Screening of Phthalates in Polymer Materials by Pyrolysis GC/MS

Maruyama, Fumitaka; Fujimaki, Shigehiko; Sakamoto, Yuki; Kudo, Yukihiko; Miyagawa, Haruhiko

doi:10.2116/analsci.31.3

Cited by 19 publications

(18 citation statements)

References 4 publications

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“…Specifically, pyrolysis gas chromatography mass spectrometry (Py-GC–MS) was proposed as a way of screening certain phthalates as an alternative to conventional GC–MS. The proposed screening method employs direct sample injection and thermal extraction in the GC–MS analysis and does not require any complicated pre-treatment using organic solvents [ 17 , 18 , 19 , 20 ]. Py-GC–MS was originally used for identifying polymers from the pattern of peaks obtained in a chromatogram [ 21 , 22 , 23 ].…”

Section: Introductionmentioning

confidence: 99%

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

Yanagisawa¹,

Kudo

Nakagawa

et al. 2018

Molecules

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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.

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Section: Introductionmentioning

confidence: 99%

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

Yanagisawa¹,

Kudo

Nakagawa

et al. 2018

Molecules

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“…The phthalate test method by TD–GC—MS has been standardized as part of the IEC62321 method through a sufficient verification process. Detailed validation data have been reported elsewhere [9,10,12].…”

Section: Methodsmentioning

confidence: 99%

“…A test method requiring only a small amount of sample was therefore desirable to avoid any disturbance in ongoing migration tests. Thermal desorption (TD)–GC–MS was employed as the most suitable test method to evaluate phthalate contaminant migration [8,9,10] because it allows direct injection of samples with a minimum amount (e.g., 0.5 mg) for the detection of phthalates at regulatory levels.…”

Section: Introductionmentioning

confidence: 99%

Evaluating Phthalate Contaminant Migration Using Thermal Desorption–Gas Chromatography–Mass Spectrometry (TD–GC–MS)

Ouchi¹,

Yanagisawa²,

Fujimaki³

2019

Polymers

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This study describes a methodology for evaluating regulatory levels of phthalate contamination. By collecting experimental data on short-term phthalate migration using thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS), the migration of di(2-ethylhexyl) phthalate (DEHP) from polyvinyl chloride (PVC) to polyethylene (PE) was found to be expressed by the Fickian approximation model, which was originally proposed for solid (PVC)/liquid (solvent) migration of phthalates. Consequently, good data correlation was obtained using the Fickian approximation model with a diffusion coefficient of 4.2 × 10−12 cm2/s for solid (PVC)/ solid (PE) migration of DEHP at 25 °C. Results showed that temporary contact with plasticized polymers under a normal, foreseeable condition may not pose an immediate risk of being contaminated by phthalates at regulatory levels. However, as phthalates are small organic molecules designed to be dispersed in a variety of polymers as plasticizers at a high compounding ratio, the risk of migration-related contamination can be high in comparison with other additives, especially under high temperatures. With these considerations in mind, the methodology for examining regulatory levels of phthalate contamination using TD–GC–MS has been successfully demonstrated from the viewpoint of its applicability to solid (PVC)/solid (PE) migration of phthalates.

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“…The instrument settings were the same as those used in previous studies. 6,7 Synthesis of fluorescein from phthalates The phthalates were hydrolyzed to phthalic acid with sodium hydroxide and dehydrated using the dry thermo unit. After dehydration, fluorescein was synthesized by the selective reaction between phthalic anhydride and resorcinol with concentrated sulfuric acid as the catalyst.…”

Section: Instrumentationmentioning

confidence: 99%

“…5 The Py/TD-GC-MS method enables solvent-free direct sample injection without the need for complicated pretreatment procedures. [6][7][8] However, in an actual business scenario, a simple screening method that enables manufacturers to verify the ingredients of various materials on a daily basis is needed. For example, Fourier transform infrared (FTIR) spectroscopy enables the nondestructive analysis of phthalates, 9,10 but the detection limits are usually considerably higher than the regulatory criteria and FTIR spectroscopy cannot be used for performing compliance assessment.…”

Section: Introductionmentioning

confidence: 99%