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 1.75
· DOI :10.1007/s10904-010-9336-y
Charles E. Carraher23
Estimated H-index: 23
(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)
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 (51)
  • Citations (11)
Cite
References51
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Ryuhei Ueeda2
Estimated H-index: 2
(Osaka University),
Yoshikane Kawasaki19
Estimated H-index: 19
(Osaka University)
+ 1 AuthorsRokuro Okawara26
Estimated H-index: 26
(Osaka University)
29 Citations Source Cite
Published on Jan 1, 1971
John G. Stevens10
Estimated H-index: 10
,
Virginia E. Stevens1
Estimated H-index: 1
208 Citations Source Cite
Published on Jan 1, 1984
R. H Herber1
Estimated H-index: 1
111 Citations Source Cite
Published on Jan 1, 1976
T. C. Gibb1
Estimated H-index: 1
1 The Mossbauer Effect.- 2 Hyperfine Interactions.- 3 Molecular Structure.- 4 Electronic Structure and Bonding: Diamagnetic Compounds.- 5 Electronic Structure and Bonding: Paramagnetic Compounds.- 6 Dynamic Effects.- 7 Oxides and Related Systems.- 8 Alloys and Intermetallic Compounds.- 9 Analytical Applications.- 10 Impurity and Decay After-effect Studies.- 11 Biological Systems.- Observed Mossbauer Resonances.
144 Citations Source Cite
Published on Jan 1, 1984
Gary J. Long8
Estimated H-index: 8
,
Fernande Grandjean40
Estimated H-index: 40
1. The Early Days of the Effect.- 2. Mossbauer Effect Studies of Hard Magnetic Materials.- 3. Mossbauer Effect Studies of Oxidic Spinels.- 4. Evaluation of Distributed Hyperfine Parameters.- 5. Radio Frequency Field-Induced Effects in Ferromagnetic Materials.- 6. Mossbauer Spectroscopic Studies of the High Oxidation States of Iron.- 7. Mossbauer Spectroscopic Studies of Intercalation Compounds.- 8. Mossbauer Spectroscopy of Iron and Iron-Molybdenum Hydrotreating Catalysts.- 9. The Use and Potent...
888 Citations Source Cite
G.M. Bancroft1
Estimated H-index: 1
(University of Western Ontario),
R.H. Piatt1
Estimated H-index: 1
(University of Cambridge)
Publisher Summary Mossbauer spectroscopy can be likened to ultraviolet spectroscopy. Both techniques employ a source of radiation, an absorber and a detector. In Mossbauer spectroscopy, we consider transitions between nuclear energy levels with the emission and absorption of y rays; whereas, in ultraviolet spectroscopy, we consider the transitions between electronic energy levels with the emission and absorption of ultraviolet radiation. To observe resonance, a range of source photon energies is...
183 Citations Source Cite
Published on Feb 1, 1971in Journal of Organometallic Chemistry 1.95
R.P.A. Sneeden12
Estimated H-index: 12
(Monsanto),
H.H. Zeiss14
Estimated H-index: 14
(Monsanto)
Abstract The interaction of tri(2,2,-dideutero-4-phenylbutyl)chromium and -iron with 1,7-octadiene and 3-phenylpropene, respectively, results in the formation of hydrogenation products (deutero-2-octene and 1,2-dideutero-3-phenylpropane) and isomerization products. These results prove the intermolecular transfer of hydrogen (deuterium) from the β-position of an alkyl group bonded to the metal to diene (olefin) substrate.
14 Citations Source Cite
Published on Aug 15, 2006
Charles E. Carraher23
Estimated H-index: 23
(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...
81 Citations
Published on Sep 5, 2003
Alaa S. Abd-El-Aziz22
Estimated H-index: 22
,
Charles E. Carraher23
Estimated H-index: 23
+ 2 AuthorsMartel Zeldin6
Estimated H-index: 6
128 Citations Source Cite
Published on Jan 1, 1998
P. G. Harrison1
Estimated H-index: 1
Tin - the element. Compounds of tin General trends. The inorganic chemistry of tin. Formation and cleavage of the tin-carbon bond. Organometallic compounds of tetravalent tin. Organometallic compounds of bivalent tin. Tin-metal bonded compounds. Radical chemistry of tin. The uses of organotin compounds in organic synthesis. Recent studies on the mode of biological action of the di- and trialkyltin compounds. Health and safety aspects of tin chemicals. Industrial uses of tin chemicals. Solid stat...
315 Citations Source Cite
Cited By11
Published on Sep 1, 2015in Journal of Inorganic Biochemistry 3.06
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 ...
2 Citations Source Cite
Published on Nov 1, 2014in Inorganica Chimica Acta 2.26
Charles E. Carraher7
Estimated H-index: 7
(Florida Atlantic University),
Ngoc Trang Caroline Truong2
Estimated H-index: 2
(Florida Atlantic University)
+ 3 AuthorsNancy T. Trang5
Estimated H-index: 5
(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. Carraher23
Estimated H-index: 23
(Florida Atlantic University),
Ngoc Trang Caroline Truong2
Estimated H-index: 2
(Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(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
(Florida Atlantic University),
Girish Barot11
Estimated H-index: 11
(Boston University)
+ 2 AuthorsMichael R. Roner19
Estimated H-index: 19
(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
Charles E. Carraher7
Estimated H-index: 7
(Florida Atlantic University),
Marian Ayoub3
Estimated H-index: 3
(Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(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...
8 Citations Source Cite
Published on Nov 1, 2014in Inorganica Chimica Acta 2.26
Charles E. Carraher7
Estimated H-index: 7
(Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(University of Texas at Arlington)
+ 1 AuthorsAlisa Moric Johnson2
Estimated H-index: 2
(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
Charles E. Carraher23
Estimated H-index: 23
(Florida Atlantic University),
Alicia Morrison2
Estimated H-index: 2
(Florida Atlantic University)
+ 2 AuthorsNancy T. Trang5
Estimated H-index: 5
(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
Published on Feb 1, 2014in Journal of Organometallic Chemistry 1.95
Charles E. Carraher23
Estimated H-index: 23
(Florida Atlantic University),
Michael R. Roner19
Estimated H-index: 19
(University of Texas at Arlington)
Abstract Organotin polymers are easily synthesized employing interfacial polymerization systems involving the reaction of difunctional Lewis bases and organotin halides. A wide variety of organotin-containing polymeric products have been synthesized including the first water soluble organotin polymers. The organotin polymers exhibit a wide range of biological activities including the inhibition of a wide variety of cancer cell lines including cell lines associated with ovarian, colon, lung, pros...
63 Citations Source Cite
Published on Jul 1, 2011in Journal of Mass Spectrometry 2.11
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
Charles E. Carraher7
Estimated H-index: 7
(Florida Atlantic University),
Alicia Morrison2
Estimated H-index: 2
(Florida Atlantic University)
+ 3 AuthorsLindsey Miller4
Estimated H-index: 4
(University of Texas at Arlington)
4 Citations Source Cite