scholarly journals Optimization of Copper Stain Removal from Marble through the Formation of Cu(II) Complexes in Agar Gels

Gels ◽  
2021 ◽  
Vol 7 (3) ◽  
pp. 111
Author(s):  
Antonio Sansonetti ◽  
Moira Bertasa ◽  
Cristina Corti ◽  
Laura Rampazzi ◽  
Damiano Monticelli ◽  
...  
Keyword(s):  
Inductively Coupled Plasma ◽  
Copper Complexes ◽  
Ethylenediaminetetraacetic Acid ◽  
Ammonium Citrate ◽  
Copper Salts ◽  
Agar Gel ◽  
Paramagnetic Resonance ◽  
Agar Gels ◽  
Stain Removal ◽  
Vis Spectroscopy

Copper complexes with different ligands (ethylenediaminetetraacetic acid, EDTA, ammonium citrate tribasic, TAC, and alanine, ALA) were studied in aqueous solutions and hydrogels with the aim of setting the optimal conditions for copper stain removal from marble by agar gels, with damage minimization. The stoichiometry and stability of copper complexes were monitored by ultraviolet-visible (UV-Vis) spectroscopy and the symmetry of Cu(II) centers in the different gel formulations was studied by electron paramagnetic resonance (EPR) spectroscopy. Cleaning effectiveness in optimized conditions was verified on marble laboratory specimens through color variations and by determining copper on gels by inductively coupled plasma-mass spectrometry (ICP-MS). Two copper complexes with TAC were identified, one having the known stoichiometry 1:1, and the other 1:2, Cu(TAC)2, never observed before. The stability of all the complexes at different pH was observed to increase with pH. At pH 10.0, the gel’s effectiveness in removing copper salts from marble was the highest in the presence of ALA, followed by EDTA, TAC, and pure agar gel. Limited damage to the marble surface was observed when gels with added EDTA and TAC were employed, whereas agar gel with ALA was determined to be the most efficient and safe cleaning material.

scholarly journals Copper Complexes of Benzoylacetone Bis-Thiosemicarbazones: Metal and Ligand Based Redox Reactivity

2021 ◽  
Vol 74 (1) ◽  
pp. 34 ◽  
Author(s):  
Jessica K. Bilyj ◽  
Jeffrey R. Harmer ◽  
Paul V. Bernhardt
Keyword(s):  
Electron Paramagnetic Resonance ◽  
Cyclic Voltammetry ◽  
Copper Complexes ◽  
Atmospheric Oxygen ◽  
The Other ◽  
Oxidation Reactions ◽  
Paramagnetic Resonance ◽  
Time Resolved ◽  
Vis Spectroscopy ◽  
Electron Paramagnetic

Bis-thiosemicarbazones derived from the β-diketone benzoylacetone (H3banR, R=Me, Et, Ph) are potentially tetradentate N2S2 ligands whose coordination chemistry with copper is reported. In the absence of oxygen and in the presence of base they form anionic CuII complexes of the fully deprotonated ligands [CuII(banR)]–. Upon exposure to atmospheric oxygen they undergo a complex series of reactions leading to two types of products; one a ligand oxidised ketone complex [CuII(banRO)] and the other an unprecedented dimeric di-CuIII complex [(CuIII(banR))2] depending on the R substituent. Time-resolved UV-vis spectroscopy, cyclic voltammetry, spectroelectrochemistry, and electron paramagnetic resonance (EPR) spectroscopy have been used to identify intermediates on the way to stable products formed under both anaerobic and aerobic conditions. It is found that both ligand-centred and Cu-centred oxidation reactions are occurring in parallel leading to this unusually complicated mixture of products.

scholarly journals Synthesis and Structure of Copper Complexes of a N6O4 Macrocyclic Ligand and Catalytic Application in Alcohol Oxidation

