KMID : 0895420060160030222
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Journal of Korean Society of Occupational and Enviromental Hygiene 2006 Volume.16 No. 3 p.222 ~ p.232
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Gas Chromatographic Analysis of TDI, MDI and HDI Using 2-Chlorobenzyl Alcohol and 2,4-Dichlorobenzyl Alcohol Derivatives
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Yun Su-Song
Park Jun-Ho Lee Kang-Myoung Choi Hong-Soon Cho Young-Bong Koh Sang-Baek Cha Bong-Suk
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Abstract
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Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6- TDI), 4,4¡¯-methylenediphenyl diisocyanate(4,4¡¯-MDI) and 1,6- hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD).
Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4¡¯-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed.
Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4¡¯-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were 87 ¡É and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PDECD and GC/MSD.
Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4¡¯-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.
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KEYWORD
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total isocyanate, TDI, MDI, HDI, urethane, gas chromatography
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