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Solid State Analysis of Metal-Containing Polymers Employing Mössbauer Spectroscopy, Solid State NMR and F EI TOF MALDI MS

Published on Sep 1, 2010in Journal of Inorganic and Organometallic Polymers and Materials 1.64
· DOI :10.1007/s10904-010-9336-y
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Frank D. Blum25
Estimated H-index: 25
(Missouri University of Science and Technology)
+ 8 AuthorsLorenzo Pellerito7
Estimated H-index: 7
(University of Palermo)
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Abstract
Polymers in general and metal-containing polymers in particular are often sparingly soluble or insoluble, in contrast to small molecules. Thus, special significance is attached to characterization techniques that can be applied to the materials as solids. Here, three techniques are discussed that give structural information gained from the solid material. Mossbauer spectroscopy is a powerful technique that may give information on the structure about the metal-containing moiety for about 44 different nuclei. Its use in describing the structure of the product obtained from organotin dichlorides and the unsymmetrical ciprofloxacin is presented along with the reaction implications of the results. Solid state NMR is also a useful tool in describing the structure of metal-containing polymers and its use is briefly described. Finally, MALDI MS can be used to gain structural information. For many metals it is particularly useful because of the presence of different isotopes that allow the identification of units through comparison of these isotope abundances with ion fragment clusters. Each of these tools can provide important structural characterization information.
  • References (52)
  • Citations (11)
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References52
Newest
Published on Aug 15, 2006
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University)
Introduction to Polymers History of Polymers Why Polymers? Today's Marketplace Environmental Assessment Managing Sustainability Polymer Structure (Morphology) Stereochemistry of Polymers Molecular Interactions Polymer Crystals Amorphous Bulk State Polymer Structure-Property Relationships Crystalline and Amorphous Combinations Cross-Linking Molecular Weight of Polymers Introduction Solubility Average Molecular Weight Values Fractionation of Polydisperse Systems Chromatography Colligative Molecula...
85 Citations
Published on Dec 1, 2009in BMC Cancer 2.93
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington),
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University)
+ 2 AuthorsGirish Barot11
Estimated H-index: 11
(FAU: Florida Atlantic University)
Background Monomeric Group IVB (Ti, Zr and Hf) metallocenes represent a new class of antitumor compounds. There is literature on the general biological activities of some organotin compounds. Unfortunately, there is little information with respect to the molecular level activity of these organotin compounds. We recently started focusing on the anti-cancer activity of organotin polymers that we had made for other purposes and as part of our platinum anti-cancer effort.
16 Citations Source Cite
Published on Oct 21, 2009in Materials 2.97
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
Organotin polyethers are easily synthesized employing interfacial polymerization systems involving the reaction of hydroxyl-containing Lewis bases and organotin halides. A wide variety of organotin-containing polymeric products have been synthesized including those derived from natural and synthetic polymers such as lignin, xylan, cellulose, dextran, and poly(vinyl alcohol). Others have been synthesized employing known drug diols such as dicumarol, DES, and dienestrol and a wide variety of synth...
24 Citations Source Cite
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington),
Kimberly Shahi10
Estimated H-index: 10
(UTA: University of Texas at Arlington)
+ 2 AuthorsCharles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University)
Pancreatic cancer kills nearly all patients within 3–6 months after detection. There is no effective chemotherapy for it. We have found a number of organotin polymers that are effective at inhibiting pancreatic cancer cell lines with Chemotherapeutic Index values greater than two with some to values of 50.
24 Citations Source Cite
Girish Barot11
Estimated H-index: 11
(FAU: Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
+ 3 AuthorsCharles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University)
A variety of dibutyltin polyethers have been synthesized employing the interfacial polymerization technique. The products are polymers with degrees of polymerization ranging from 60 to 390. Infrared spectral and mass spectral results are consistent with the proposed structure. The products show good inhibition of a variety of cancer cells including those associated with bone, breast, prostrate, and lung cancers. Some also show good viral inhibition of the HSV-1 (herpes simplex) and Vaccina (smal...
26 Citations Source Cite
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
+ 2 AuthorsGirish Barot11
Estimated H-index: 11
(FAU: Florida Atlantic University)
Organotin polyethers containing the synthetic estrogen diethylstilbestrol have been made in moderate yield with chain lengths ranging from 20 to 200 repeat units employing the interfacial polycondensation procedure. Infrared spectroscopy shows the absence of the O–H group and formation of the Sn–O linkage consistent with the formation of the polyether. F-MALDI MS results are consistent with the presence of organotin-containing fragmentation clusters containing one and two tin atoms and ion fragm...
