HPLC mg 5 RSD 10%

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1 24 8 Vol. 24 No Chemical Research /L- and Application Aug HPLC 1 2 2* / TG /DTA HPLC 10 /min 300 ml /min TG DTG ~ HPLC mg /g mg 5 RSD 10% / TG /DTA HPLC O A Establishment of a thermogravimetry/ differential thermal analysis-cambridge filter-absorption bottle trapping unit-high performance liquid chromatography and its applicaton in volatile phenols LU Lan 1 2 YANG Liu 2* WU Yi-qin 2 YANG Ji 2 3 MENG Zhao-yu 2 MOU Ding-rong 2 1. College of Chemistry and Chemical Engineering Kunming University of Science and Technology Kunming China 2. R&D Center of Hongta Tobacco Group Co. Ltd Yuxi China 3. School of Chemical Science and Technology Yunnan University Kunming China Abstract A new combination system of thermogravimetry /differential thermal analysis TG /DTA -Cambridge filter-absorption bottle trapping unit-high performance liquid chromatography HPLC was established and applied to analysis the seven volatile phenols in evolved pyrolysis products and the reliability of the new system. Firstly the main weight loss temperature MWLT of pipe tobacco was obtained according to the TG and DTG curves at 10 /min heating rate and 300 ml /min of nitrogen flow which was from room temperature to 600 then the seven volatile phenols was trapped and analysed qualitatively and quantitatively using the combination system in MWLT. Results indicated that volatile phenols in evolved gas was trapped selectively by the two different trapping ways cambridge filter was more inclined to trap hydroquinone resorcinol and catechol while absorption bottle was more inclined to liuyang929@ 126. com

2 trap phenol p-cresol m-cresol o-cresol. Yields of each polyphenol in evolved gas was different in the same condition phenol and catechol was higher than others which was and mg /g respectively While resorcinol was the lowest which was mg /g. This combination system had high reliability as the relative standard deviation RSD of each volatile phenol in 5 parallel experiments were all bellow 10% and it could be used to study the generation of volatile phenols in the pyrolysis process with temperature programming. Key words thermogrametry /differential thermal analysis TG /DTA cambridge absorption bottle trapping unit evolved products volatile phenols high performance liquid chromatography HPLC Pyris Diamond TG /DTA / SII Aligent Aligent 44 mm Whatman WHO Fisher - Supelco 5 - Dr. Ehrenstoffe GmbH MΩ. cm AB204-S g Py-GC /MS Fig. 1 Trapping diagram of cambridge filter coupling with absorption bottle Py-GC /MS /4 44 mm

3 8 - HPLC ml 1% 2 10 /min ml /min TG 200 mg mg - DTG mg - ~ ml g ml ~ 600 1% 100 ml 1% μg / ml μg /ml μg /ml ± 1 2 h 40 Fig. 2 The thermogravimetric and derivative thermogravimetric curves of pipe tobacco μg ~ 500 ml / min YC /T HPLC ml /min 50 /min min 32 mg ± mg 300 ml /min 10 /min 600 3a Fig. 3a Chromatogram of the seven volatile phenols in standard sample 25 ml ml 1% 20 min 5 min μm HPLC μm HPLC 2 3b 2. 1 Fig. 3b Chromatogram of the seven volatile phenols in absorption solution

4 ml 1% = ρ V /n mg /g ρ μg /ml V 3c n mg Fig. 3c Chromatogram of the seven volatile phenols in cambridge filter Table 1 1 mg /g Yields of volatile phenols in cambridge filter and absorption solution RSD% n = % - - > - - > - > - > % % % Table 2 Trapping effect of cambridge filter and absorption solution % % ml 1% ml 1%

5 8 - HPLC % TG /DTA - - HPLC 66. 4% % % RSD 1 5 RSD 10 Torikai K Yoshida S Takahashi H. Effects of tempera- 1. ture atmosphere and PH on the generation of smoke compounds during tobacco pyrolysis J. Food Chem Toxicol J J M. 3. M M DietrichI Hoffwann Ilse Hoffwann. The less harmfull cigarette A controversial issue. A tribute to Ernst L Wynder J. Chem Res Toxieol polycylic aromatic hydrocarbons formed during the pyrolysis of phenylalanine J. J Chromatogr A HPLC J J. 14 YC /T Thomas E McGrath Gedffrey Chan W Mohanad R Hajaligol. Low temperature mechanism for the formation of polycyclic aromatic hydrocarbons from the pyrolysis of cellulose J. J Anal Appl Pyrol Baker R R Bishop L J. The pyrolysis of tobacco ingredients J. J Anal Appl Pyrol Paulik F Paulik J Arnold M. Examination of phase equi- librium of the Ca NO 3 2 -H 2 O system with quasi-isothermal-quasi-isobaric themogravimetry and DTA J. J Therm Anal Su-Fang Wang Bai-Zhan Liu Kai-Jian Sun et al. Gas chromatographic-mass spectrometric determination of S. 15 Schmeltz I Scholotzhauer W S. Benzo a pyrene phenols and other products from pyrolysis of the cigarette additive d 1 -menthol J. Nature J