Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection)
The aim of this work was to develop a method to comprehensively characterize extracts from polyamide 11 powder samples used in the laser sintering process. Firstly, high resolution mass spectrometry was applied to identify low molecular compounds in the material. Secondly, by means of an inverse gra...
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doaj-250e3c9db22a484fa161a20882a0538e2021-06-25T04:50:57ZengElsevierTalanta Open2666-83192021-08-013100023Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection)Beate Scherer0Frank-Michael Matysik1BMW AG, Dingolfing, Germany; Department of Chemistry and Pharmacy, University of Regensburg, Regensburg, GermanyDepartment of Chemistry and Pharmacy, University of Regensburg, Regensburg, Germany; Corresponding author at: University of Regensburg, Department of Chemistry and Pharmacy, 93040 Regensburg, Germany.The aim of this work was to develop a method to comprehensively characterize extracts from polyamide 11 powder samples used in the laser sintering process. Firstly, high resolution mass spectrometry was applied to identify low molecular compounds in the material. Secondly, by means of an inverse gradient high-performance liquid chromatography (HPLC) in combination with a triple detection system consisting of a diode array detector (DAD), a mass spectrometer (MS), and a charged aerosol detector (CAD), a method was established to determine the amount of monomer and oligomers up to the linear tetramer and cyclic pentamer. Furthermore, the oxidation stabilizer identified as Irganox 1098 was determined. The DAD was utilized for the quantification of the UV-active oxidation stabilizer. Thus, to be able to extract the low molecular weight compounds, various protocols were studied and finally accelerated solvent extraction was used. As there is a lack of commercial standards of polyamide 11 related oligomers, these compounds were detected with the CAD, taking advantage of its uniform response behavior in conjunction with an inverse gradient HPLC protocol. In addition, the MS was utilized as a qualitative detector for peak identification. The information regarding low molecular weight compounds are required as the powder is subject to the thermal loading of the sintering process, which influences the composition of the low molecular weight compounds. Thus, the method was applied to new and oven-aged polyamide 11 samples. Finally, it was possible to monitor the change of low molecular weight compounds in stressed polyamide 11 powder samples.http://www.sciencedirect.com/science/article/pii/S2666831920300230Triple detection systemCharged aerosol detectionInverse gradientPolymer sample extractionPolyamide 11Oligomers |
collection |
DOAJ |
language |
English |
format |
Article |
sources |
DOAJ |
author |
Beate Scherer Frank-Michael Matysik |
spellingShingle |
Beate Scherer Frank-Michael Matysik Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) Talanta Open Triple detection system Charged aerosol detection Inverse gradient Polymer sample extraction Polyamide 11 Oligomers |
author_facet |
Beate Scherer Frank-Michael Matysik |
author_sort |
Beate Scherer |
title |
Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
title_short |
Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
title_full |
Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
title_fullStr |
Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
title_full_unstemmed |
Investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer Irganox 1098 by utilizing inverse gradient HPLC in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
title_sort |
investigations of polymer samples of polyamide 11 concerning the content of monomer, oligomers, and the oxidation stabilizer irganox 1098 by utilizing inverse gradient hplc in combination with a triple detection system (diode array detection/mass spectrometry/charged aerosol detection) |
publisher |
Elsevier |
series |
Talanta Open |
issn |
2666-8319 |
publishDate |
2021-08-01 |
description |
The aim of this work was to develop a method to comprehensively characterize extracts from polyamide 11 powder samples used in the laser sintering process. Firstly, high resolution mass spectrometry was applied to identify low molecular compounds in the material. Secondly, by means of an inverse gradient high-performance liquid chromatography (HPLC) in combination with a triple detection system consisting of a diode array detector (DAD), a mass spectrometer (MS), and a charged aerosol detector (CAD), a method was established to determine the amount of monomer and oligomers up to the linear tetramer and cyclic pentamer. Furthermore, the oxidation stabilizer identified as Irganox 1098 was determined. The DAD was utilized for the quantification of the UV-active oxidation stabilizer. Thus, to be able to extract the low molecular weight compounds, various protocols were studied and finally accelerated solvent extraction was used. As there is a lack of commercial standards of polyamide 11 related oligomers, these compounds were detected with the CAD, taking advantage of its uniform response behavior in conjunction with an inverse gradient HPLC protocol. In addition, the MS was utilized as a qualitative detector for peak identification. The information regarding low molecular weight compounds are required as the powder is subject to the thermal loading of the sintering process, which influences the composition of the low molecular weight compounds. Thus, the method was applied to new and oven-aged polyamide 11 samples. Finally, it was possible to monitor the change of low molecular weight compounds in stressed polyamide 11 powder samples. |
topic |
Triple detection system Charged aerosol detection Inverse gradient Polymer sample extraction Polyamide 11 Oligomers |
url |
http://www.sciencedirect.com/science/article/pii/S2666831920300230 |
work_keys_str_mv |
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1721360457633103872 |