Mixed Solvent Of Acetone Research Articles

Enrichment and analysis of long-chain normal alkanals from Zhundong subbituminous coal

Zhundong subbituminous coal was exhaustively extracted with isometric carbon disulfide (CDS) and acetone mixed solvent. The extract was fractionated with petroleum ether (PE) and CDS into PE-extractable portion (E1) and CDS-extractable portion (E2). E2 was sequentially eluted with PE and 30% CDS/PE mixed solvent through a silica gel-packed column. A series of long-chain normal alkanals (LCNAs, C18−27) were enriched from E2 and identified with a gas chromatography/mass spectrometer. The fractional extraction and subsequent column chromatography provide an effective approach for enriching LCNAs from middle- and low-rank coals. LCNAs could be a class of important biomarkers.

Enrichment of oxygen-containing aromatics in an extract from Zhundong subbituminous coal

Zhundong subbituminous coal (ZSBC) was exhaustively extracted with isometric carbon disulfide (CDS)/acetone mixed solvent to afford extract 1 (E 1 ), which was sequentially extracted with petroleum ether (PE) and CDS to afford extracts 2 (E 2 ) and 3 (E 3 ). E 3 was gradiently eluted into effluent portions 1 to 5 (EPs 1 to 5) through a silica gel-packed column sequentially with PE, CDS/PE mixed solvents with volume ratio of 3:7, 1:1 and 7:3, and CDS. According to analysis with a gas chromatography/mass spectrometer, in total, 22 alkyl phenyl carbonates were enriched into EP 3 , and anthraquinone and its two derivatives, nine polycyclic aromatic ketones and two polycyclic aromatic lactones into EP 4 . Most of the oxygen-containing aromatics are value-added chemicals.

Enzymatic Synthesis of l-Ascorbyl Laurate in DMSO–Acetone Mixed Solvent

In the present study, a dimethyl sulfoxide (DMSO)–acetone mixed solvent was used as a reaction medium to study lipase-catalyzed esterification of l-ascorbic acid with lauric acid as the acyl donor....

A study on Fourier transform infrared spectroscopy, thermal, mechanical, NLO and laser damage properties on unidirectional Glycinium Picrate Mono Glycine crystal

By directional solidification, single crystal of Glycinium Picrate Mono Glycine (GPMG) was successfully grown by Sankaranarayanan–Ramasamy (SR) method. An optically transparent crystal of GPMG has been grown along 〈011〉 plane by a mixed solvent of acetone and double distilled water. The evaporation rate was controlled and a single crystal of 12mm diameter and 35mm length was obtained. Single crystal X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR), thermal, mechanical, SHG and laser damage studies were carried out. The results are discussed in detail.

A new photo-responsive organogel containing benzophenone group

Benzophenone group was introduced into the gel system in order to fabricate a new ALS2 organogel which was photo-responsive. In the gel state with mixed solvent of acetone and water (5%), helical fibres were formed. The light control on the morphological change from fibres to core–shell spheres was followed by transmission electron microscope, which supplied a new paradigm for the morphology control triggered by stimulus. Moreover, the gel could serve as light absorbent without being mixed with polymer.

Growth, optical, thermal, mechanical and dielectric characterization of brucinium hydrogen maleate

Brucinium hydrogen maleate (BHM) has been synthesized by the chemical reaction method. The solubility of the synthesized material was determined in water, acetone and water–acetone mixed solvents. Based on the solubility studies, the single crystals of BHM were grown from the 4:5 water–acetone mixed solvent by the solvent evaporation method. The crystallinity of the grown crystals was proved from the single crystal and powder XRD data. BHM was found to crystallize in monoclinic symmetry with non-centrosymmetric space group P21. BHM crystals of size 12×4×3mm3 were obtained in 20 days. The compound exhibits good physicochemical stability upto 237.78°C. Various thermodynamical parameters were calculated from the TG data. The UV transparency cutoff wavelength of BHM was found to be 215nm and the complex is transparent (42%) over the entire range of visible region showing that it is a good candidate for NLO applications. The growth feature of the BHM single crystals was observed by etching studies, which reveals the formation of layer growth pattern. The dielectric behavior of the grown crystal was analyzed for different frequencies at different temperatures. The mechanical properties of the crystal were estimated by Vickers hardness test.

A novel and simple pathway to synthesis of porous polyurea absorbent and its tests on dye adsorption and desorption

A novel one-step protocol for the preparation of porous polyurea material (PPU) through precipitation polymerization of toluene diisocynate (TDI) is presented. The process is based on step polymerization of one single monomer, TDI, with water in water–acetone mixed solvent. PPU is obtained without need for any porogen or additives, and no any chemical modification on the outcome polymer is necessary. The morphology, pore size and size distribution of PPU are characterized by scanning electron microscope and BET nitrogen adsorption. Taking acid fuchsine (AF) and Congo Red as dye examples in wastewaters, their adsorption on, desorption from PPU and the reusability of PPU were tested. Experimental conditions for AF adsorption were optimized with regard to pH, adsorption time, AF concentration and amount of PPU. Results demonstrate that the as-prepared PPU is of high performance in dyes adsorption and recycled use. This work presents therefore a novel and attractive candidate for removal of anionic dyes from wastewaters.

