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Molecules 2018, 23(4), 728; https://doi.org/10.3390/molecules23040728

Simultaneous Screening of Major Flame Retardants and Plasticizers in Polymer Materials Using Pyrolyzer/Thermal Desorption Gas Chromatography Mass Spectrometry (Py/TD–GC–MS)

1
Consumer & Retail Service Division, SGS Japan Inc. YBP East Tower 12F, 134 Godo-cho, Hodogaya-ku, Yokohama 240-0005, Japan
2
Analytical & Measuring Instrument Division, Shimadzu Corporation, 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 640-8511, Japan
*
Author to whom correspondence should be addressed.
Received: 8 February 2018 / Revised: 14 March 2018 / Accepted: 20 March 2018 / Published: 22 March 2018
(This article belongs to the Special Issue Functional Molecular Materials)
Full-Text   |   PDF [8192 KB, uploaded 3 May 2018]   |  

Abstract

This study was conducted with the aim of achieving the simultaneous screening of various additives in polymer materials by utilizing a solvent-free pyrolyzer/thermal desorption gas chromatography mass spectrometry (Py/TD-GC–MS) method. As a first step to achieve this goal, simultaneous screening has been examined by selecting major substances representing plasticizers and flame retardants, such as short chain chlorinated paraffins (SCCPs), decabromodiphenyl ether (DecaBDE), hexabromocyclododecane (HBCDD), and di(2-ethylhexyl) phthalate (DEHP). A quantitative MS analysis was performed to check for the peak areas and sensitivities. Since Py/TD-GC–MS is fraught with the risk of thermal degradation of the sample, temperatures during the analytical process were finely tuned for securing reliable results. The instrumental sensitivity was confirmed by the S/N ratio on each component. The detection limits of all components were less than 50 mg/kg, which are sufficiently lower than the regulatory criteria. With regard to reproducibility, a relative standard deviation (RSD) of about 5% was confirmed by employing a spike recovery test on a polystyrene polymer solution containing mixed standard solution (ca. 1000 mg/kg). In conclusion, the results obtained in this study indicate that Py/TD-GC–MS is applicable for the screening of major flame retardants and plasticizers in real samples with sufficient reproducibility at regulatory levels. View Full-Text
Keywords: additives; short chain chlorinated paraffins; decabromodiphenyl ether; hexabromocyclododecane; di(2-ethylhexyl) phthalate; pyrolysis; thermal desorption; plasticizer; HBCDD; DEHP additives; short chain chlorinated paraffins; decabromodiphenyl ether; hexabromocyclododecane; di(2-ethylhexyl) phthalate; pyrolysis; thermal desorption; plasticizer; HBCDD; DEHP
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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    Description: Supplementary material Table S1. Summary of experimental parameters; sensitivity, correlation coefficient (R2) and relative standard deviation (RSD) at 1000 mg/kg SCCPs solution. Supplementary material Table S2. In accordance with the provisions of IEC62321-8 (student’s t-statistic with 99% confidence,), detection limits were determined by multiplying t (n-1, risk rate) =3.14 (risk rate = 0.01) to each the standard deviation. Supplementary material Table S3. LODs obtained by spiking mixed standard (ca. 200 mg/kg) to PS polymer matrix (0.5 mg). In accordance with the provisions of student’s t-statistic with 99% confidence, LODs were determined by multiplying t(n-1, α) =4.54 (α= 0.01) to each the standard deviation of 4 repeated measurements.
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Yanagisawa, H.; Kudo, Y.; Nakagawa, K.; Miyagawa, H.; Maruyama, F.; Fujimaki, S. Simultaneous Screening of Major Flame Retardants and Plasticizers in Polymer Materials Using Pyrolyzer/Thermal Desorption Gas Chromatography Mass Spectrometry (Py/TD–GC–MS). Molecules 2018, 23, 728.

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