Hyphenated Techniques

Falkenhagen, Jana; Weidner, Steffen M.

doi:10.1002/9783527641826.ch7

Cited by 3 publications

(2 citation statements)

References 102 publications

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“…In the 21st century, developments in software and hardware for the better coupling of several techniques led to innovative approaches using, for example, Ion Mobility Spectrometry coupled with Mass Spectroscopy (IMS-MS). Two-dimensional chromatographic setups have also been studied specifically for polymer characterization, providing simultaneous information regarding molar mass and chemical functionality, such as co-polymer composition ratio and polymer chain end-groups.This has been achieved by taking advantage of liquid adsorption chromatography at critical conditions (LACCC), obtaining separation in polymer chain functionalization and combining it with size exclusion chromatography (SEC), which separates molecules by molar weight [1,3,23,24].…”

Section: Introductionmentioning

confidence: 99%

“…In such cases, the common overlapping of the oligomer derivative is visible only by analyzing the MS spectra. As another example, a simple homopolymer with average molecular mass (M n ) = 3.3 × 10 3 g•mol −1 and polydispersity (Pd) of 1.27 will present 60 distinct masses, without considering isomer analogs [22,24]. In the last two decades, significant development in custom scripts for MS data interpretation has been achieved.…”

Section: Introductionmentioning

confidence: 99%

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Polypy: A Framework to Interpret Polymer Properties from Mass Spectroscopy Data

Vlnieska,

Khanda,

Gilshtein

et al. 2024

Polymers

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Mass spectroscopy (MS) is a robust technique for polymer characterization, and it can provide the chemical fingerprint of a complete sample regarding polymer distribution chains. Nevertheless, polymer chemical properties such as polydispersity (Pd), average molecular mass (Mn), weight average molecular mass (Mw) and others are not determined by MS, as they are commonly characterized by gel permeation chromatography (GPC). In order to calculate polymer properties from MS, a Python script was developed to interpret polymer properties from spectroscopic raw data. Polypy script can be considered a peak detection and area distribution method, and represents the result of combining the MS raw data filtered using Root Mean Square (RMS) calculation with molecular classification based on theoretical molar masses. Polypy filters out areas corresponding to repetitive units. This approach facilitates the identification of the polymer chains and calculates their properties. The script also integrates visualization graphic tools for data analysis. In this work, aryl resin (poly(2,2-bis(4-oxy-(2-(methyloxirane)phenyl)propan) was the study case polymer molecule, and is composed of oligomer chains distributed mainly in the range of dimers to tetramers, in some cases presenting traces of pentamers and hexamers in the distribution profile of the oligomeric chains. Epoxy resin has Mn = 607 Da, Mw = 631 Da, and polydispersity (Pd) of 1.015 (data given by GPC). With Polypy script, calculations resulted in Mn = 584.42 Da, Mw = 649.29 Da, and Pd = 1.11, which are consistent results if compared with GPC characterization. Additional information, such as the percentage of oligomer distribution, was also calculated and for this polymer matrix it was not possible to retrieve it from the GPC method. Polypy is an approach to characterizing major polymer chemical properties using only MS raw spectra, and it can be utilized with any MS raw data for any polymer matrix.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Polypy: A Framework to Interpret Polymer Properties from Mass Spectroscopy Data

Vlnieska,

Khanda,

Gilshtein

et al. 2024

Polymers

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Semifluorinated PMMA Block Copolymers: Synthesis, Nanostructure, and Thin Film Properties

Pospiech

Jehnichen

Eckstein

et al. 2017

Macro Chemistry & Physics

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Diblock copolymers (BCP) with poly(methyl methacrylate) and poly(1H,1H,2H,2H-perfluorodecyl methacrylate) (PsfMA) blocks prepared by anionic polymerization in tetrahydrofuran at −78 °C and atom transfer radical polymerization (ATRP) at 60 °C, respectively, with stepwise varied composition over a wide range in the phase diagram are compared with respect to synthesis limits, phase separation behavior in bulk, and properties of thin films. Both methods yield BCPs with low dispersity (1.1-1.2) at molar masses below 100 kg mol −1 . Higher semifluorinated contents can be achieved by ATRP in 1,3-bis(trifluoromethyl)benzene which ensured solubility of PsfMA. BCPs obtained by anionic polymerization show a more distinct phase separation, that is, more regular nanostructures. Additionally, self-organization of the semifluorinated side chains occurs generating smectic layers which alters in turn the BCP morphology especially in thin films as compared to non-semifluorinated BCP. All BCPs show amphiphilic behavior and form micelles in organic solvents which can be used to deposit nanoparticles. periodic structures is the low dispersity − D of both blocks in the BCP which can mostly be achieved by employing controlled polymerization conditions. Although more and more methods of controlled polymerizations appear, such as light-controlled polymerization of methacrylates to BCP in a one-pot procedure, [7] visible-light polymerization from hyperbranched poly(methyl methacrylate) macroinitiators catalyzed by Mn 2 (CO) 10 , [8] combination of polymerization and click chemistry, and many others, and taking the variety of BCP syntheses results reported into account, standard techniques for BCP synthesis as anionic polymerization and atom transfer radical polymerization (ATRP) still appear to be the most successful with regards to achieving low dispersity and high control over the structure and molar mass.In this study, we want to compare diblock copolymers with a poly(methyl methacrylate) (PMMA) and a

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