A facile route to preparation of uniform polymer microspheres by quiescent polymerization with reactor standing still without any stirring

This paper presents a novel and facile route to preparation of highly uniform polymeric microspheres through a quiescent polymerization with the reactor standing still without any stirring. Using one single monomer, isophorone diisocyanate (IPDI), highly uniform polyurea microspheres are achieved with high yield via precipitation polymerization of IPDI with water in water–acetone mixed solvent. Full conversion of IPDI to polymer is readily achieved thanks to the step polymerization mechanism involved. The monomer concentration can go up to 11wt.% with the polymerization accomplished within 2h, with a much higher yield of microspheres in a much shorter time than those reported with vinyl monomers. The size of the microspheres is adjustable by changing IPDI concentration, acetone/H2O ratio in the solvent or polymerization temperature. Without need of any stirring or shaking during the polymerization, the protocol renders the fabrication of uniform microspheres more practical and economical, particularly for large scaled production.

In situ doping of carbon and sulfur from multifunctional agents to TiO2 nanospheres in water–acetone mixed solvent

A novel strategy allowed the synthesis of carbon and sulfur codoped TiO2 nanospheres from multifunctional agents: Ti(SO4)2 as Ti source and sulfur donor, polyvinyl pyrrolidone (PVP) as surfactant and carbon donor. Ti(SO4)2 nanospheres precipitated in water–acetone mixed solvent. In situ doping of S to TiO2 was achieved when Ti(SO4)2 nanospheres transformed to TiO2 nanospheres during solvothermal process. PVP was firstly coated on the surface of the Ti(SO4)2 nanospheres and successively combined with the TiO2 nanospheres. PVP decomposed during the calcinations and carbon was further doped to the TiO2 nanospheres. The codoped TiO2 nanospheres had an average diameter of 70nm and highly porous structure. The final products exhibited significant red shift of the light absorption edge in comparison with that of the Degussa P25. These results demonstrated that doped TiO2 can be synthesized from reactants or surfactants containing doped elements without additional dopants.

Synthesis, growth and characterisation of tetrathiourea cadmium tetrathiocyanato zincate single crystals

Tetrathiourea cadmium tetrathiocyanato zincate (TCTZ) has been synthesised by the chemical reaction method. The solubility of the synthesised material was determined in water, acetone and water–acetone mixed solvents. Based on the solubility studies, the single crystals of TCTZ were grown from the 3:1 water–acetone mixed solvent by the solvent evaporation method. The crystallinity of the grown crystals was proved from the powder XRD data. TCTZ was found to crystallise in tetragonal symmetry with non-centrosymmetric space group I¯4. The presence of functional group and the coordination of the metal with the ligands were proved from the FTIR studies. The compound exhibits good physicochemical stability up to 182°C. The UV transparency cut off wavelength of TCTZ was found to be 290nm and the complex is transparent (69%) over the entire range of visible region showing that it is a good candidate for NLO applications. The growth feature of the TCTZ single crystals was observed by etching studies, which reveals the formation of layer growth pattern. The mechanical property of the crystal was estimated by Vickers hardness test.

Smoothening electrospinning and obtaining high-quality cellulose acetate nanofibers using a modified coaxial process

The present research investigates a modified coaxial process for smoothening electrospinning of cellulose acetate (CA) and obtaining its nanofibers with high quality. With 11 w/v% CA in mixed solvent of acetone and N,N-dimethylacetamide (DMAc) (v:v, 3:1) as electrospinnable core fluid, different solvents (acetone, DMAc and their mixture) are taken as sheath fluids to conduct the modified process. SEM observations demonstrate that the modified process is effective in retarding the clogging of spinneret for a smooth electrospinning and in obtaining high quality CA nanofibers in terms of structural uniformity, diameters, and their distributions. The mechanism about the influence of sheath fluid on the process and the formation of nanofibers is discussed. The key for the modified coaxial process is the reasonable selection of sheath fluids and a sheath-to-core flow rate ratio matching the drawing process of core CA fluid during the electrospinning. The present paper provides a simple method to implement the modified coaxial process for smoothening the electrospinning and obtaining polymer nanofibers with high quality.

