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1.

This study is aimed at developing a promising method of strontium impurity separation from concentrated molybdenum solutions originating from molybdenum recycling from irradiated CerMet nuclear fuels with an isotopically tailored molybdenum matrix. Strontium sorption onto thirteen inorganic or composite absorbers from a slightly alkaline (pH 9.1) ammonium molybdate surrogate solution was studied. Based on the evaluation of weight distribution ratios, their dependence on molybdenum concentration and pH, and kinetics of sorption, calcium activated barium sulfate (Ba(Ca)SO4) was identified as the most promising material. In a dynamic column experiment performed with the Ba(Ca)SO4-PAN absorber, 2700 BV of the solution with cSr = 10−4 mol L−1 could be treated with a breakthrough of lower than 1% and 100% breakthrough was not achieved even after processing almost 7000 BV of the feed.

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2.

In this paper, a novel pipette tip micro-solid phase extraction based on molecularly imprinted polymer as a selective sorbent was developed and applied for extraction, pre-concentration and high-performance liquid chromatographic determination of trace amounts of malachite green (MG), rhodamine B (RB), methyl orange (MO) and acid red 18 (AR) dyes in seawater samples. Different parameters affecting the extraction efficiency such as type and volume of eluent solvent, sample volume, number of cycles of extraction and desorption, amount of sorbent and pH of the sample solution were evaluated using one-variable-at-a-time and response surface methodology. In order to optimize dyes extraction, seven factors in three levels were used for Box–Behnken experimental design. Under optimum extraction condition, pH of sample solution was 3.1 for MG, 3.0 for RB, 7.1 for MO and 6.1 for AR; volume of eluent solvent (HCl, 0.5 mol L−1) was 200 µL; volume of the sample solution was 10 mL (for MG) and 4 mL (for RB, MO and AR); the concentration of triton X-114 was 0.085 (MG), 0.10 (RB), 0.08 (MO) and 0.075 (AR) % v/v; the number of extraction cycles was 10 (MG), 6 (RB), 5 (MO) and 7 (AR); the number of elution cycles was 10, 6, 5 and 9, respectively, for MG, RB, MO and AR; NaCl concentration was 0.4 mol L−1; and amount of MIP was 2.0 mg for all dyes. The linear range of calibration curves was 0.5–250.0 µg L−1 for malachite green and methyl orange and 0.5–150.0 µg L−1 for both rhodamine B and acid red 18. The detection limits calculated to be 0.083, 0.10, 0.12 and 0.17 µg L−1 for MG, RB, MO and AR, respectively. The developed protocol was successfully used for determination of dyes in seawater of Chabahar Bay. The mean recoveries were ranged between 76.1 and 97.3% by mean relative standard deviations of 1.2–7.1%.

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3.
In this paper, a combined hollow fiber-based liquid three-phase microextraction and voltammetric method are applied for the first time as a highly selective and sensitive method of electrochemical analysis. Desipramine, used as a model compound was extracted from 8 mL aqueous solution (donor phase, 0.10 mol L−1 NaOH) through a thin phase of propyl benzoate inside the pores of a polypropylene hollow fiber and finally into a 10 μL acidic acceptor solution inside the hollow fiber. Three microelectrodes designed and constructed for the purposes of this study were placed into the two ends of the hollow fiber inside the acceptor solution, and voltammetric analysis was performed in-situ during the extraction. After 15 min, the final stable signal was used for analytical applications. Under the optimized conditions, an enrichment factor of 301 was achieved and the relative standard deviation (R.S.D.) of the method was 6.2% (n = 5). The calibration curve was obtained in the range of 5-5000 nmol L−1 with a reasonable linearity (R2 > 0.988) and the limit of detection (LOD) was found to be 0.8 nmol L−1. Finally, the applicability of the proposed method was evaluated by extraction and determination of desipramine in plasma and urine samples without any dilutions.  相似文献   

