Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry
The international analytical standard IEC62321–8 specifies a pyrolyzer/thermal desorption-gas chromatography-mass spectrometry (Py/TD-GC/MS) method of screening seven phthalate esters in polymers that requires an analysis time of 30 min. This article describes a new, high-speed method that dramatica...
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| Format: | Article |
| Language: | English |
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Elsevier
2022-11-01
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| Series: | Journal of Chromatography Open |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2772391722000214 |
| _version_ | 1811187903910379520 |
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| author | Yukihiko Kudo Xue Chu Koki Tanaka Tomohiro Uchimura |
| author_facet | Yukihiko Kudo Xue Chu Koki Tanaka Tomohiro Uchimura |
| author_sort | Yukihiko Kudo |
| collection | DOAJ |
| description | The international analytical standard IEC62321–8 specifies a pyrolyzer/thermal desorption-gas chromatography-mass spectrometry (Py/TD-GC/MS) method of screening seven phthalate esters in polymers that requires an analysis time of 30 min. This article describes a new, high-speed method that dramatically reduces this analysis time to about 12 min with a method detection limit (MDL) under 30 mg/kg for all phthalate esters. When this high-speed method was used to analyze phthalate ester-containing reference materials of various base polymers, the phthalate ester recovery rates ranged from 92 to 115%. The conventional method described in IEC62321–8 and this high-speed method were also used to analyze real samples and reference materials (24 samples in total) to evaluate equivalence between the two methods. Linear approximation of a scatter plot of quantitative results obtained by both methods produced a regression line that showed good correlation between the methods with a slope of 1.0326 and a coefficient of determination (R2) of 0.9699. A Bland-Altman plot was also used to analyze the concentration range under 2000 mg/kg, which is near the phthalate ester level restricted by the RoHS (Restriction of the use of certain Hazardous Substances in electrical and electronic equipment) Directive (1000 mg/kg) and important for screening outcomes. As a result, the bias in the difference between the two methods was +20 mg/kg, the 95% confidence interval limits of agreement were -134 mg/kg and +175 mg/kg, and no fixed bias or proportional bias was observed. These findings indicate that the high-speed method is equivalent to the conventional method and can be used to screen for phthalate esters. |
| first_indexed | 2024-04-11T14:11:25Z |
| format | Article |
| id | doaj.art-81387350660945e8b1d5a1b6cb7f44c4 |
| institution | Directory Open Access Journal |
| issn | 2772-3917 |
| language | English |
| last_indexed | 2024-04-11T14:11:25Z |
| publishDate | 2022-11-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Journal of Chromatography Open |
| spelling | doaj.art-81387350660945e8b1d5a1b6cb7f44c42022-12-22T04:19:42ZengElsevierJournal of Chromatography Open2772-39172022-11-012100050Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometryYukihiko Kudo0Xue Chu1Koki Tanaka2Tomohiro Uchimura3Analytical & Measuring Instrument Division, Shimadzu Corporation, 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 640-8511, Japan; Department of Materials Science and Engineering, Graduate School of Engineering, University of Fukui, 3-9-1, Bunkyo, Fukui 910-8507, Japan; Corresponding author at: Analytical & Measuring Instrument Division, Shimadzu Corporation, 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 640-8511, Japan.Analytical & Measuring Instrument Division, Shimadzu Corporation, 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 640-8511, JapanAnalytical & Measuring Instrument Division, Shimadzu Corporation, 1 Nishinokyo Kuwabara-cho, Nakagyo-ku, Kyoto 640-8511, JapanDepartment of Materials Science and Engineering, Graduate School of Engineering, University of Fukui, 3-9-1, Bunkyo, Fukui 910-8507, JapanThe international analytical standard IEC62321–8 specifies a pyrolyzer/thermal desorption-gas chromatography-mass spectrometry (Py/TD-GC/MS) method of screening seven phthalate esters in polymers that requires an analysis time of 30 min. This article describes a new, high-speed method that dramatically reduces this analysis time to about 12 min with a method detection limit (MDL) under 30 mg/kg for all phthalate esters. When this high-speed method was used to analyze phthalate ester-containing reference materials of various base polymers, the phthalate ester recovery rates ranged from 92 to 115%. The conventional method described in IEC62321–8 and this high-speed method were also used to analyze real samples and reference materials (24 samples in total) to evaluate equivalence between the two methods. Linear approximation of a scatter plot of quantitative results obtained by both methods produced a regression line that showed good correlation between the methods with a slope of 1.0326 and a coefficient of determination (R2) of 0.9699. A Bland-Altman plot was also used to analyze the concentration range under 2000 mg/kg, which is near the phthalate ester level restricted by the RoHS (Restriction of the use of certain Hazardous Substances in electrical and electronic equipment) Directive (1000 mg/kg) and important for screening outcomes. As a result, the bias in the difference between the two methods was +20 mg/kg, the 95% confidence interval limits of agreement were -134 mg/kg and +175 mg/kg, and no fixed bias or proportional bias was observed. These findings indicate that the high-speed method is equivalent to the conventional method and can be used to screen for phthalate esters.http://www.sciencedirect.com/science/article/pii/S2772391722000214PyrolyzerThermal desorptionGC/MSPhthalate estersScreeningHigh-speed analysis |
| spellingShingle | Yukihiko Kudo Xue Chu Koki Tanaka Tomohiro Uchimura Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry Journal of Chromatography Open Pyrolyzer Thermal desorption GC/MS Phthalate esters Screening High-speed analysis |
| title | Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry |
| title_full | Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry |
| title_fullStr | Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry |
| title_full_unstemmed | Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry |
| title_short | Evaluation of the effectiveness of a high-speed method of screening phthalate esters in polymers using pyrolyzer/thermal desorption–gas chromatography-mass spectrometry |
| title_sort | evaluation of the effectiveness of a high speed method of screening phthalate esters in polymers using pyrolyzer thermal desorption gas chromatography mass spectrometry |
| topic | Pyrolyzer Thermal desorption GC/MS Phthalate esters Screening High-speed analysis |
| url | http://www.sciencedirect.com/science/article/pii/S2772391722000214 |
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