Palladium(II) Containing γ-Keggin Silicodecatungstate That Efficiently Catalyzes Hydration of Nitriles

A mixture of Pd(OAc)(2) and TBA(4)[γ-SiW(10)O(34)(H(2)O)(2)] (TBA-SiW10, TBA = [(n-C(4)H(9))(4)N](+)) showed high catalytic activities for hydration of various kinds of structurally diverse nitriles including aromatic, aliphatic, heteroaromatic, and double bond-containing ones. For hydration of 3-cyanopyridine, the turnover frequency was 860 h(-1), and the turnover number reached up to 670. A dipalladium-substituted γ-Keggin silicodecatungstate, [γ-H(2)SiW(10)O(36)Pd(2)(OAc)(2)](4-) (I), was successfully synthesized by the reaction of [γ-SiW(10)O(34)(H(2)O)(2)](4-) with Pd(OAc)(2) in a mixed solvent of acetone and water. The crystal structure of I was a monomeric, dipalladium-substituted, γ-Keggin silicodecatungstate with bidentate acetate ligands. Compound I showed similar activities and selectivities to those of a simple mixture of Pd(OAc)(2) and TBA-SiW10. The kinetic, mechanistic, and density functional theory calculation studies show that the dipalladium site plays an important role in the present hydration, and the nucleophilic attack of a hydroxide or water to the nitrile carbon atom is included in the rate-determining step.

A Facile Titanium Glycolate Precursor Route to Mesoporous Au/Li4Ti5O12 Spheres for High-Rate Lithium-Ion Batteries

A facile, green strategy is explored to synthesize mesoporous Au/Li(4)Ti(5)O(12) spheres based on in situ conversion of titanium glycolate in LiOH aqueous solution. Compared with TiO(2) precursors, titanium glycolate possesses some strengths: (i) fast and easy preparation; (ii) direct reaction with LiOH without introduce of TiO(2) impurity. In the synthesis, the produced chemical waste is only the mixed solvent of acetone and ethylene glycol (EG). Furthermore, acetone and EG in chemical waste can be easily separated by distillation and reused in the next synthesis process due to the great difference between their boiling points. In particular, the as-prepared mesoporous Au/Li(4)Ti(5)O(12) spheres combines the advantages of large specific surface area (166 m(2)/g) and good electronic conduction enhanced by Au nanoparticles when used as an anode electrode material. The electrochemical tests show that the mesoporous Au/Li(4)Ti(5)O(12) spheres display excellent high rate capability and cycling performance.

Electrostatic Spray Deposition of Highly-Crystalline TIPS Pentacene Thin Films for Fabrication of Organic Field-Effect Transistors

ABSTRACTThis paper demonstrates that electrostatic spray deposition (ESD) method is a promising solution process to fabricate highly-crystalline organic films (6,13-bis(triisopropylsilylethynyl) pentacene; TIPS pentacene) for the use in bottom-contact organic field-effect transistors (OFETs). We obtained large crystalline domains (i.e., molecularly-oriented domains) by using an o-DCB:acetone mixed solvent (1:1), and observed good transistor behavior in an OFET having the channel length of 20 μm.

FeCl3 · 6H2O-Catalyzed Acceleration of the Acylation of Sodium Azide with N-Acylbenzotriazoles

Catalyzed by ferric chloride hexahydrate (FeCl3 · 6H2O), the acylation of sodium azide with N-acylbenzotriazoles was greatly accelerated in a mixed solvent of acetone and water. Thus, good to excellent yields of a variety of acyl azides were obtained at room temperature in a short time. Furthermore, because of the complete conversion of N-acylbenzotriazoles and the easy removal of the by-product, purification by column chromatography was no longer required, which made the protocol suitable for large-scale preparation.

A novel protocol for the preparation of uniform polymer microspheres with high yields through step polymerization of isophorone diisocyanate

AbstractUniform polymer microspheres with neat surface are of high interests. Precipitation polymerization of vinylic monomers remains a very limited process owing to very low monomer concentration allowed. Here, a fully novel protocol for the production of uniform polymeric microspheres is presented. Using one single monomer, isophorone diisocyanate, highly monodisperse polyurea microspheres were achieved with very high yield in a very short time period via precipitation polymerization in water–acetone mixed solvent. Results demonstrated that the ratio of water–acetone and polymerization temperature played important roles in the process. The size of the microspheres was readily adjustable by varying monomer concentration, water/acetone ratio or polymerization temperature. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011

A novel process for precipitation of ultra-fine particles using sub-critical CO 2