Catalysts ◽  
2019 ◽  
Vol 9 (5) ◽  
pp. 424 ◽  
Author(s):  
Zhen Ma ◽  
Qijun Wang ◽  
Elisabete C. B. A. Alegria ◽  
M. Fátima C. Guedes da Silva ◽  
Luísa M. D. R. S. Martins ◽  
...  
Keyword(s):  
Copper Complexes ◽  
Electron Paramagnetic Resonance Spectroscopy ◽  
Aerobic Oxidation ◽  
Electrochemical Techniques ◽  
Macrocyclic Ligand ◽  
Copper Cation ◽  
Molecular Structures ◽  
Resonance Spectroscopy ◽  
Copper Salts ◽  
Paramagnetic Resonance

Reactions between N6O4 macrocyclic 1,4,19,22,25,40-hexaaza-10,13,31,34-tetraoxa-6,14,27,35(1,4)-tetrabenzenacyclopentacontane (L) and several copper salts (viz. trifuoromethane and toluene sulfonates, nitrate, perchlorate, benzoate, and acetate) led to the formation of dinuclear compounds [Cu2(OSO2CF3)2(DMF)2L](SO3CF3)2 (1), [Cu2(p-OSO2C6H4Me)2L(DMF)2](SO3C6H4Me)2 (2), [Cu2(ONO2)2L(DMF)2](NO3)2 (3), [Cu2(OClO3)2(DMF)2L](ClO4)2 (4), [Cu2(OOCPh)2L(H2O)2](O2CPh)2 (5), and [Cu2(OOCMe)4L] (6), which were characterized by IR, elemental analysis and TG-DTA (thermogravimetric-differential thermal analysis), as well as by single-crystal X-ray diffraction, EPR (electron paramagnetic resonance) spectroscopy, and electrochemical techniques (cyclic voltammetry and controlled potential electrolysis). The molecular structures of compounds 1–6 reveal a considerable conformational flexibility of the ligand L, which allowed its readjustment for the formation of the metal compounds and confirmed the presence of dinuclear endo macrocyclic species. In every case, the L ligand coordinates to each copper cation via three nitrogen atoms, with the remaining coordination positions of the metal square pyramid environment being accomplished by neutral or anionic ligands. The macrocyclic cavities appear to be adequate for the enclosure of a neutral species as proved by compound 6 with 1,4-dioxane. The compounds, in combination with the TEMPO (2,2,6,6-tetramethyl-piperidinyloxyl) radical and in alkaline aqueous solution, act as efficient catalysts in the aerobic oxidation of different alcohols to the corresponding aldehydes (yields up to 99% and TON up 232) after 20 h at 70 °C. In addition, the microwave-assisted solvent-free peroxidative oxidation (by tert-butylhydroperoxide, TBHP) of 1-phenylethanol led to acetophenone yields up to 99% and TOF of 1.1 × 103 after 0.5 h, without any additive.

Investigation of Antioxidant Activity of Pomegranate Juices by Means of Electron Paramagnetic Resonance and UV-Vis Spectroscopy

2015 ◽  
Vol 98 (4) ◽  
pp. 866-870 ◽  
Author(s):  
Violetta Kozik ◽  
Krystyna Jarzembek ◽  
Agnieszka Jędrzejowska ◽  
Andrzej Bąk ◽  
Justyna Polak ◽  
...  
Keyword(s):  
Electron Paramagnetic Resonance ◽  
Free Radical ◽  
Epr Spectroscopy ◽  
Antioxidant Properties ◽  
Free Radical Scavenger ◽  
Pomegranate Juice ◽  
Radical Scavenger ◽  
Paramagnetic Resonance ◽  
Vis Spectroscopy ◽  
Electron Paramagnetic

