Polímeros: Ciência e Tecnologia
Polímeros: Ciência e Tecnologia
Standards and Methods

Determination of Phthalates in Polymer Materials – Comparison of GC/MS and GC/ECD Methods

Jaworek, Katarzyna; Czaplicka, Marianna

Downloads: 1
Views: 1006


The paper presents two methods for determination of phthalates in polymer materials. The methods compared were gas chromatography combined with the mass spectrometry (GC/MS) and gas chromatography with electron capture detector (GC/ECD). The GC/ECD technique was chosen for this comparison, because the ECD detector was one of few capable of detecting phthalates. In both cases the same procedure of sample preparation with ultrasonic extraction was applied. Overall recoveries were 76-100 % with relative of standard deviation (R.S.D.) values in the range 0.6-19 %. The values of limit of detection (LOD) for GC/MS method ranged from 3.46 μg mL–1 to 10.10 μg mL–1, depending on the determined phthalate, while in case of the GC/ECD method they were in the range from 2.97 μg mL–1 to 4.29 μg mL–1. The methods were applied for determination of: dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate, diisononyl phthalate, diisoocyl phthalate in polymer material. The seventeen kinds of samples were analyzed. Most of the materials selected for the analyses were made from polyethylene (PE), polyvinyl chloride (PVC) and polystyrene (PS).


Gas chromatography, mass spectrometry, electron capture detector, phthalates, polymer material


1. Higuchi, T. T.; Palmer, J. S. & Kane, C. M. - Toxicol. Sci., 72, p.301 (2003). PMid:12655036. http://dx.doi. org/10.1093/toxsci/kfg036

2. Directive of the European Parliament and of the Council 2000/60/EC. Disponível em: .

3. U.S. Environmental Protection Agency. - ”Technology Transfer Network Air Toxics Website: Bis(2-ethylhexyl) phthalate (DEHP)” (2000). Disponível em: .

4. Directive of the European Parliament and of the Council 2005/84/EC. Disponível em: .

5. Marín, M. L.; Jimenez, A.; Berenguer, V. & Lopez, J. - J. Supercri. Fluids, 12, p.271 (1998). http://dx.doi. org/10.1016/S0896-8446(98)00086-2

6. Li, X.; Zeng, Z.; Chena, Y. & Xu, Y. – Talanta, 63, p.1013 (2004). PMid:18969528. http://dx.doi.org/10.1016/j. talanta.2004.01.006

7. Niino, T.; Ishibashi, T.; Itho, T.; Sakai, S.; Ishiwata, H.; Yamada, T. & Onodera, S. - J. Chromatogr. B, 780, p.35 (2002).

8. Li, X.; Zhong, M.; Xu, S. & Sun, C. - J. Chromatogr. A, 1135, p.101 (2006). PMid:17022987. http://dx.doi. org/10.1016/j.chroma.2006.09.051

9. Ballesteros, O.; Zafra, A.; Navalon, A. & Vilchez, J. L. - J. Chromatogr. A, 1121, p.154 (2006). PMid:16690068. http://dx.doi.org/10.1016/j.chroma.2006.04.014

10. Sablayrolles, C.; Montrejaud-Vignoles, M. & Benanou, D. - J. Chromatogr. A, 1072, p.233 (2005). http://dx.doi. org/10.1016/j.chroma.2005.02.074

11. Cai, Y.-Q.; Jiang, G.-B.; Liu, J.-F. & Zhou, Q.-X. - Anal. Chim. Acta, 494, p.149 (2003). http://dx.doi.org/10.1016/j. aca.2003.08.006

12. Zhao, R.-S.; Wang, X.; Yuan, J.-P. & Lin, J.-M. - J. Chromatogr. A, 1183, p.15 (2008). PMid:18243227. http:// dx.doi.org/10.1016/j.chroma.2008.01.021

13. Liang, P.; Xu, J. & Li, Q. - Anal. Chimi. Acta, 609, p.53 (2008). PMid:18243873. http://dx.doi.org/10.1016/j. aca.2007.12.025

14. Jen, J.-F. & Liu, T.-Ch. - J. Chromatogr. A, 1130, p.28 (2006). PMid:16837003. http://dx.doi.org/10.1016/j. chroma.2006.06.029

15. Liang, P.; Li, Q.; Xu, J. & Du, D. - Chromatographia, 68, p.393 (2008). http://dx.doi.org/10.1365/s10337-008- 0744-x

16. Lopez-Jimenez, F.J.; Rubio, S. & Perez-Bendito, D. - Anal. Chimi. Acta, 551, p.142 (2005).

17. Jara, S.; Lysebo, C.; Greibrokk, T. & Lundanes, E. - Anal. Chimi. Acta, 407, p.165 (2000). http://dx.doi.org/10.1016/ S0003-2670(99)00829-6

18. Ito, R.; Seshimo, F.; Miura, N.; Kawaguchi, M.; Saito, K. & Nakazawa, H. - J. Pharma. Biomed. Analysis, 39, p.1036 (2005). PMid:16061340. http://dx.doi.org/10.1016/j. jpba.2005.06.016

19. Baker, J. K. - J. Pharma. Biomed. Analysis, 15, p.145 (1996). http://dx.doi.org/10.1016/0731-7085(96)01830-4

20. Penalver, A.; Pocurull, E.; Borrull, F. & Marce, R. M. - J. Chromatogr. A, 872, p.191 (2000). http://dx.doi. org/10.1016/S0021-9673(99)01284-4

21. Li, J. D.; Cai, Y. Q.; Shi, Y. L.; Mou, S. F. & Jiang, G. B. - Talanta, 74, p.498 (2008). PMid:18371667. http:// dx.doi.org/10.1016/j.talanta.2007.06.008

22. Prokupková, G.; Holadová, K.; Poustka, J. & Hajšlová, J. - Anal. Chimi. Acta, 457, p.211 (2002).

23. Cao, X. -L. - J. Chromatogr. A, 1178, p.231 (2008). PMid:18082753. http://dx.doi.org/10.1016/j. chroma.2007.11.095

24. Bago, B.; Martin, Y.; Mejia, G.; Broto-Puig, F.; Diaz- Ferrero, J.; Agut, M. & Comellas, L. – Chemosphere, 59, p.1191 (2005). PMid:15833494.

25. Aparicio, I.; Santos, J. L. & Alonso, E. - Anal. Chimi. Acta, 584, p.455 (2007). PMid:17386637. http://dx.doi. org/10.1016/j.aca.2006.11.039

26. Czaplicka, M. & Chmielarz, A. - J. Haz. Mat., 163, p.645 (2009). PMid:18718712. http://dx.doi.org/10.1016/j. jhazmat.2008.07.010
5883719c7f8c9d0a0c8b49a7 polimeros Articles
Links & Downloads

Polímeros: Ciência e Tecnologia

Share this page
Page Sections