23 Citations Source Cite
Published on Jan 1, 2008
Alaa S. Abd-El-Aziz1
Estimated H-index: 1
Synthetic Versatility and Structural Modularity in Organometallic Polymers.- Hyperbranched Polymers Containing Transition Metals: Synthetic Pathways and Potential Applications.- Transition Metal ?-Acetylide Polymers Containing Main Group Elements in the Main Chain: Synthesis, Light Emission and Optoelectronic Applications.- The Spectroscopy and Photophysical Behavior of Diphosphine- and Diisocyanide-Containing Coordination and Organometallic Oligomers and Polymers: Focus on Palladium and Platinu...
17 Citations
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Amitabh Battin6
Estimated H-index: 6
(FAU: Florida Atlantic University)
+ 1 AuthorsMichael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
A number of diaminopyrimidines have been incorporated into dibutyltin polyamines with molecular weights ranging from 3.5 × 104 to 3.7 × 106 and product yields from 47 to 88%. Infrared spectroscopy is consistent with the inclusion of the diaminopyridines into the polymer backbone with the IR spectroscopy showing the formation of the Sn–N bond as well as the presence of bands from both reactants being present in the polymer. F MALDI MS is also consistent with the products being polymeric and conta...
26 Citations Source Cite
Girish Barot11
Estimated H-index: 11
(FAU: Florida Atlantic University),
Kimberly Shahi10
Estimated H-index: 10
(UTA: University of Texas at Arlington)
+ 1 AuthorsCharles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University)
A series of organotin poly(ethylene glycols) were synthesized including the first water soluble organotin polymers. These products are all polymeric with weight average molecular weights about 105. Infrared spectroscopy shows the presence of moieties from both reactants and the formation of the Sn–O linkage. F MALDI MS shows the presence of up to over a hundred units and by isotopic abundance the presence of one, two, and three tin-containing ion fragments. The polymers inhibit the growth of can...
34 Citations Source Cite
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Kenzo Morie1
Estimated H-index: 1
Organotin polyesters have been synthesized employing the classical interfacial polycondensation of organotin dihalides and the salt of 1,1′-ferrocenedicarboxylic acid. The products are oligomeric (DP = 5) to polymeric (DP = 220). The presence of new IR bands characteristic of formation of the Sn–O band are present. Ion fragments characteristic of the repeat unit and greater are found employing F MALDI MS.
11 Citations Source Cite
Cited By11
Newest
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
+ 5 AuthorsPaul Slawek2
Estimated H-index: 2
(FAU: Florida Atlantic University)
Polyesters were rapidly synthesized employing interfacial polymerization from reaction of the salt of camphoric acid with Group VA (Group 15) triphenylmetallic dihalides. Yields range from 25 to 46 percent with chain lengths about 250. Infrared spectroscopy shows the formation of two new bands one assigned to the symmetrical M–O stretching and the second assigned to the asymmetrical M–O stretching. The bridging structure about the metal atom increases as the metal atom size increases. MALDI MS a...
2 Citations Source Cite
Charles E. Carraher7
Estimated H-index: 7
(FAU: Florida Atlantic University),
Alicia Morrison2
Estimated H-index: 2
(FAU: Florida Atlantic University)
+ 3 AuthorsLindsey Miller4
Estimated H-index: 4
(UTA: University of Texas at Arlington)
4 Citations Source Cite
Published on Sep 1, 2015in Journal of Inorganic Biochemistry 3.22
Claudia Pellerito14
Estimated H-index: 14
(University of Palermo),
O. Morana1
Estimated H-index: 1
(University of Palermo)
+ 4 AuthorsTiziana Fiore14
Estimated H-index: 14
(University of Palermo)
Abstract This work deals with the synthesis, the chemical characterization of dibutyltin(IV) complex of caffeic acid (Bu 2 Sn(IV)HCAF, caf1 ) and its cytotoxic action on tumor cells. The coordination environment at the tin center was investigated by FTIR, 119 Sn{ 1 H} cross polarization magic angle spinning, electrospray ionization mass spectroscopy in the solid state and UV–vis, fluorescence and 1 H, 13 C and 119 Sn NMR spectroscopy in solution phases. Density functional theory study confirmed ...
