New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis
In this work a series of thermoresistant polysiloxanes containing silarylene units and macrocyclic silicon phthalocyanine (Pc) units (PS-1 – PS-6) were synthesized. The Pc is linked to the polymer chain through a siloxane central group, which has two covalent bonds with two nitrogen atoms of the mac...
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Elsevier
2025-05-01
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| Series: | Journal of Chromatography Open |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2772391725000192 |
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| author | Mihaela-Liliana Ţînţaş Valérie Peulon-Agasse Marco Piparo Pierre Giusti Jean-Maurice Mallet Pascal Cardinael |
| author_facet | Mihaela-Liliana Ţînţaş Valérie Peulon-Agasse Marco Piparo Pierre Giusti Jean-Maurice Mallet Pascal Cardinael |
| author_sort | Mihaela-Liliana Ţînţaş |
| collection | DOAJ |
| description | In this work a series of thermoresistant polysiloxanes containing silarylene units and macrocyclic silicon phthalocyanine (Pc) units (PS-1 – PS-6) were synthesized. The Pc is linked to the polymer chain through a siloxane central group, which has two covalent bonds with two nitrogen atoms of the macrocycle and two covalent bonds with the polymer chain. The sol‒gel method led to the formation of polymeric chains with a random arrangement of monomers and OH-terminated chains. Thermogravimetric analyses revealed that the polymers are stable at high temperatures exhibiting, with a weight loss of 10 % between 384 and 442 °C during heating.Coated as stationary phases for gas chromatography, polymers PS-1, PS-2 and PS-5 showed good film-forming ability. The columns prepared with PS-1 and PS-5 had 3300 and 3800 plates m−1, respectively, as determined using pentadecane at 130 °C for fused silica capillary columns with an internal diameter of 250 µm, a film thickness of 0.25 µm and a length of 10 m. Polarity was estimated as moderate polarity (Rohrschneider–McReynolds constants were between 841 and 916) and stationary phases can achieve very good separation of Grob’s mixture, polycyclic aromatic hydrocarbons and essential oils. In addition, the columns provided excellent high temperature stability with very low bleeding (17.0 pA at 420 °C). Repeated injections of high boiling analytes revealed that PS-1 is the most stable stationary phase at very high temperatures, as the smallest decrease of retention times (9.2 s) were observed after 50 successive injections (temperature program from 40 °C (hold 3 min) at 7 °C/min to 420 °C (hold 2 min). Moreover, it has been demonstrated that PS-1 is more stable than commercial high-temperature columns such as ZB-XLB-HT and ZB-35HT (35 % phenyl/65 % dimethylpolysiloxane) from Phenomenex®. |
| format | Article |
| id | doaj-art-fe4ad73b00a441e498da43968b697a59 |
| institution | OA Journals |
| issn | 2772-3917 |
| language | English |
| publishDate | 2025-05-01 |
| publisher | Elsevier |
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| series | Journal of Chromatography Open |
| spelling | doaj-art-fe4ad73b00a441e498da43968b697a592025-08-20T02:13:40ZengElsevierJournal of Chromatography Open2772-39172025-05-01710022110.1016/j.jcoa.2025.100221New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysisMihaela-Liliana Ţînţaş0Valérie Peulon-Agasse1Marco Piparo2Pierre Giusti3Jean-Maurice Mallet4Pascal Cardinael5Univ Rouen Normandie, FR3038, SMS, UR3233, F-76000 Rouen, FranceUniv Rouen Normandie, FR3038, SMS, UR3233, F-76000 Rouen, FranceOne Tech – R&D – Downstream Processes & Polymers, TRTG - TotalEnergies Research & Technology Gonfreville, Harfleur - France; International Joint Laboratory - iC2MC, Complex Matrices Molecular Characterization, TRTG, Harfleur, FranceOne Tech – R&D – Downstream Processes & Polymers, TRTG - TotalEnergies Research & Technology Gonfreville, Harfleur - France; International Joint Laboratory - iC2MC, Complex Matrices Molecular Characterization, TRTG, Harfleur, FranceChimie Physique, Chimie du Vivant (CPCV), Département de chimie, École Normale Supérieure, PSL University, Sorbonne Université, CNRS, 75005 Paris, FranceUniv Rouen Normandie, FR3038, SMS, UR3233, F-76000 Rouen, France; Corresponding author at: Université de Rouen Normandie, SMS UR3233, Emile Blondel 76821 Mon-Saint-Aignan Cedex, France.In this work a series of thermoresistant polysiloxanes containing silarylene units and macrocyclic silicon phthalocyanine (Pc) units (PS-1 – PS-6) were synthesized. The Pc is linked to the polymer chain through a siloxane central group, which has two covalent bonds with two nitrogen atoms of the macrocycle and two covalent bonds with the polymer chain. The sol‒gel method led to the formation of polymeric chains with a random arrangement of monomers and OH-terminated chains. Thermogravimetric analyses revealed that the polymers are stable at high temperatures exhibiting, with a weight loss of 10 % between 384 and 442 °C during heating.Coated as stationary phases for gas chromatography, polymers PS-1, PS-2 and PS-5 showed good film-forming ability. The columns prepared with PS-1 and PS-5 had 3300 and 3800 plates m−1, respectively, as determined using pentadecane at 130 °C for fused silica capillary columns with an internal diameter of 250 µm, a film thickness of 0.25 µm and a length of 10 m. Polarity was estimated as moderate polarity (Rohrschneider–McReynolds constants were between 841 and 916) and stationary phases can achieve very good separation of Grob’s mixture, polycyclic aromatic hydrocarbons and essential oils. In addition, the columns provided excellent high temperature stability with very low bleeding (17.0 pA at 420 °C). Repeated injections of high boiling analytes revealed that PS-1 is the most stable stationary phase at very high temperatures, as the smallest decrease of retention times (9.2 s) were observed after 50 successive injections (temperature program from 40 °C (hold 3 min) at 7 °C/min to 420 °C (hold 2 min). Moreover, it has been demonstrated that PS-1 is more stable than commercial high-temperature columns such as ZB-XLB-HT and ZB-35HT (35 % phenyl/65 % dimethylpolysiloxane) from Phenomenex®.http://www.sciencedirect.com/science/article/pii/S2772391725000192Stationary phasesSilarylenePhthalocyanine polysiloxanesHigh-temperatureGas chromatography |
| spellingShingle | Mihaela-Liliana Ţînţaş Valérie Peulon-Agasse Marco Piparo Pierre Giusti Jean-Maurice Mallet Pascal Cardinael New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis Journal of Chromatography Open Stationary phases Silarylene Phthalocyanine polysiloxanes High-temperature Gas chromatography |
| title | New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis |
| title_full | New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis |
| title_fullStr | New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis |
| title_full_unstemmed | New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis |
| title_short | New silicon phthalocyanine-containing polysiloxanes as stationary phases for high-temperature gas chromatography analysis |
| title_sort | new silicon phthalocyanine containing polysiloxanes as stationary phases for high temperature gas chromatography analysis |
| topic | Stationary phases Silarylene Phthalocyanine polysiloxanes High-temperature Gas chromatography |
| url | http://www.sciencedirect.com/science/article/pii/S2772391725000192 |
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