Abstract Pomegranate fruit (Punica granatum L.) is a source of numerous phenolic compounds, and it contains flavonoids such as anthocyanins, anthocyanidins, cyanidins, catechins and other complexes of flavonoids, ellagitannins, and hydrolyzed tannins. Pomegranate juice shows antioxidant, antiproliferative, and anti-atherosclerotic properties. The antioxidant capacity (TEAC) of the pomegranate juices was measured using electron paramagnetic resonance (EPR) spectroscopy and 1,1-diphenyl-2-picrylhydrazyl (DPPH•) as a source of free radicals, and the total phenolic (TP) content was measured using UV-Vis spectroscopy. All the examined pomegranate juices exhibited relatively high antioxidant properties. The TEAC values determined by means of EPR spectroscopy using Trolox (TE) as a free radical scavenger were in the range of 463.12 to 1911.91 μmol TE/100 mL juice. The TP content measured by the Folin-Ciocalteu method, using gallic acid (GA) as a free radical scavenger, widely varied in the investigated pomegranate juice samples and ranged from 1673.62 to 5263.87 mg GA/1 L juice. The strongest antioxidant properties were observed with the fresh pomegranate juices obtained from the fruits originating from Israel, Lebanon, and Azerbaijan. Correlation analysis of numerical data obtained by means of EPR spectroscopy (TEAC) and UV-Vis spectroscopy (TP) gave correlation coefficient (r) = 0.90 and determination coefficient (r2) = 0.81 (P <0.05).

A study of the decomposition behaviour of 12-tungstophosphate heteropolyacid in solution

2003 ◽  
Vol 81 (10) ◽  
pp. 1044-1050 ◽  
Author(s):  
Zhirong Zhu ◽  
Ruan Tain ◽  
Colin Rhodes
Keyword(s):  
Aqueous Solution ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Potentiometric Titration ◽  
Inductively Coupled Plasma ◽  
High Performance ◽  
Atomic Emission ◽  
Inductively Coupled ◽  
Vis Spectroscopy ◽  
Decomposition Behaviour

In this paper, the decomposition of H3PW12O40 in aqueous solution or in mixed solutions of water–ethanol or water–acetone is investigated by potentiometric titration and 31P NMR. Identification of the products from H3PW12O40 decomposition over a pH range of 1–12 was achieved using preparation high performance liquid chromatography (Pre-HPLC) combined with IR, UV–vis spectroscopy, and inductively coupled plasma atomic emission spectroscopy (ICP). It is found that H3PW12O40 in aqueous solution decomposes in a stepwise fashion with increasing pH, with the following solution compositions: [PW12O40]3– (at pH ~ 1) [Formula: see text] [PW12O40]3– + [P2W21O71]6– + [PW11O39]7– (at pH 2.2) [Formula: see text] [PW12O40]3– + [P2W21O71]6– + [PW11O39]7– + [P2W18O62]6– + [P2W19O67]10– (at pH 3.5) [Formula: see text] [P2W21O71]6– + [PW11O39]7– + [P2W18O62]6– (at pH 5.4) [Formula: see text] [PW9O34]9– (at pH 7.3) [Formula: see text] PO43– + WO42– (pH > 8.3). In the first stages at pH < 8, H3PW12O40 decomposes partially with removal of W=O units. In the second stage at pH > 8, tungstophosphoric completely decomposes to PO43–. In contrast, the decomposition of H3PW12O40 is reduced, or the stability of the [PW12O40]3– anion is enhanced, in ethanol–water or acetone solution at pH < 8. Key words: 12-tungstophosphate heteropolyacid, decomposition behaviour, potentiometric titration, 31P NMR, preparation high performance liquid chromatography.

Determination of Phosphorus and Potassium in Commercial Inorganic Fertilizers by Inductively Coupled Plasma-Optical Emission Spectrometry: Single-Laboratory Validation

2014 ◽  
Vol 97 (3) ◽  
pp. 687-699 ◽  
Author(s):  
James M Bartos ◽  
Barton L Boggs ◽  
J Harold Falls ◽  
Sanford A Siegel
Keyword(s):  
Inductively Coupled Plasma ◽  
Optical Emission ◽  
Optical Emission Spectrometry ◽  
Ammonium Citrate ◽  
Emission Spectrometry ◽  
Icp Oes ◽  
Inductively Coupled ◽  
Plasma Optical Emission Spectrometry ◽  
Single Laboratory

