Synthesis of heterotelechelic poly(ethylene glycol)s and their characterization by MALDI-TOF-MS

1999 ◽  
Vol 200 (6) ◽  
pp. 1363-1373 ◽  
Author(s):  
Nicolas Hans Völcker ◽  
Doris Klee ◽  
Martin Hanna ◽  
Hartwig Höcker ◽  
Jordi J. Bou ◽  
...  
Keyword(s):  
Ethylene Glycol ◽  
Poly Ethylene Glycol ◽  
Maldi Tof Ms ◽  
Maldi Tof ◽  
Poly Ethylene ◽  
Tof Ms

SEC/MALDI-TOF Mass spectrometry study of hydroxy-, carboxy- and methyl ester-terminated aliphatic polyesters

e-Polymers ◽  
2005 ◽  
Vol 5 (1) ◽  
Author(s):  
Slim Salhi ◽  
Martine Tessier ◽  
Jean-Claude Blais ◽  
Rachid El Gharbi ◽  
Alain Fradet
Keyword(s):  
Dimethyl Ester ◽  
Calibration Method ◽  
Size Exclusion ◽  
Aliphatic Polyesters ◽  
Maldi Tof Ms ◽  
Maldi Tof ◽  
Calibration Curves ◽  
End Groups ◽  
Poly Ethylene ◽  
Tof Ms

AbstractPoly(ethylene adipate) (PEA) and poly(ethylene dodecanedioate) (PED) with dicarboxy-, dihydroxy-, dimethyl ester- and hydroxy-carboxy end-groups were synthesized and characterized by 13C NMR and MALDI-TOF MS. Size-exclusion chromatography (SEC) fractions of these polyesters were analyzed by MALDI-TOF MS and used as standards to obtain SEC calibration curves leading to the absolute molar masses of the unfractionated polyesters. PEA and PED calibration curves were different from each other, but the same calibration curve was obtained for each type of polyester, irrespective of the nature of end-groups, showing the predominant role of the nature of repeating units on the hydrodynamic volume of oligoesters. The study also shows that the conventional SEC calibration method using polystyrene standards leads to a significant overestimation of polyester average molar masses.

MALDI−TOF MS and DIOS−MS Investigation of the Degradation and Discoloration of Poly(ethylene terephthalate)

2006 ◽  
Vol 39 (23) ◽  
pp. 7872-7881 ◽  
Author(s):  
Flaviu Calin Ladasiu Ciolacu ◽  
Namita Roy Choudhury ◽  
Naba Dutta ◽  
Nicolas H. Voelcker
Keyword(s):  
Ethylene Terephthalate ◽  
Maldi Tof Ms ◽  
Maldi Tof ◽  
Poly Ethylene Terephthalate ◽  
Poly Ethylene ◽  
Tof Ms

High Temperature Bulk Reaction between Poly(ethylene terephtalate) and Lactones: 1H NMR and SEC/MALDI-TOF MS Study

2004 ◽  
Vol 205 (5) ◽  
pp. 581-592 ◽  
Author(s):  
Delphine Tillier ◽  
Hervé Lefebvre ◽  
Martine Tessier ◽  
Jean-Claude Blais ◽  
Alain Fradet
Keyword(s):  
High Temperature ◽  
1H Nmr ◽  
Maldi Tof Ms ◽  
Maldi Tof ◽  
Bulk Reaction ◽  
Poly Ethylene ◽  
Tof Ms

scholarly journals Synthesis and MALDI-ToF characterization of dendronized poly(ethylene glycol)s

2013 ◽  
Vol 49 (spe) ◽  
pp. 45-55 ◽  
Author(s):  
Brittany K. Myers ◽  
Joanna E. Lapucha ◽  
Scott M. Grayson
Keyword(s):  
Ethylene Glycol ◽  
Poly Ethylene Glycol ◽  
Maldi Tof ◽  
Product Characterization ◽  
End Groups ◽  
Linear Poly ◽  
Mass Spectrometric Approach ◽  
Poly Ethylene ◽  
End Group

Well-defined hybrids of linear poly(ethylene glycol)s (PEGs) and dendritic polyesters were prepared via the dendronization of the alcohol end groups of the mono and difunctional linear PEGs. Though useful for rudimentary product characterization, GPC and NMR could not verify the overall structural purity of these linear-dendritic hybrids. On the other hand, the detailed data provided by MALDI-ToF mass spectrometry enabled confirmation of the high structural purity of the dendronized PEGs at each step of the dendronization procedure. The well-defined number of functionalities on these dendronized PEGs, renders them particularly useful for research in the biomedical sphere where functionality and purity are of the utmost importance. The MALDI-ToF mass spectrometric approach described herein represents a valuable technique for detailed monitoring of these dendronization reactions, as well as a variety of other polymer end group modifications.

scholarly journals A Facile Strategy for the High Yielding, Quantitative Conversion of Polyglycol End-Groups to Amines

Polymers ◽  
2021 ◽  
Vol 13 (9) ◽  
pp. 1403
Author(s):  
Jie Yan ◽  
Paula Facal Marina ◽  
Anton Blencowe
Keyword(s):  
Nmr Spectroscopy ◽  
Ethylene Glycol ◽  
Slight Reduction ◽  
Poly Ethylene Glycol ◽  
End Groups ◽  
Poly Ethylene ◽  
Poly Propylene ◽  
Work Up ◽  
End Group ◽  
Tof Ms

Amino end-group functionalised polyglycols are important intermediates in the synthesis of sophisticated polymeric architectures and biomaterials. Herein, we report a facile strategy for the end-group conversion of hydroxyl-terminated polyglycols to amino-terminated polyglycols in high isolated yields and with excellent end-group fidelity. Following traditional conversion of polyglycol hydroxyl end-groups to azides via the corresponding mesylate, reduction with zinc in the presence of ammonium chloride afforded a range of amino end-group functionalised poly(ethylene glycol) and poly(propylene glycol) homopolymers and copolymers with isolated yields of 82–99% and end-group conversions of >99% as determined by NMR spectroscopy and MALDI ToF MS. Furthermore, this process is applicable to a sequential reagent addition approach without intermediate polymer isolation steps with only a slight reduction in yield and end-group conversion (95%). Importantly, a simple work-up procedure provides access to high purity polyglycols without contamination from other reagents.

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