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1.
A new type of sulfonate gemini surfactant with three lipophilic alkyl chains (3C10-DS) was synthesized, and the structure of the product was confirmed by using the infrared spectrum and mass spectrum. Its critical micelle concentration (CMC) is 0.41 mmol/L, one order of magnitude lower than those of convectional (single-chain) surfactants, and the minimum surface tension is 27.6 mN/m. The interfacial tension (IFT) between the compound system of 3C10-DS and petroleum sulfonate (PS) and the simulated oil reaches ultra-low levels (10?3 mN/m), and there exists significant synergistic effect between 3C10-DS and PS. The compound flooding system consisting of polymer and the mixture of 3C10-DS and PS can effectively improve oil recovery for high-medium permeability cores and have a good application prospect in enhancing oil recovery.  相似文献   

2.
Higher alcohol has been considered as a potential fuel additive. Higher alcohol, including C2–C4 alcohol was synthesized by catalytic conversion of syngas (with a ratio of CO/H2?=?1) derived from natural gas over modified Cu/ZnO/Al2O3 catalyst. Modified Cu/ZnO/Al2O3 catalysts promoted by alkali metal (Li) for higher alcohol synthesis (HAS) were prepared at different pH (6, 6.5, 7, 8, and 9) by co-precipitation to control Cu surface area and characterized by N2 physisorption, XRD, SEM, H2-TPR and TPD. The HAS reaction was carried out under a pressure of 45 bar, GHSV of 4000 h?1, ratio of H2/CO?=?1, and temperature ranges of 240 and 280 °C. It was found that the malachite phase of copper causes the size of copper to be small, which is suitable for methanol synthesis. Methanol and HAS share a common catalytic active site and intermediate. It was also found that the productivity to higher alcohol was correlated with Cu surface area.  相似文献   

3.
A novel solid ternary complex, [Nd(C6H4NO2)2·C9H6NO·2H2O], was synthesized in a water bath (333.15 K) by three kinds of reagents: neodymium chloride, vitamin B3 (C6H5NO2), and 8-hydroxylquinoline (C9H7NO). Its composition and structure were characterized by elemental analysis, IR spectra, UV spectra, molar conductance, and thermogravimetric analysis. During the process of coordination, C6H5NO2 was bidentate-coordinated with Nd3+ in the form of an acidic group by removing the proton; hydroxyl oxygen atom and heterocyclic nitrogen atom of C9H7NO formed a chelate ring. Particularly, in this article, a thermochemical cycle in the calorimetric solvent (V HCl:V DMF:V EtOH = 3:1:1) was designed on the basis of Hess’s law. At 298.15 K, the dissolution enthalpies of the reactants and products were determined by a advanced solution–reaction isoperibol microcalorimeter, respectively. According to the above results and relevant literature data, the standard molar enthalpy of formation of [Nd(C6H4NO2)2·C9H6NO·2H2O], was estimated to be $ \Updelta_{f} H_{m}^{\Uptheta} $ [[Nd(C6H4NO2)2·C9H6NO·2H2O(s)], 298.15 K] = ?(2,129.1 ± 2.5) kJ mol?1.  相似文献   

4.
《Analytical letters》2012,45(1):110-118
The new ionic liquid-modified polymer sorbent was developed by surface chemical modification of the synthesized polymer particles using ionic liquids. The obtained ionic liquid-modified polymer was successfully used as a special sorbent in a solid-phase extraction (SPE) process to isolate caffeine and theophylline from green tea. A comparison of different SPE cartridges using the blank polymer, C18, and ionic liquid-modified polymer revealed that the highest recovery was obtained using ionic liquid-modified polymer sorbent. Quantitative analysis was carried out by using a C18 column (5 µm, 150 × 4.6 mm) as an analytical column. Good linearity was obtained from 5 × 10?4 to 0.5 mg/mL (r2>0.999) for the two analytes with relative standard deviations <4.5%.  相似文献   

5.
Methods are described for the determination of ultratrace amounts of copper and cadmium in seawater by graphite furnace atomic absorption spectrometry with flow-injection, microcolumn preconcentration. A new type of C18 column loaded with sodium diethyldithiocarbamate (sodium-DDC) was used to extract copper and cadmium from seawater as the DDC chelates. The analytical effects of the pH of the mixture of the sample and sodium-DDC solutions and the concentration of the chelating reagent were studied. Sodium-DDC-loaded columns and unloaded C18 columns with different shapes and volumes were compared. To determine copper in seawater, a simple aqueous calibration was made with a mixture of palladium and magnesium nitrate as a matrix modifier, while for cadmium no matrix modifier was necessary. This method required only small seawater volumes, 600 and 400 μl for the determination of copper and cadmium respectively, with preconcentration factors of 15-fold for copper and 10-fold for cadmium. Detection limits for the preconcentration of aqueous solutions of copper and cadmium were 0.024 and 0.004 μg liter−1 (3σ), respectively. Results for determinations of copper and cadmium in National Research Council of Canada, CASS-2, Nearshore Seawater Reference Material showed no significant differences between the certified values and the measured values, based on Student′s t test at the 95% confidence level. The relative standard deviations of the various measurements varied between 2 and 8%.  相似文献   