Abstract A two-part single-laboratory validation study was conducted for determination of the P and K content in commercial fertilizer materials by inductively coupled plasma-optical emission spectrometry (ICP- OES). While several methods exist for determination of P and K in fertilizer products, the main focus of this study was on ICP-OES determination, which offers several unique advantages. Fertilizer samples with consensus P and K values from the Magruder and Association of Fertilizer and Phosphate Chemists (AFPC) check sample programs were selected for this study. Validation materials ranging from 4.4 to 52.4% P2O5 (1.7 to 22.7% P) and 3 to 62% K2O (2.5 to 51.5% K) were utilized. Because all P and K compounds contained in fertilizer materials are not "available" for plants to use, this study was conducted in two parts. Part A focused on ammonium citrate–disodium EDTA as the extraction solvent, as it estimates the pool of fertilizer P and K that is considered available to plants. Part B focused on hydrochloric acid as the digestion solvent, as it estimates the total P and K content of the fertilizer product. Selectivity studies indicated that this method can have a high bias for fertilizer products containing sources of phosphite or organic P compared to gravimetric or colorimetric methods that measure just orthophosphate. Provided the analytical challenges outlined in this study are addressed, this method offers the potential for a quick, accurate, and safe alternative for determining the P and K content of commercial inorganic fertilizer materials.

Synthesis, characterization and application of green seaweed mediated silver nanoparticles (AgNPs) as antibacterial agents for water disinfection

2018 ◽  
Vol 78 (1) ◽  
pp. 235-246 ◽  
Author(s):  
D. Dixit ◽  
D. Gangadharan ◽  
K. M. Popat ◽  
C. R. K. Reddy ◽  
M. Trivedi ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Silver Nanoparticles ◽  
Inductively Coupled Plasma ◽  
Antibacterial Agents ◽  
Bacterial Count ◽  
Water Disinfection ◽  
Bacterial Strains ◽  
Vis Spectroscopy ◽  
Green Seaweed

Abstract A simple and eco-friendly method for the synthesis of hybrid bead silver nanoparticles (AgNPs) employing the aqueous extract derived from natural and renewable source namely tropical benthic green seaweed Ulva flexuosa was developed. This route involves the reduction of Ag+ ions anchored onto macro porous methacrylic acid copolymer beads to AgNPs for employing them as antibacterial agents for in vitro water disinfection. The seaweed extract itself acts as a reducing and stabilizing agent and requires no additional surfactant or capping agent for forming the AgNPs. The nanoparticles were analyzed using high-resolution transmission electron microscopy, UV–Vis spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray analysis and inductively coupled plasma optical emission spectroscopy. The study elucidates that such biologically synthesized AgNPs exhibit potential antibacterial activity against two Gram positive (Bacillus subtilis, Staphylococcus aureus) and two Gram-negative (Escherichia coli, Pseudomonas aeruginosa) bacterial strains tested. The bacterial count in treated water was reduced to zero for all the strains. Atomic force microscopy was performed to confirm the pre- and post-state of the bacteria with reference to their treatment with AgNPs. Attributes like facile environment-friendly procedure, stability and high antibacterial potency propel the consideration of these AgNPs as promising antibacterial entities.

Electron Paramagnetic Resonance Spectroscopic (EPR) Study of Copper Amine Treated Southern Pine in Wood Preservation

Holzforschung ◽  
2000 ◽  
Vol 54 (4) ◽  
pp. 343-348 ◽  
Author(s):  
J. Zhang ◽  
D. P. Kamdem
Keyword(s):  
Electron Paramagnetic Resonance ◽  
Copper Complexes ◽  
Electron Paramagnetic Resonance Spectroscopy ◽  
Treated Wood ◽  
Wood Preservation ◽  
Resonance Spectroscopy ◽  
Paramagnetic Resonance ◽  
Electronic Parameters ◽  
Electron Paramagnetic ◽  
Copper Amine

Summary The structure of copper complexes in copper amine treated wood samples were elucidated by the application of electron paramagnetic resonance spectroscopy (EPR). EPR axial spectra were observed for all Cu-amine treated samples irrespective of the formulations. The values of A∥ and g∥ of the axial spectra indicate that the stereo-structure of copper complexes in copper amine treated wood was either tetragonal-based octahedral or square-based pyramidal. Comparison of electronic parameters of A∥ and g∥ in Cu-amine treated wood with those of the Cu-amine treating solution and the values in literature suggests that the interaction of wood with copper amine is through complexation in which wood functional groups are complexed with copper amine perpendicularly. The copper complexes in both treating solution and treated wood are in the form of CuN2O2, where copper is ligated with 2 nitrogen and 2 oxygen.