3 Citations Source Cite
Published on Nov 1, 2014in Inorganica Chimica Acta 2.43
Charles E. Carraher7
Estimated H-index: 7
(FAU: Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
+ 1 AuthorsAlisa Moric Johnson2
Estimated H-index: 2
(UTA: University of Texas at Arlington)
Abstract Poly(amine esters) are rapidly formed employing the interfacial condensation of group VA triphenylmetal dihalides with the antibacterial agent norfloxacin in moderate yield and low to high polymers with respect to average chain length. Infrared spectroscopy shows the formation of M-oxygen and M N bonds. The products are largely bridging structures about the metal atom. Proton NMR and MALDI MS results are consistent with the formation of the poly(amine esters). All of the polymers show g...
4 Citations Source Cite
Published on Nov 1, 2014in Inorganica Chimica Acta 2.43
Charles E. Carraher7
Estimated H-index: 7
(FAU: Florida Atlantic University),
Ngoc Trang Caroline Truong2
Estimated H-index: 2
(FAU: Florida Atlantic University)
+ 3 AuthorsNancy T. Trang5
Estimated H-index: 5
(UTA: University of Texas at Arlington)
Abstract Polyether esters are rapidly formed employing the interfacial condensation of organotin dihalides with glycyrrhetinic acid in high yield and oligomeric to polymeric chain length. Infrared spectroscopy shows the formation of tin–oxygen bonds. The products are a mixture of bridging and non-bridging structures about the tin atom. Proton NMR and MALDI MS results are consistent with the formation of the poly(ether esters). The dimethyltin, dibutyltin, and diphenyltin polymers exhibit good in...
7 Citations Source Cite
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Alicia Morrison2
Estimated H-index: 2
(FAU: Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(UTA: University of Texas at Arlington)
Organotin polyesters were synthesized from the interfacial condensation of organotin dihalides and salts of 3,5-pyridinedicarboxylic acid. The polymers are synthesized in moderate to high yields and are moderate to high polymers. MALDI MS, IR spectral, and NMR spectral results are consistent with the proposed structure. The Sn–O stretching band is found at about 1,028 cm−1. Infrared spectra are consistent with majority of the products having a non-bridged structure about the tin. All of the poly...
7 Citations Source Cite
Charles E. Carraher24
Estimated H-index: 24
(FAU: Florida Atlantic University),
Ngoc Trang Caroline Truong2
Estimated H-index: 2
(FAU: Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(UTA: University of Texas at Arlington)
Polyether esters were rapidly formed employing the interfacial condensation of Group VA triphenylmetal dihalides with glycyrrhetinic acid in moderate yield and chain length. Infrared spectroscopy shows the formation of metal–oxygen bonds. The products are a mixture of bridging and non-bridging structures about the metal atom. Proton NMR and MALDI MS results are consistent with the formation of the polyether esters. Some of the polymers exhibit inhibition of the growth of pancreatic cancer cell l...
8 Citations Source Cite
Charles E. Carraher7
Estimated H-index: 7
(FAU: Florida Atlantic University),
Marian Ayoub3
Estimated H-index: 3
(FAU: Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(UTA: University of Texas at Arlington)
In this study, organotin polyesters have been formed from the interfacial reaction between the disodium salt of chelidonic acid and a variety of organotin dihalides. Reactions occur rapidly within less than 15 seconds. Yields vary from moderate to high, and chain length varies from 30 to 800 repeat units. Infrared spectral analysis shows the presence of the Sn–O linkage and is consistent with the geometry about the tin being generally a mixture of tetrahedral or nonbridging and octahedral or bri...
9 Citations Source Cite
Charles E. Carraher7
Estimated H-index: 7
(FAU: Florida Atlantic University),
Girish Barot11
Estimated H-index: 11
(BU: Boston University)
+ 2 AuthorsMichael R. Roner19
Estimated H-index: 19
(UTA: University of Texas at Arlington)
The degradation of water soluble organotin polyether in the presence of trypsin was studied. The polymer was found to be stable to 4 days, the typical cancer cell line testing time. This is consistent with polymer activity against cancer cell lines being a result of the non-degraded chain and not controlled release of the organotin moiety. As a control trypsin activity was studied employing light scattering photometry and gel electrophoresis. The trypsin was active degrading bovine serine albumi...
12 Citations Source Cite
Published on Jul 1, 2011in Journal of Mass Spectrometry 2.27
Mark F. Wyatt12
Estimated H-index: 12
(Swansea University)
A mini-review of the characterisation of metal-containing compounds by matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS) is presented. Organometallic and coordination compounds have many varied applications, most notably in industrial catalytic processes and also in the electronics and healthcare sectors. In general, the compounds discussed, be they small or large molecules, have a high percentage metal content, rather than simply containing ‘a metal atom...
26 Citations Source Cite