6.
《Analytical letters》2012,45(11):1921-1930
This paper describes a simple and sensitive method for the determination of manganese in human urine by graphite furnace atomic absorption spectroscopy (GFAAS), which includes sample preparation by microwave digestion. Matrix modifier combinations, the digestion power, pyrolysis, and atomization temperatures were optimized. A mixture of 5.0 µg Pd(NO3)2 and 3.2 µg Mg(NO3)2 modifier presented the best performance. The optimal temperatures for pyrolysis and atomization were 1500°C and 1950°C, respectively. The GFAAS method was compared to inductively coupled plasma–mass spectrometry (ICP–MS) for the determination of manganese in urine. Analytical figures of merit for GFAAS and ICP–MS were: accuracy (3.46%, 2.19%), precision (3.61%, 5.84%), LOD (0.109 µg · L?1, 0.015 µg · L?1), LOQ (0.327 µg · L?1, 0.045 µg · L?1), and recovery (80–100%, 74–89%). Both methods were employed for the determination of Mn in urine and the results were compared statistically.  相似文献   

7.
The atmospheric corrosion of copper and silver influenced by graphite and alumina as particulate matter (PM) in an environment containing 200 μg m?3 SO2 + 150 μg m?3 NO2 at 85% RH and 25 °C was analyzed. Different proportions of PM mixture conditions were used, and the corrosion rate was followed using gravimetric analysis. Results of linear sweep voltammetry (LSV) and coulometric reduction (CR) indicated that larger corrosion rates were obtained in the presence of deposited PM. Under present exposure conditions, copper corrosion rate was larger than silver corrosion rate. X-ray diffraction (XRD) shows the presence of cuprite (Cu2O) and brochantite (Cu4SO4(OH)6) in the case of copper and achantite (Ag2S) in the case of silver.  相似文献   

8.
A new modified carbon paste electrode for determination of Cu2+ made in our laboratory that used a new synthesized macrocycle 7,16-diaza-1-thia-4,10,13,19-tetraoxa-6,17-dioxo-2,3;20,21-dinaphtho-cyclouneicosane as modifier. This sensor exhibits a good affinity toward copper (II) ions over a wide variety of other metal ions. The electrode exhibits a Nernstian slope of 30 (±0.5) mV per decade for copper (II) ions over a wide concentration range (1.0 × 10?8–1.0 × 10?2 mol L?1), with a limit of detection of 7.0 × 10?9 mol L?1 (~0.45 ppb). It has a response time of 30 s and can be used for at least 3 months without any considerable divergence in responses. The potentiometric response of the electrode is independent of the pH of test solution in the pH range 3.5–7.5. Finally, it was successfully used as an indicator electrode for determination of copper (II) in real samples such as Karoun river and tap water.  相似文献   

9.
《Analytical letters》2012,45(5-6):592-602
The aim of the present work was to develop and validate a rapid and accurate method of arsenic determination in leachate samples by electrothermal atomic absorption spectrometry. Leachate samples from sanitary landfills are considered difficult samples to analyze due to severe matrix interferences. A comparative study of various chemical modifiers was performed: Pd, Mg, Au, Pt, Ru, Rh, Ir, C6H8O7 (citric acid), Pd + Mg, Ir + Mg, and the permanent modifier Zr – Ir.

Among the modifiers tested, the mixture 5 µg Ir + 40 µg Mg provided the best performance, followed by the permanent modifier Zr – Ir (a coating of 200 µg Zr + 20 µg Ir). The permanent modifier was finally chosen due to the decreased background signal and sufficient sensitivity.

