The few available reports show that the element has been used for the simultaneous detection of dopamine and ascorbic acid on a glassy carbon electrode  and the detection of rutin with CNTs on glassy carbon . These reports provide evidence of the ability of neodymium to improve the conductivity and increase the surface area of an electrode.
The aim and novelty of this work is to take advantage of the conductivity and bioaffinity capabilities of CNTs and Nd to develop a sensor with similar properties of selectivity, sensitivity and stability as those in previous reports. Materials and methods 2. Electrolyte solutions were prepared in a pH range from 2. Then, each mixture was pressed into a PVC cavity until contact was made with a copper wire as the electrical contact.
The surfaces of the electrodes were polished with filter paper until the surfaces were smooth. It was possible to obtain three fresh surfaces with each electrode by removing the excess material from the surface and repolishing. The electrodes were stored in dry state at room temperature. Sample preparation Pharmaceutical dosages of PCM in the form of tablets, powders and syrup were obtained from a pharmacy in Ibague City Colombia.
The tablets and powder samples were weighed and crushed in a mortar and then diluted with mL of ultrapure water, and the syrup sample was diluted fold. Before each analysis, no pretreatment as filtration to eliminate possible interference was necessary. For validation study, 5.
Measurement procedures 2. Stripping and cyclic voltammetry measurements To the electrochemical cell, 9. Each voltammogram reading was repeated three times. Square-wave stripping voltammetry SWV was applied to the electrochemical cell containing 1.
The tested electrolyte was Results and discussion 3. The anodic peak currents for PCM increased from 1. The results showed that the anodic and cathodic peak currents were increased when the surface of the electrodes was modified and that the potential moved to less positive values. It is possible that a considerable increase in the surface area and the high conductivity of the surface with Nd2O3 and SWCNTs contributed to the electrocatalytic performance of the electrode in the redox reaction with PCM as in previous reports with Nd2O3 with chitosan for detected dopamine and ascorbic acid .
The hydrolytic scission of P-C bond has been reported for diphosphonium derivatives in the reaction media [30, 31] but has never been observed on the sorbent during chromatographic purufication.
It is noteworthy that the very mild conditions of transformation of 4 to 5 allow retaining the double bond in the substrate leading to a formation of the vinylphosphonium product that is the only example among very few phosphonium phosphine oxides that have been reported up to date.
Compound 5 was fully characterized by NMR spectra Exp. The C 11 carbon atom is slightly out of the plane of the Cp ligand the deviation is 0. The structure of this moiety coincides with that one of the vinyl fragment in complex 3 described by us recently . Nafion film, the polymer bearing sulfonyl groups and having a number of advantages, was used as the protonating agent. The reaction very gently proceeds throughout a film of the polymeric acid at low temperature that prevents the products from gumming.
The phosphonium products can be easily isolated from the reaction mixture by an exchange of the counter ion. When metal complexes are used as the reactants, the metal containing products of their destruction remain in the polymer film and do not contaminate the products that is very important for synthetic chemistry, specifically, for syntheses of pharmaceutical substances.
The reported method uses sc-CO2 as the "green" solvent allowing the use of polymer reagents. The one step syntheses of new phosphonium salts proceed at low temperature in the absence of highly reactive reactants and in good yields give rise the products relative to the compounds widely used in synthetic chemistry.
So, this approach is promising to cover a variety of nucleophiles. A protonation of substrates with Nafion in sc-CO2 allows generating the labile cationic intermediates and isolating the stable products of their transformations thus elucidating both the structures of the intermediates and mechanisms of the reactions involving their formation.
Finally, the first vinylphosphonium phosphine oxide derivative, a product of the mild hydrolytic cleavage of the P-C bond, was obtained. Acknowledgments This work was financially supported by the Russia Foundation for Basic Research project nos. Kizas, D. Antonov, Y. Vopilov, I. Godovikov, A. Peregudov, N. Kagramanov, L. Bulatnikova, L. Khokhlov, Hydration of terminal alkynes on Nafion film in supercritical carbon dioxide, J. Fluids 76 Elliott, S.
Hanna, A. Elliott, G. Gelbard, Organic synthesis by catalysis with ion-exchange resins, Ind. Jessop, T. Ikariya, R. Darr, M. Beckmann, Supercritical and near-critical CO2 in green chemical synthesis and processing, J. Fluids 28 Jessop, Homogeneous catalysis using supercritical fluids: Recent trends and systems studied, J.
