Browse > Article
http://dx.doi.org/10.5806/AST.2012.25.3.178

Study on verification of various national standards regarding phthalate testing in industrial products  

Song, Moon-Hwan (Product Eco-testing Laboratory, Korea Institute of Industrial Technology)
Cho, Young-Dal (Product Eco-testing Laboratory, Korea Institute of Industrial Technology)
Choe, Eun-Kyung (Product Eco-testing Laboratory, Korea Institute of Industrial Technology)
Myoung, Young-Chan (Korean Agency for Technology and Standards)
Publication Information
Analytical Science and Technology / v.25, no.3, 2012 , pp. 178-189 More about this Journal
Abstract
As phthalates classified as toxic to reproduction category 2 and endocrine disrupting chemicals were more strictly regulated as Substances of Very High Concern (SVHC) for authorization in under EU REACH and considered as priority substances in RoHS II, standardization of phthalate testing method is now being proposed in IEC 62321 of IEC TC 111 and the 2nd revision of KS M 1991 is also finished. In order to assist standardization activities related to phthalating testing, solvent extraction part of existing national standards were compared and verified. Recovery of DEHP (diethylhexyl phthalate) from PVC (polyvinyl chloride) by Soxhlet extraction increased in the order of methanol, toluene, dichloromethane and hexane from 46.9% to 95.3% as measured by GC-MS. Optimum extraction time was verified to be 6 hours using hexane. Recovery of DBP (dibutyl phthalate), BBP (butylbenzyl phthalate), and DEHP from different matrixes such as PVC, nitro cellulose, ABS (acrylonitrile butadiene styrene). and EPDM(ethylene propylene diene monomer) rubber were evaluated to be more than 90% up to 99%. The detection limits of phthalates in solvent extraction followed by GC-MS analysis were 0.08~0.3 ${\mu}g/mL$ in solution and 8~30 mg/Kg in polymeric samples. GC-MS analyses of phthalates were carried out using different solvent extraction based on the EN 14372, ASTM D 7083, Japanese test method (MHLW 0906-4) and KS M 1991, proving that equivalent recoveries ranging from 98%~99% were obtained. DBP and DEHP were detected in three consumer products such as a child toy, a power cable and manicure with the amount of 22~1,910 mg/kg.
Keywords
phthalate testing; solvent extraction; recovery; GC-MS; Korea Standard; International Standard; polymeric materials; industrial products;
Citations & Related Records
Times Cited By KSCI : 3  (Citation Analysis)
연도 인용수 순위
1 http://echa.europa.eu/reach/authorisation_under_reach/authorisation_list_en.asp.
2 COM (2008) 809/4, "EU Commission's recast proposal for Directive 2002/95/EC", the European Parliament, 2008.
3 http://echa.europa.eu/reach/restriction/restrictions_under_consideration_en.asp
4 Korean Agency for Technology and Standards Announcement No. 2010-0259(2010.08.20), Republic of Korea.
5 "Oeko-Tex Standard 100", Ed.01/2011, Oeko-Tex International, Zuerich, 2011.
6 IEC 62321, IEC, Geneva. Switzerland, 2008.
7 Y. D. Cho, S. W. Byun, E. K. Choe and S. H. Kim, Clean Technol., 18(1), 1-13 (2012).   DOI   ScienceOn
8 http://www.chemsec.org/images/stories/2011/chemsec/SIN_List_2.0_all_378.pdf.
9 KS M 1991 : 2011, Determination of phthalates contents in polymer materials.
10 J. W. Kim, New Working Item Proposal, 13th Meeting of IEC TC 111 WG 3, Melbourne, October 26, 2011.
11 KS M 1991 : 2008, Determination of phthalates contents in plastic materials.
12 National Institute for Occupational Safety and Health (NIOSH), Manual of Analytical Method No. 5522, United States, 1998.
13 EN 14372, CEN(European Committee for Standardization), 2004.
14 Food Sanitation Publication No. 0904-4(Annex) (2010. 09. 06), Ministry of Health, Labour and Welfare, Japan.
15 ASTM D 2124-99, ASTM International, United States, 2004.
16 ASTM D 7083, ASTM International, United States, 2004.
17 Test method : CPSC-CH-1001-09.1, US Consumer Product Safety Commission, United States, 2009.
18 Method C-34, Health Canada, Canada, 2006.
19 Y. Y. Kang, S. K. Shin, J. S. Park, W.-i. Kim, J. W. Chun, H. J. Heo and S.-H. Koo, Anal. Sci. Technol., 23(4), 357-362 (2010).   DOI   ScienceOn
20 U.-S. Shin, H.-S. Ahn and H.-S. Shin, Anal. Sci. Technol., 15(5), 475-481 (2002).
21 S.-W. Myung, Y.-J. Chang, S.-H. Yoon, H.-W. Cho and M.-S. Kim, Anal. Sci. Technol., 15(4), 360-364 (2002).
22 AB 1108, California Toxic Toys Bill (2007.06.05), U.S.A.
23 S. Kim and H. Kim, 45th Conference of the Korean Soc. of Anal. Sci., Ramada Plaza Hotel, Jeju, 150 (2010).
24 M. H. Song, S. H. Son, Y. D. Cho and E. K. Choe, Clean Technol., 17(2), 124-133 (2011).
25 http://www.chemsec.org/images/stories/2011/chemsec/SIN_List_2.0_22_new_substances.pdf.
26 H. R. 4030, The Federal Hazardous Substances Act (2007.10.31), U.S.A.
27 Public Law 110-314 (H. R. 4040), Consumer Product Safety Improvement Act (2008.08.14), U.S.A.
28 Cosmetic Directive 76/768/EEC (2004.09.22), EU.
29 Food Sanitation Law : MHLW Notice No.370(1959), amended (Revision of Phthalate Requirements) (2010. 09. 06), Japan.
30 Canada Consumer Product Safety Act (2010.12.10), Canada.
31 Korean Agency for Technology and Standards Notification No. 2001-367(2001.07.10), Republic of Korea.
32 Korean Agency for Technology and Standards Notification No. 2007-523(2001.07.10), Republic of Korea.
33 Regulation (EC) No 1907/2006, REACH, the European Parliament and the Council of the European Union, 2006.
34 http://echa.europa.eu/chem_data/authorisation_process/candidate_list_table_en.asp.