• Journal of the Korean Chemical Society
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• v.57 no.1
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• pp.40-51
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• 2013

In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were $2.58{\mu}g/L$ and $7.82{\mu}g/L$, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the $r^2$ value was 0.9992 in the concentration range of $7.82-100{\mu}g/L$, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the $^{19}F$ NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.

• Journal of the Korean Chemical Society
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• v.29 no.3
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• pp.213-219
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• 1985

The relative stability as a function of geometry in rigid cyclopropylcarbinyl cations was examined by $^{19}$F-nmr spectroscopy. 8-p-Fluorophenyl-tricyclo[3.3.1.0$^{2,7}$]octane-8-yl-(I), 9-p-fluorophenyl-tricyclo[3.3.1.0$^{2,8}$]nonane-9-yl (II), and 10-p-fluorophenyl-tricyclo[4.3.1.0$^{2,9}$]decane-10-yl cation(Ⅲ) were prepared from the corresponding carbinols in FSO$_3$H-SO$_2$ClF solution at -120$^{\circ}C$. $^{19}$F-nmr data indicate that the symmetrical bisected geometry of cyclopropane ring for ${\sigma}$-conjugation is a very impotant factor in charge delocalization. However, varied orientation of the bond angle ${\theta}$ within the bisected conformation does not affect the charge delocalization into the cyclopropane ring.