Fluids 38 — Process Res. Peach and J. Eastoe, Suprcritical carbon dioxide: a solvent like no other, Beilstein J. Zhang, S. Heinonen and E. Kemmere, T. Meyer Ed. Fujita, H. Yoshida, K. Asai, X. Meng, M. Fluids 60 — Chaschin, T. Grigorev, M. Gallyamov, A. Khokhlov, Direct deposition of chitosan macromolecules on a substrat from solutions in supercritical carbondioxide: Solubility and conformational analysis, Eur.
Elmanovich, M. Kondratenko, D. Kolomytkin, M. Khokhlov, Active layer materials coated with Teflon AF nano-films deposited from solutions in supercritical CO2 for fuel cell applications, Int. Hydrogen Energy 38 Campardelli, L. Baldino, E. Reverchon, Supercritical fiuids applications in nanomedicine, J. Fluids — Ahn, S.
Bae, M. Kim, S. Cho, S. Balk, J. Lee, J. Cha, Review of supercritical CO2 power cycle technology and current status of research and development, Nucl. Ghoreishi, A. Hedayati, K. Ansari, Experimental investigation and optimization of supercritical carbon dioxside extraction of toxic heavy metals from solid waste using different modifiers and chelating agents, J. Monhemi, M. Housaindokht, Chemical modification of biocatalyst for function in supercritical CO2: In silico redesign of stable lipase, J.
Fluids Petrenko, M. Antipova, D. Gurina, Salisylic acid, acetylsalicylic acid, methyl salicylate, salicylamide, and sodium salicylate in supercritical carbon dioxide: Solute — cosolvent hydrogen bonds formation, J. Fluids 62— Filatova, O. Turova, I. Kuchumov, A. Kostenko, A.
Nigmatov, S. Zlotin, Asymmetric catalytic synthesis of functionalized tetrahydroquinolines in supercritical fluids, J. Fluids 35— Belomoina, E. Bulycheva, L. Nikitin, V. Bruma, Stady of the process of poly phenylquinoxaline s formation in supercritical carbon dioxide, J. Fluids 66— Sodeifian, S. Sajadian, N. Ardestani, Supercritical fluid exstraction of omega-3 from Dracocephalum kotschyi seed oil: Process optimization and oil properties, J. Polloni, J. Veneral, E.
Rebelatto, D. Oliveira, P. Tenorio, C. Pando, A. Fluids 7— Chauvet, M. Sauceau, J. Ushiki, N. Takahashi, T.Your aspirin product as well as a commercial aspirin tablet will be compared to a standard 0. Kizas, I. Tenorio, C.
The results showed that the anodic and cathodic peak currents were increased when the surface of the electrodes was modified and that the potential moved to less positive values.
Diphosphonium polymers ehxibit enhanced thermostability and can be used to generate energy .
Elliott, G. Ahn, S. Acknowledgments This work was financially supported by the Russia Foundation for Basic Research project nos. The mixture was heated on a hot plate until all the salicylic acid was dissolved.
Gelbard, Organic synthesis by catalysis with ion-exchange resins, Ind.
Measurement procedures 2. It should be noted that structural relatives of phosphonium derivatives are widely used in organic  and asymmetric synthesis [31, 36], as the precursors of ylides [30, ] and frustrated Lewis pairs , and as radiolabels in SPECT and PET tomography . Hedayati, K. Ahn, S.
Procedure: 1. To add titles to the plot, select layout, axis titles, and then chart titles. In addition, the experimental data exhibited an elevation of the temperature to favor the hydration reaction rather then a formation of the onium derivatives.
Sodeifian, S. Next add 20 ml of distilled water and cool in an ice bath. In this experiment, the crude product will be the desired product. Hydrogen atoms were placed geometrically and included in the structure factors calculation in the riding motion approximation. Ahn, S. Also, your melting point range may be greater than 2 degrees.
We have disclosed that despite the presence of notable quantities of water in Nafion  the protonation of 1 in sc-CO2 in the presence of nucleophiles PPh3, DPPE makes it possible to obtain the products of direct interaction of cation 2 with the phosphines. If impurities are present in your crude sample, the melting point range for your product will be lower than the range of pure aspirin. Figure Carbon dioxide 9 MPa was injected in the reactor at room temperature. Nafion film, the polymer bearing sulfonyl groups and having a number of advantages, was used as the protonating agent. On purification by preparative TLC on Al2O3, salt 4 was found to undergo it a hydrolytic scission of the P-C Fc bond giving rise ferrocenylvinyl phosphonium phosphine oxide tetrafluoroborate 5.
All experiments were carried out in the stainless steel reactor 10 cm3. Measure out 6. Godovikov, F. Is the crude product above of below this mark? Published on Dec 10, Abstract In this experiment you will synthesize aspirin and determine the yield or fraction of the theoretical amount which can be made. The crystals were filterer using a Buchner filter and extracted using chilled water.