4.
This paper reports silica gel loaded with p-tert-butylcalix[8]arene as a new solid phase extractor for determination of trace level of uranium. Effective extraction conditions were optimized in column methods prior to determination by spectrophotometry using arsenazo(III). The results showed that U(VI) ions can be sorbed at pH 6 in a mini-column and quantitative recovery of U(VI) (>95–98%) was achieved by stripping 0.4 mol L−1 HCl. The sorption capacity of the functionalized sorbent is 0.072 mmol uranium(VI) g−1 modified silica gel. The relative standard deviation and detection limit were 1.2% (n = 10) for 1 μg uranium(VI) mL−1 solution and 0.038 μg L−1, respectively. The method was employed to the preconcentration of U(VI) ions from spiked ground water samples.  相似文献   

5.
Graphene oxide (GO) was chemically modified with a poly(propylene)imine Generation 3.0 dendrimer (DAB-Am-16). The characterization, structure and properties of hybrid graphene oxide/DAB-Am-16 dendrimer was studied by Raman spectroscopy, Fourier-Transforming Infrared Spectroscopy (FT-IR), X-Ray Photoelectron Spectroscopic (XPS), X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Thermogravimetric analysis. After functionalized the hybrid material (GOD) can interact with copper and subsequently with hexacyanoferrate (III) ions (GODHCu). The GODHCu incorporated into a graphite paste electrode (20% w/w) was applied to an electrocatalytic detection of neurotransmitter l-dopamine using differential pulse voltammetry. The analytical curve showed a linear response in the concentration range from 1.0 × 10−7 to 1.0 × 10−5 mol L−1 with a corresponding equation Y(A) = 1.706 × 10−5 + 0.862 [l-dopamine] and a correlation coefficient r2 = 0.998. The detection limit was 6.36 × 10−7 mol L−1 with a relative standard deviation of ±4% (n = 3) and an amperometric sensitivity of 0.862 A/mol L−1.  相似文献   

6.
A multicommutation-based flow system with photometric detection was developed, employing an analytical microsystem constructed with low temperature co-fired ceramics (LTCC) technology, a solid-phase reactor containing particles of Canavalia ensiformis DC (urease source) immobilized with glutaraldehyde, and a mini-photometer coupled directly to the microsystem which monolithically integrates a continuous flow cell. The determination of urea in milk was based on the hydrolysis of urea in the solid-phase reactor and the ammonium ions produced were monitored using the Berthelot reaction. The analytical curve was linear in the urea concentration range from 1.0 × 10−4 to 5.0 × 10−3 mol L−1 with a limit of detection of 8.0 × 10−6 mol L−1. The relative standard deviation (RSD) for a 2.0 × 10−3 mol L−1 urea solution was lower than 0.4% (n = 10) and the sample throughput was 13 h−1. To check the reproducibility of the flow system, calibration curves were obtained with freshly prepared solutions on different days and the RSD obtained was 4.7% (n = 6). Accuracy was assessed by comparing the results of the proposed method with those from the official procedure and the data are in close agreement, at a 95% confidence level.  相似文献   

7.

Alumina nanofluids are one of the most useful nanofluids, especially for increasing the thermal conductivity. Due to importance of porous media in the improvement of heat transfer, this study investigates the transport and retention of gamma alumina/water nanofluid in the water-saturated porous media. For this purpose, alumina nanofluids were introduced to the porous media consisting of water-saturated glass beads possessing various pH values (4, 7 and 10) and different ionic strengths (0.001 M of KCl, CaCl2, AlCl3, K2SO4, CaSO4, Al2(SO4)3, K2CO3 and CaCO3). Then the break through curve of each experiment was drawn and modeled by combining classical filtration theory with advection–dispersion equation. Single collector efficiency (η0) and attachment efficiency (α) were calculated by classical filtration theory. Also curve fitting of experiments and modeling was achieved by minimizing the sum of squared residuals, to calculate retardation factor (R) and hydrodynamic dispersion coefficient (D) of each experiment. According to the results, in general, increase in pH and ionic strength will enhance the removal rate coefficient, retardation factor and retention while decreasing the steady-state break through concentration and the hydrodynamic dispersion coefficient. The opposite of this rule was observed and analyzed for aluminum salts. The lowest retention of nanoparticles at 31.04% can be related to their transport in background solution with pH = 4 [α = \(3.87 \times 10^{ - 2}\), Katt = \(3.33 \times 10^{ - 3}\) (min−1), R = 3.93, D = 0.91 (cm2 min−1)], and the highest retention in nanoparticle content of 94.29% was observed in background solution containing CaCO3 [α = \(14.33 \times 10^{ - 2}\), Katt = \(137.82 \times 10^{ - 3}\) (min−1), R = 12.02, D = 0.62 (cm2 min−1)]. Therefore, chemistry of water plays an important role in transport and retention parameters. The classical filtration theory and the advection–dispersion model are able to perfectly model and quantify the parameters of the alumina nanofluid transport in saturated porous media.