In order to investigate the presence of matrix interference and exploit the possibility of performing calibrations by simple aqueous solutions, calibration with aqueous standards, matrix matched standards and with standard additions was performed. It was observed that, in the presence of the Zr – Ir permanent modifier, the slopes of the calibration curve and the matrix-matched/standard addition curves were statistically different (checked by t-test). The recoveries from matrix-matched calibrations for three concentration levels were ranged between 96.4% and 100%. Precision experiments were also performed and the relative standard deviation (%RSD) for four different concentrations was ≤10%. The method was applied to the determination of arsenic in leachate samples collected in the solid waste sanitary landfill of Ano Liossia, Attika, Greece.  相似文献   

10.
Titanium butyl phosphates (TiBP) synthesized by reacting Ti(SO4)2 with a mixture of mono-(C4H9PO4H2) and dibutyl phosphates ((C4H9)2PO4H) in aqueous ethanol solution at 25 °C were characterized by various conventional techniques. XRD pattern of TiBP possessed a peak at 2θ?=?5.5° and a broad hump at 2θ?=?15–30°. This fact indicated that the material was composed of a multilayer alternating bilayer of butyl groups of the phosphates and amorphous titanium phosphate phase. The TiBP was spherical particles with a size of ca. 100 nm and the chemical formula of this material was Ti((C4H9O)2PO2)x(C4H9OPO3)y(OH)z. The TiBP possessed a UV absorption property due to charge transfer of O2? ? Ti4+. The layered structure of TiBP was exfoliated in ethanol at 25 °C up to TiBP concentration of 1.0?×?105 ppm to form nanosheet. The nanosheet dispersing solution exhibited a UV absorption property and the property depends on nanosheet concentration.  相似文献   

11.
A series of dissymmetric gemini imidazolium surfactants with different spacer length ([CmCsCnim]Br2, m + n = 24, m = 12, 14, 16, 18; s = 2, 4, 6) were synthesized and characterized by 1H NMR and ESI-MS spectroscopy. Their adsorption and thermodynamic properties were investigated by the surface tension and electrical conductivity methods. Consequently, the surface activity parameters (cmc, γcmc, πcmc, pC20, cmc/C20, Γmax, Amin) and thermodynamic parameters (ΔGmθ, ΔHmθ, ΔSmθ) were obtained. The effects of the dissymmetry (m/n) and the spacer length (s) on the surface activity and micellization process of surfactants have been discussed in detail.  相似文献   

12.
Lignin, the world's largest resource of renewable aromatics, with annually roughly 50 million tons of accruing technical lignin, mainly Kraft lignin, is highly underdeveloped regarding the production of monoaromatics. We demonstrate the oxidative depolymerization of Kraft lignin at 180 °C to produce vanillin 1 in yields up to 6.2 wt % and 92 % referred to the maximum yield gained from the quantification reaction utilizing nitrobenzene. Using peroxodicarbonate (C2O62−) as “green” oxidizer for the degradation, toxic and/or harmful reagents are prevented. Also, the formed waste can serve as makeup chemical in the pulping process. Na2C2O6 is synthesized in an ex-cell electrolysis of aqueous Na2CO3 at BDD anodes, achieving a yield of Na2C2O6 with 41 %. At least, the oxidation and degradation of Kraft lignin is analysis via UV/Vis and NMR spectroscopy.  相似文献   

13.
Cobalt ferrite magnetic nanoparticles (CoFe2O4-MNPs) were synthesized by hydrothermal and co-precipitation methods using different precursors such as nitrates, chlorides, and acetates, at different concentrations with/without surfactant under different growth conditions. The structural and morphological analyses reveal the formation of a single-phase CoFe2O4 in nanoplatelet-shaped NPs with average particle size between 11 and 26 nm depending on synthesis condition. The specific surface area of these NPs obtained by hydrothermal method was ~ 34 m2 g?1. Electrochemical performances of the obtained nanoparticles in a three-electrode configuration with a 6 M KOH electrolyte revealed a specific capacitance (C s) of 429 F/g at 0.5 A/g, with excellent capacitance retention of 98.8% after 6000 cycles at 10 A/g for the electro-active NPs synthesized by hydrothermal method at 200 °C for 18 h.  相似文献   

