . , HPLC HPLC . 4.1 MAP MAP 2 9-( ) . HPLC . 25 mL 10.8 mmol(2.47 g) 9-( ) (98 % ) . . 37 mL 54.4 mmol(4.69 g) (99 % ) 21.8 mmol(3.04 mL) (99.5 % ) . 250 mL 2- . 30 9-( ) . 10 mL . 2 . 130 mL 1 3 . . MAP . . . MAP . MAP , . 50 mm

7、80 mm . . 80 mL MAP . 5 . . 20 mL 5 . . . , . . . (PTFE) 20 mL . (TLC) ( ) 1 L UV . MAP . , 400 mL . MAP KS I ISO 17735:2012 4 . , 1.0 L 1.5 L . MAP TLC . MAP TLC . TLC . TLC . 100 mm30 mm . 15 mm L 10 mm . 5 mm . . MAP UV . UV . Rf MAP Rf MAP . TLC MAP . . , . 35 40 . MAP . MAP . ( 20 mL) MAP . MAP

8、 . 6.67 mPa1) . 125 130 . . MAP . . 2.236 g(74 % ) . MAP 146 147 . MAP HPLC 99 % . 1 9-( ) 2 3 MAP 2 MAP 1) 1 Pa 7.5 torr KS I ISO 17735:2012 5 4.2 4.2.1 99 % . . MAP 110 4 mol/L (27.6 mg/L) . . 4.2.2 MAP 2 mg/mL . . 4.2.3 MAP 1104mol/L (27.6 mg/L) . . 4.2.4 2 . 1 . 4.3 (standard matching solution)

9、UV MAP . MAP MAP . UV . . 1 MAP 1 MAP . n . MAP MAP . . 1 MAP . 4.3.1 0.5 mmol(1 milliequivalent) 1 mmol(1 milliequivalent) 4 . 10 mL . 1.2 mmol MAP(20 % ) 4 . 20 mL . MAP 10 15 . 1 . . Bchner . MAP . 20 mL . KS I ISO 17735:2012 6 PTFE . 95 % . , . 4.3.2 HPLC MAP 5.0105mol( ) 2.5105mol( )(5.0105 ) 1

10、0 mL (KS L ISO 10421, A) . (dimethylformaide, DMF) DMF . MAP ( 2,4-TDI) . 5.0103mol/L( ) 2.5103mol( ) . . 2.0104mol/L( ) 1.0104mol/L( ) . , 1107mol/L( ) 0.5107mol/L( ) . 3 . 1 MAP meq MAP MAP 1-(9- ) MAP 276.38 276.38 57.05 57.05 333.43 333.43 99.13 99.13 375.51 375.51 119.12 119.12 395.50 395.50 1,

11、6- 1,6- HDI 168.20 84.10 720.96 360.48 (2,4- 2,6- ) TDI 174.16 87.08 726.92 363.46 1- 3- 3,5,5- IPDI 222.29 111.14 775.05 387.52 4,4- di-(4- ) 4,4- MDI 250.26 125.13 803.02 401.51 MDI (-4- ) 4,4- HMDI 262.35 131.18 815.11 407.56 NCO 42 42 4.3.3 (SPE) (SPE) MAP . DMF MAP DMF SPE . SPE . 2,4-TDI MAP K

12、S I ISO 17735:2012 7 . 2,6-TDI MDI MAP . MDI MAP MAP 1103mol/L( ) 0.5103mol/L( ) . MDI MAP 2104mol/L . . 4.3.4 HDI IPDI . 0.5 g 7 mL . 4.5 g(3.4 mL) . . 1 100(10 L 1 mL) . 25 L 975 L 5104mol/L MAP . 2 . . , 5 L HPLC 2 . 4.4 HPLC HPLC pH . ： . pH . MAP pH . pH . 4.4.1 3 840 mL 46.1 g 85 % ( 27 mL, 0.

13、4 mol) 15.1 mL 96 % (0.4 mol) . pH 1.6 . 10 mL (99.5 % ) 117 mL . pH 6.0 . , pH 6.0 . 2 L . 33.5 mL HCl . pH 1.6 . 2 L 33.5 mL . pH 1.6 6.0 0.1 mol/L 0.1 mol/L . 6 . 4.4.2 ( A) 65 % 35 % pH 6.0 . ( B) 65 % 35 % pH 1.6 . 0.45 m . . 6 . 4.4.3 35 mL 85 % 350 mL . 650 mL KS I ISO 17735:2012 8 . 0.45 m .

14、 . 6 . 5 5.1 ( 13). MAP (KS I ISO 17737). , MAP . 2 m ( ) . 2 m ( ), . 14 MAP . MDI ( 15) 2 m . 2 m 2 m , MAP . 5.1.1 ( ) , 5 % . . ( 37 mm , 13 mm ). (20 m ) , (IOM), . , ( 16). 5.1.2 . 1 mm 2 mm . . 5.2 2 L/min EN 12326 . 5.3 900 mm , . . ( , ) KS I ISO 17735:2012 9 . 2) . . , 3) . 5.4 5 % . 1 . 5.5 HPLC 0.45 m . 0.45 m PTFE . SPE (SPE) . PTFE . 500 mg 6 mL SPE PTFE . 5.6 5.6.1 5.6.2 HPLC