Supercritical CO 2 has been utilized as solvent, cosolvent or antisolvent in several processes for production of ultra-fine solid particles with narrow size distribution. The key to the precipitation of such particles is to produce a very large, rapid and uniform supersaturation in the solution of a solid substance. This can be achieved either by a rapid and large reduction in the temperature of solution or by drastically increasing the CO 2 solubility for imparting the antisolvent effect. Most of these CO 2 processes require high-pressure pumps, specially designed nozzles and accurate control of process parameters. In order to obviate these requirements, a simple technique of precipitation by pressure reduction over the gas-expanded liquids (PPRGEL), such as CO 2-expanded organic solutions has been utilized to impart a large, uniform and rapid reduction of temperature in the solution for instantaneous precipitation of ultra-fine particles. This process utilizes sub-critical CO 2 at relatively low pressures of 40–70 bar and near ambient temperature of 303 K for creating a temperature drop of 30–70 K in the solution within seconds, without using any specially designed nozzle or high-pressure pumps. The present paper validates the process principle for precipitation of Zinc acetate (ZnAc) nanoparticles from its organic solution in a mixed solvent of acetone and dimethyl sulfoxide (DMSO). Nanoparticles are produced with the average size of 20–250 nm (from 100 ml of solution in a high-pressure vessel of 1.09 L working volume), and vary in shapes such as long needles, rods and near spherical depending on pressure (40–70 bar at 303 K), solid concentration (0.01–0.05 g/ml) and addition of stabilizer.

Determination of Indoxacarb Residue in Foodstuffs of Plant and Animal Origin by GC-ECD and LC-MS/MS

An effective method for the trace analysis of indoxacarb residue in foodstuffs of plant and animal origin [grapefruit, ginger, fresh soybean, bamboo shoot, qing-gen-cai (cruciferous vegetable), chicken, fish, and pork] was developed using gas chromatography (GC-ECD) and liquid chromatography tandem mass spectrometry (LC-MS/MS). Samples were extracted using acetone and n-hexane mixed solvent (1:2, v/v) and then purified using solid-phase extraction (SPE) columns. The extracts were analyzed using GC-ECD and LC-MS/MS. The multiple reaction monitoring (MRM) scheme used involved transitions of the precursor ions to selected two product ions in which one pair for identification was m/z 529 → 293 and another pair for quantification was m/z 529 → 249. The detection limits (LODs) of the method were 0.0015 and 0.0006 mg kg −1, and the quantification limits (LOQs) were 0.005 and 0.002 mg kg −1 for GC-ECD and LC-MS/MS, respectively. The relative standard deviations (RSDs) of recovery for indoxacarb were lower than 15% in 10 types of agro-products. Ten repetitive determinations of recovery achieved good reproducibility for indoxacarb and the recovery ranged from 72.08 to 113.74%. The proposed procedure was applied to the analysis of several real samples of different origin from Fujian Province, China, and 299 samples were screened for indoxacarb residue, of which 5 positive samples were found.

Extraction and HPLC Characterization of Chlorogenic Acid from Tobacco Residuals

Chlorogenic acid is a highly valuable natural polyphenol compound used in medicine and industries. Its current commercial sources are from plant extracts of Lonicera japonica Thunb and Eucommia ulmoides Oliver. These sources are limited and expensive. On the other hand, tobacco residuals contain chlorogenic acid and other natural polyphenol compounds. Large quantities of tobacco residuals are produced each year as waste materials from tobacco manufacturing, potentially providing an alternative commercial source of chlorogenic acid and other valuable compounds. In this paper, microwave and ultrasound extractions of chlorogenic acid with mixed solvent were studied. Total polyphenol concentrations in extract solutions obtained with different extraction methods were analyzed with the method of ferrous tartrate and UV‐Vis spectrophotometry and compared. The extraction solutions were also characterized for polyphenol compositions with the method of HPLC. Experimental results indicated that high extract concentrations of chlorogenic acid were obtained with a mixed solvent of acetone and water (1:2 v/v). A total polyphenol concentration of up to 4.87 mg/ml and a chlorogenic acid concentration of up to 2.12 mg/ml were achieved. The application of microwave and ultrasound significantly increased the extract concentrations. The extraction time needed was also much reduced. HPLC analysis indicated that acetone water mixed solvent extraction achieved much higher relative concentrations of chlorogenic acid to other compounds in the extract solutions. These results indicted that fast and effective extraction of chlorogenic acid from tobacco residuals were achieved.

Growth and characterization of l-prolinium picrate single crystal: A promising NLO crystal

l-Prolinium picrate was synthesized and its solubility in the mixed solvent of acetone and water was estimated. Employing temperature reduction method crystals of size 22×4×3 mm 3 were grown. The cell dimensions were obtained by single-crystal X-ray diffraction study. FT-IR, UV–vis–NIR and fluorescence spectral analyses were carried out for the grown crystals. The optical band gap estimated for this crystal is about 2.4 eV. Thermogravimetric study was carried out to determine the thermal properties of the grown crystal. Kurtz powder second harmonic generation (SHG) efficiency measurement revealed that the SHG efficiency is about 52 times that of potassium dihydrogen orthophosphate. Mechanical strength was tested by Vicker's microhardness test.