14.
The reaction of 2‐amino‐benzothiazole with allyl bromide resulted in a mixture of 2‐imino‐3‐allyl‐benzothiazole and 2‐imino‐3‐allyl‐benzothiazolium bromide.Using such a mixture and copper(II) chloride in acetonitrile solution in alternating‐current electrochemical synthesis crystals of the [(CuCl)C10H10SN2] ( I ) have been obtained. The same procedure, performed in ethanol solution, has led to formation of [C10H11SN2+]2[Cu2Cl4]2? ( II ). In the same manner the bromine derivative [C10H11SN2+]2[Cu2Br4]2? ( III ) has been synthesized. All three compounds were X‐ray structurally investigated. I :monoclinic space group P21/n, a = 13.789(6), b = 6.297(3), c = 13.830(6) Å, β = 112.975(4)°, V = 1105.6 (9) Å3, Z = 4 for CuCl·C10H10 SN2 composition. Compounds II and III are isomorphous and crystallize in triclinic space group. II a = 7.377(3), b = 8.506(3), c = 9.998(4) Å, α = 79.892(10)°, β = 82.704(13)°, γ = 78.206(12)°, V = 601.9(4) Å3, Z = 1. III a = 7.329(2), b = 8.766(3), c = 10.265(3) Å, α = 79.253(9)°, β = 82.625(9)°, γ = 77.963(9)°, V = 630.9(3) Å3, Z = 1. In the structure I [(CuCl)C10H10SN2] building blocks are bound into infinitive spiral‐like chains via strong N‐H..Cl hydrogen bonds. In the zwitter‐ionic II and III compounds copper and halide atoms form centrosymmetric [Cu2X4]2? anions, which are interconnected via N‐H..X hydrogen bonds into infinite butterfly‐like chains. The strongest Cu‐(C=C) π‐interaction has been observed in structure I , where copper possesses coordination number 3. Increasing copper coordination number to 4 in II as well as replacing chlorine atoms by bromine ones in III suppresses markedly this interaction.  相似文献   

15.
CuFe2(C2O4)3·4.5H2O was synthesized by solid-state reaction at low heat using CuSO4·5H2O, FeSO4·7H2O, and Na2C2O4 as raw materials. The spinel CuFe2O4 was obtained via calcining CuFe2(C2O4)3·4.5H2O above 400 °C in air. The CuFe2(C2O4)3·4.5H2O and its calcined products were characterized by thermogravimetry and differential scanning calorimetry, Fourier transform FT-IR, X-ray powder diffraction, scanning electron microscopy, energy dispersive X-ray spectrometer, and vibrating sample magnetometer. The result showed that CuFe2O4 obtained at 400 °C had a saturation magnetization of 33.5 emu g?1. The thermal process of CuFe2(C2O4)3·4.5H2O experienced three steps, which involved the dehydration of four and a half crystal water molecules at first, then decomposition of CuFe2(C2O4)3 into CuFe2O4 in air, and at last crystallization of CuFe2O4. Based on KAS equation, OFW equation, and their iterative equations, the values of the activation energy for the thermal process of CuFe2(C2O4)3·4.5H2O were determined to be 85 ± 23 and 107 ± 7 kJ mol?1 for the first and second thermal process steps, respectively. Dehydration of CuFe2(C2O4)3·4.5H2O is multistep reaction mechanisms. Decomposition of CuFe2(C2O4)3 into CuFe2O4 could be simple reaction mechanism, probable mechanism function integral form of thermal decomposition of CuFe2(C2O4)3 is determined to be 1 ? (1 ? α)1/4.  相似文献   

16.
Supercapacitor electrode material MnO2 was prepared by liquid co-precipitation with different concentration of anionic surfactant sodium dodecyl sulfate (SDS). As evidenced by X-ray diffraction, the obtained MnO2 are all typical amorphous α-MnO2 with poor crystallinity. Scanning electron microscopy reveals that the dispersity of MnO2 initially get better and then worse with the increase of SDS, and the particle sizes first become smaller then larger as well. It is worthwhile noting that the morphology of MnO2 tested by transmission electron microscopy undergoes a changeable process: fibrous, pine needle like, cotton like, round bubble like, flocculent, and nervous tissue like as SDS increases. Through cyclic voltammetry and galvanostatic charge/discharge tests, SDS addition amount 0.2 g (0.017 mol L?1) is found to be the optimal effect value, and the as-prepared Mn-0.2 obtains the highest specific capacitance (C sp) of 154.5 F g?1 at a current density of 500 mA g?1. Compared with the sample Mn-0 synthesized without SDS, the C sp increases by about 50 % (±5 %), which can be attributed to its largest Brunauer–Emmett–Teller–specific surface area of 255.9 m2 g?1, best particle dispersity, and smallest particle size of approximately 50–80 nm. Meanwhile, the rate capability and cycle stability of Mn-0.2 also improves obviously, and the equivalent series resistance decreases a lot, only 0.120 Ω.  相似文献   