scholarly journals Comparison of the Ammonium Oxalate Extraction of Fertilizer for K2O, Method 983.02, with the Ammonium Citrate/EDTA Extraction, Method 993.31

2003 ◽  
Vol 86 (4) ◽  
pp. 640-642 ◽  
Author(s):  
Natalie F Newlon
Keyword(s):  
Ethylenediaminetetraacetic Acid ◽  
Extraction Procedure ◽  
Ammonium Oxalate ◽  
T Test ◽  
Ammonium Citrate ◽  
Official Method ◽  
Wide Range ◽  
Significant Difference ◽  
Oxalate Extraction ◽  
Edta Extraction

Abstract The direct available method for phosphorus in fertilizers, Method 960.03, is an Official Method for extraction of both P2O5 and K2O. Because K2O is much more soluble and easier to extract than P2O5, the conditions of the extraction procedure are set for efficient extraction of P2O5, and the extraction of K2O is, in effect, a bonus. In 1993, a modified extraction procedure, using an extractant of ammonium citrate/ethylenediaminetetraacetic acid (EDTA) solution, was evaluated for P2O5 and then collaboratively studied. This now-modified extraction procedure for phosphorus is Official Method 993.31, which is used extensively as an alternative to Method 960.03 for phosphorus because it is less labor-intensive. Method 993.31 was also evaluated in our laboratory for K2O extraction, but it was never formally collaboratively studied for K2O. To demonstrate the suitability of Method 993.31 as an extraction procedure for K2O, as well as P2O5 in fertilizers, Method 993.31 extraction for K2O was compared with Method 983.02, the traditional ammonium oxalate extraction procedure for K2O. A wide range of fertilizer samples was extracted by using both procedures. The t-test for samples containing &lt;30% K2O had a t-value of 1.23 and a probability of 0.22, which indicates there was no significant difference in the results obtained by the 2 extraction methods. The t-test for samples containing &gt;30% K2O had a t-value of 0.30 and a probability of 0.77, also indicating no significant difference. It is recommended that Method 983.02 be modified to include the ammonium citrate/EDTA extraction procedure as an additional option for extraction of K2O from commercial fertilizers.

scholarly journals Fast Microwave Synthesis of Gold-Doped TiO2 Assisted by Modified Cyclodextrins for Photocatalytic Degradation of Dye and Hydrogen Production

Catalysts ◽  
2020 ◽  
Vol 10 (7) ◽  
pp. 801
Author(s):  
Cécile Machut ◽  
Nicolas Kania ◽  
Bastien Léger ◽  
Frédéric Wyrwalski ◽  
Sébastien Noël ◽  
...  
Keyword(s):  
Titanium Oxide ◽  
Microwave Synthesis ◽  
Inductively Coupled Plasma ◽  
Dye Degradation ◽  
Optical Emission ◽  
Titanium Chloride ◽  
Stabilizing Agents ◽  
Inductively Coupled ◽  
Vis Spectroscopy ◽  
Alkaline Conditions

A convenient and fast microwave synthesis of gold-doped titanium dioxide materials was developed with the aid of commercially available and common cyclodextrin derivatives, acting both as reducing and stabilizing agents. Anatase titanium oxide was synthesized from titanium chloride by microwave heating without calcination. Then, the resulting titanium oxide was decorated by gold nanoparticles thanks to a microwave-assisted reduction of HAuCl4 by cyclodextrin in alkaline conditions. The materials were fully characterized by UV-Vis spectroscopy, X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and N2 adsorption-desorption measurements, while the metal content was determined by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). The efficiency of the TiO2@Au materials was evaluated with respect to two different photocatalytic reactions, such as dye degradation and hydrogen evolution from water.

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