1. INVESTIGATION OF MONO-ISOPROPYLNAPHTHALENE, DI-ISOPROPYLNAPHTHALENE AND TRI-ISOPROPYLNAPHTHALENE IN THE ENVIRONMENT AROUND THE PAPER RECYCLING PLANT Suzuki M, Matsumura C, Moriguchi Y, Nakano T Hyogo Prefectural Institute of Public Health and Environmental Sciences, 3-1-27 Yukihira-cho, Suma-ku, Kobe, Hyogo, 654-0037 Japan MIPN TIPN DIPN 1 2 45 6 7 8 3 Mono-Isopropylnaphthalene ( MIPN ), Di-Isopropylnaphthalene ( DIPN ) and Tri- Isopropylnaphthalene ( TIPN ) are widely used for PCBs substitutes such as jet printer ink, pesticide solvent and so on. They are concerned to have harmful influences to health and environment because of their high persistent and accumulating properties, but their fate in the environment had not been illustrated. Their optimum analytical methods for environmental samples had not been developed. Water sample 1L water sample ＋ NaCl 30g Clean up by sulfuric acidExtracted by 10mL Hexane Analyzed by GC/MS Shaking or mixing Concentrated to 200μL Cleaned up 20g sample methanol-hexane partition Extracted by alkaline degradation with 50mL KOH/MeOH for about 12 hours. Sediment and Biological sample Air sample Extracted by 30mL DCM Sampling 0.5 m 3 ~ 10m 3 air were introduced into PS-Air GC/MS ： Agilent6890N/JMS-Q1000GC Column ： Supelcowax-10 （ Polyethleneglycol ） Oven ： 50 ℃（ 1 ） →20 ℃ /min→100 ℃ →5 ℃ /min→210 ℃ →20 ℃ /min→270 ℃（ 1 ） Injection ： Injection Volume ： 2μL Injection Temp. ： 270 ℃ Carrier Gas ： He （ 1mL/min ） Interface ： 240 ℃ Split less （ Purge ON 1.5min ） Ion Source ： 210 ℃ Ionization ： 300μA, 70eV Detection Mode ： SIM Monitor Ion: HCB- 13 C 6 （ Internal Standard ） : GC (0.32mm×30m×0.25μm) MS 254 、 212 、 170 、 156 、 142 290, 255 2 1,3 1,7 DIPN MIPN TIPN 2,3 1,6 2,6 2,7 1,4 1,5 1 ① ② ③ ④ ⑤ ⑥ N.D. 5. It was considered that DIPN in sea bass was metabolized because the rates of decomposition were different by isomers. 2. DIPN and TIPN were detected from the water, the sediment, the air and the biological samples and MIPN was not detected all samples. 4. It was considered that there was another pollution resource of DIPN and TIPN in the Ibo River because high concentration of TIPN and the unusual fingerprint of DIPN isomers were detected from the sediment which was not influenced by the wastewater from the recycled paper factory. Wastewater from Paper Recycling plant Air sampling at Point C Algae Sediment 0 1000m The Paper Recycling Plant Ibo river at Point F Off the coast of Himeji Hyogo Pref. Point A Point B Point C Point E Point D Point D ’ Point F Point G Introduction Sampling Results Analytical procedure Conclusion GC/MS Condition Fig.1 The chromatogram of MIPN, DIPN and TIPN standard. Fig.2 Separated DIPN isomer peaks by columns. Wax-10 Ultra-2 Equity-5 ・ DIPN isomers peaks was rather separated by using polar column than medium polar one. ・ MIPN and DIPN isomers can be assigned and 6 TIPN isomers peaks was separated. Analyzed by GC/MS Concentrated to 200μL Analyzed by GC/MS Concentrated to 200μL Ibo River DIPN Water SedimentAlgae TIPN SedimentAlgae Sea bass Air News paper N.A. N.D. N.A. by the silica gel containing 5% water or florisil or sulfuric acid Recovery Detection limit (water) amount ： 20ng or 40ng Unit: ng/L Fig.3 The concentration of DIPN and TIPN in samples. 1. Development of their simultaneous analytical methods for the water, the air, the sediment and the biological samples. 2. Investigation of their concentration and isomer fingerprints in the environmental samples around the paper recycling plant. Fig.4 The fingerprints of DIPN isomers in samples. Y axis indicates a ratio to 2,6-DIPN. References Brzozowski R, Skupinski W, Jamroz H, M, Skarzynski M, Otwinowska H. Journal of Chromatography A 2002;946 3. The wastewater and the exhaust from the paper recycling plant were one of loading sources of DIPN. 1. The simultaneous analytical methods of MIPN, DIPN and TIPN in the water, the air, the sediment and the biological samples were developed. (1-MIPN) (1,3-DIPN) (1,3,5-TIPN) purpose (the roof of our institute)