17.
This work compares the performance of dispersive liquid–liquid method (DLLME) as a prior step for determining copper by flame atomic absorption spectrometry (FAAS), when using the ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate (C4MIm-PF6) or the IL-based surfactant 1-hexadecyl-3-butylimidazolium bromide (C16C4Im-Br) as extractant solvents. For the water-insoluble C4MIm-PF6, the most conventional DLLME mode using acetonitrile as dispersive solvent was employed. For the water-soluble C16C4Im-Br, the in situ DLLME mode with lithium bis[(trifluoromethane)sulfonyl]imide (Li-NTf2) as metathesis reagent was employed. In both approaches, some effective parameters such as volumes of extractant and dispersive solvents, concentration of complexing agent, pH of sample solution, salting-out effect and final diluting solvent to ensure compatibility with FAAS, were properly optimised. The optimum conditions for the IL-DLLME method using C4MIm-PF6 were: 100 μL of neat C4MIm-PF6, 1 mL of acetonitrile, 10 mL of water, no control of pH for environmental waters, NaCl content of 23 g L?1, diethyl dithiocarbamate (DDTC) as complexing agent at 10 mg L?1 and final dilution of the micro-droplet with acetonitrile up to 70 µL. The optimum conditions for the in situ IL-DLLME method using C16C4Im-Br were: 0.8 mL of acetonitrile, 10 mL of water containing C16C4Im-Br at 25.2 mmol L?1, final dilution step of the micro-droplet with 200 µL of acetonitrile and remaining conditions as those of C4MIm-PF6. The analytical performance of both methods was similar, being slightly better for the IL-DLLME method using C4MIm-PF6, with limits of detection (LOD) of 3.3 µg L?1 (versus 5.1 µg L?1 when using C16C4Im-Br), precision values as intraday relative standard deviation (RSD in %) lower than 8.8% (being of 10% for the C16C4Im-Br method) and an enrichment factor of 54 (being 27 when using C16C4Im-Br). The DLLME-FAAS method with C4MIm-PF6 was used in the analysis of environmental waters with successful performance, with relative recoveries of 110% and 105%, and interday precision with RSD values of 21% and 7.4% for spiked levels of 60 and 160 µg L?1, respectively. The results obtained when analysing an urban wastewater sample coming from an inter-laboratory exercise was comparable to those obtained for other 93 laboratories. The method was also valid for the determination of Cu2+ in presence of foreign ions commonly found in natural waters.  相似文献   

18.
1,3-Bis(4-aminophenoxy)benzene (TPER) and poly(amic acid) based on TPER and pyromellitic dianhydride (PMDA) were synthesized. After imidization of the poly(amic acid), polyimide based on TPER and PMDA was obtained. The melting process and the specific heat capacity (C p) of TPER were examined by DSC and microcalorimetry, respectively. The melting enthalpy, the melting entropy, and the C p for TPER were obtained. The enthalpy change, the entropy change, and the Gibbs free energy change for TPER were obtained within 283 and 353 K. The thermal decomposition reaction mechanism of the polyimide is classified from the TG–DTG experimental data, and the thermokinetic parameters of the thermal decomposition reaction are E a = 296.87 kJ mol?1and log (A/s?1) = 14.41.  相似文献   

19.
The complexes [Ni(L1)(pyc)2]·2H2O (1) (L1 = C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane; Hpyc = pyrazinecarboxylic acid) and [Cu(L2)(H-cpdc)] (2) (L2 = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.18,07.12]docosane; H2-cpdc = cyclopropanedicarboxylic acid) have been synthesized and structurally characterized. The crystal structure of complex 1 shows a distorted octahedral coordination geometry around the nickel(II) center, with four secondary amines in the equatorial positions and two nitrogen atoms of the pyc? ligands in the trans positions. In complex 2, the coordination environment around the copper(II) center is a Jahn–Teller distorted octahedron with four Cu–N bonds and two axial Cu–O bonds. The electronic spectra, electrochemical and TGA behavior of the complexes are significantly affected by the nature of the axial pyc? and H-cpdc? ligands.  相似文献   

20.
The bis(hydroxamato)oxovanadium(IV) complexes of composition [VO(IAH)2)] (I), [VO(IBH)2)] (II) and [VO(ICH)2)] (III) (where IAH = indole-3-acetohydroxamate; (C9H8NCONHO?); IBH = indole-3-butyrohydroxamate; (C11H12NCONHO?); ICH = indole-2-carbohydroxamate; (C8H6NCONHO?)) synthesized form the reactions of VOSO4·5H2O with bi-molar amounts of potassium salts of the respective hydroxamic acids in methanol have been characterised by elemental analyses, magnetic moment measurements and IR spectral studies. The thermal behaviour of complexes has been studied by TG and DTA techniques. Thermograms indicated that all complexes decompose in two steps yielding [VO(IAH)], [VO(IBH)] and [VO(ICH)] as intermediate of respective complexes and VO2 as the final product of decomposition in each case. From the initial decomposition temperatures (IDT), the order of thermal stability for the complexes has been inferred as II > I > III.  相似文献   

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