Analysis of modified polyamide 6.6 using coupled liquid chromatography and MALDI–TOF–mass spectrometry

Weidner, Steffen M.; Just, U.; Wittke, Wolfgang; Rittig, Frank; Gruber, Freddy; Friedrich, J.

doi:10.1016/j.ijms.2004.08.013

Cited by 21 publications

(22 citation statements)

References 8 publications

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“…polyamides, polyacetales or aromatic polyester, could be investigated by means of SEC using 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) in combination with trifluoroacetate salts as solvent. [12][13][14] Verreck et al described an application of this method for random copolymers consisting of VP and VAc [poly(VP-ranVAc)] with average molar masses between 45 and 70 kDa. [15] Therefore, this procedure was applied for our investigations.…”

Section: Determination Of Molar Masses and Mass Distributions By Sizementioning

confidence: 99%

Characterization of New Amphiphilic Block Copolymers of N‐Vinyl Pyrrolidone and Vinyl Acetate, 1 – Analysis of Copolymer Composition, End Groups, Molar Masses and Molar Mass Distributions

Fandrich

Falkenhagen

Weidner

et al. 2010

Macro Chemistry & Physics

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New amphiphilic block copolymers consisting of N‐vinyl pyrrolidone and vinyl acetate were synthesized via controlled radical polymerization using a reversible addition/fragmentation chain transfer (RAFT)/macromolecular design via the interchange of xanthates (MADIX) system. The synthesis was carried out in 1,4‐dioxane as process solvent. In order to get conclusions on the mechanism of the polymerization the molecular structure of formed copolymers was analysed by means of different analytical techniques. 13C NMR spectroscopy was used for the determination of the monomer ratios. End groups were analysed by means of matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry. This technique was also used to determine possible fragmentations of the RAFT end groups. By means of a combination of size exclusion chromatography, 13C NMR and static light scattering molar mass distributions and absolute molar masses could be analysed. The results clearly show a non‐ideal RAFT mechanism.

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Section: Determination Of Molar Masses and Mass Distributions By Sizementioning

confidence: 99%

Characterization of New Amphiphilic Block Copolymers of N‐Vinyl Pyrrolidone and Vinyl Acetate, 1 – Analysis of Copolymer Composition, End Groups, Molar Masses and Molar Mass Distributions

Fandrich

Falkenhagen

Weidner

et al. 2010

Macro Chemistry & Physics

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“…Weidner et al reported the MALDI-TOF analysis of modified PA 6.6. [13] Besides cyclic species (which are formed by inter-or intramolecular condensation), the spectra of unmodified PA 6.6 show various linear structures. Species with free amino and free carboxylic acid end groups were detected as well as species with only amino end groups (NH 2 -PA-NH 2 ) or species with only carboxylic acid functions (HOOC-PA-COOH).…”

Section: Introductionmentioning

confidence: 99%

MALDI‐TOF MS Investigations of Polyamides Synthesized in Autoclave and Microwave Assisted Processes

Nothdurft

Bode

Schmidt‐Naake

2009

Macromolecular Symposia

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Summary: Due to their excellent physical and chemical properties polyamides (PA) are used in many industrial processes. The most common products are the aliphatic polyamides synthesized by a conventional melt-polycondensation method of AH-salt in an autoclave. High temperatures, high pressure and long reaction times are necessary. On the other hand the polyamide synthesis can conducted as solution polycondensation in a microwave oven. Moreover the higher heating efficiency of microwave irradiation reduces the reaction time to about 20 minutes. The main focus of this study lies on the end group analysis by MALDI-TOF MS (matrix assisted laser desorption/ionization time of flight mass spectrometry) of aliphatic polyamides produced by autoclave -as well as microwave assisted synthesis by AABB-type condensation. The results show differences in the end group formation depending on the chosen reaction conditions. In case of following modification or protecting group chemistry, it is of course important to know the kind of end groups of the polyamide.

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“…Another useful approach is the combination of a selective chromatographic technique with a powerful spectroscopic method like NMR spectroscopy [1][2][3][4][5] or matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). [6,7] There are numerous selective modes for the liquid chromatography (LC) of polymers, including liquid chromatography at the critical point of adsorption (LCCC) [8][9][10] and isocratic or gradient polymer elution chromatography (GPEC). [11,12] Using these techniques, polymers can be separated selectively with regard to chemical composition or functionality, as it has been shown for macromonomers, random and block copolymers, and polymer blends.…”

Section: Introductionmentioning

confidence: 99%

“…As for LC in HFIP mobile phases, there are only a few applications described in the literature so far. [7,19,20] With regards to performance polymers, only a few HPLC or 2D applications are known. [22] Examples are polyamide 6 [19] and polyamide 6.6, [7,20] polycarbonates, [23] and polyesters.…”

Section: Introductionmentioning

confidence: 99%

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Structure Determination of Polyacetals by Liquid Chromatography and Hyphenated Techniques

Rittig

Fandrich

Urtel

et al. 2006

Macro Chemistry & Physics

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Summary: The structure of polyacetal copolymers with respect to their end groups is investigated. Several techniques, such as liquid chromatography, MALDI‐TOF MS, IR and NMR spectroscopy, as well as combined techniques like 2D chromatography have been applied. Cyclic oligomers and polymers with formyl, hydroxy, and aliphatic end groups are identified. 2D chromatography shows that all the separated species are homogenously distributed with respect to their molar mass.2D chromatograms of sample F97B3.magnified image2D chromatograms of sample F97B3.

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Analysis of modified polyamide 6.6 using coupled liquid chromatography and MALDI–TOF–mass spectrometry

Cited by 21 publications

References 8 publications

Characterization of New Amphiphilic Block Copolymers of N‐Vinyl Pyrrolidone and Vinyl Acetate, 1 – Analysis of Copolymer Composition, End Groups, Molar Masses and Molar Mass Distributions

Characterization of New Amphiphilic Block Copolymers of N‐Vinyl Pyrrolidone and Vinyl Acetate, 1 – Analysis of Copolymer Composition, End Groups, Molar Masses and Molar Mass Distributions

MALDI‐TOF MS Investigations of Polyamides Synthesized in Autoclave and Microwave Assisted Processes

Structure Determination of Polyacetals by Liquid Chromatography and Hyphenated Techniques

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