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8.

The lattice Boltzmann method is used to study natural convection of a CuO/water nanofluid in a hollow cavity. The hollow walls are fixed at a uniform temperature, and the effect of an applied magnetic field is examined. The Koo–Kleinstreuer–Li model, which accounts for nanoparticle’s Brownian motion, is used to gain the nanofluid effective thermal conductivity and nanofluid viscosity. The mechanisms how the inclination angle of magnetic field, Hartmann number, Rayleigh number, hollow width and nanoparticle volume fraction affect the streamlines, isotherms and rate of heat transfer are also studied. The results show that the average Nusselt number is increased by incrementing the nanoparticle volume fraction, Ra, magnetic field inclination angle and hollow width, but decreased by the Ha. For L = 0.4, the value of Ra where the dominant mechanism of heat transfer is changed from conduction to convection is larger than 105. But for L = 0.48 or 0.56, the turning point of the dominant heat transfer mechanism is at Ra < 105. Besides, at L = 0.4 or 0.48, the average Nusselt numbers in hot walls are higher than those in cold wall, but the opposite trend is found at L = 0.56.

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9.

The removal of U(VI) by biochar fibers from aqueous solutions has been investigated prior and after MnO2 surface-deposition. The removal efficiency has been studied as a function of pH, U(VI) concentration, ionic strength, temperature and contact time. The fibers morphology and surface complexes were analyzed by SEM–EDX and FTIR, respectively. Evaluation of the experimental data indicates that the composite presents extraordinary adsorption capacity (qmax = 3.8 mmol g−1, 904 mg g−1), which is attributed to the formation of inner-sphere surface complexes, and that the adsorption reaction is a relatively fast, endothermic and entropy-driven process.

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10.

Microbial hyaluronic acid (HA) production has been preferred rather than extraction from animal tissue for medical and cosmetic applications. In this context, to obtain an economically competitive HA production by Streptococcus zooepidemicus, culture conditions were studied to improve the polymer production in sugarcane molasses. The highest HA production by S. zooepidemicus ATCC 39920 achieved was 2.825 g. L−1 in a 4.5 L bioreactor with controlled pH (8.0) and medium containing molasses (85.35 g.L−1 total sugar) pretreated with activated charcoal and yeast extract (50 g.L−1). The HA produced exhibited a high molecular weight of 1.35 × 103 kDa and the DPPH radical scavenging activity of the polymer at 1 g.L−1 was 41 %. The FTIR and UV-Vis spectra showed no substantial differences in the spectral pattern between produced and standard HA. This study is a promising strategy for sugarcane molasses application by producing high value-added products such as hyaluronic acid.

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11.

In this work, two newly sensitive and selective Al(III)-modified carbon paste electrodes (MCPEs) were developed based on diphenylcarbazone (DPC) modifier mixed with tricresyl phosphate plasticizer and either graphite powder (electrode I) or graphite powder mixed with graphene (electrode II). The potentiometric performance characteristics of the two electrodes were scrutinized and discussed. The proposed sensors showed a high electrochemical response in the linear concentration range of 1.0 × 10−6 to 1.0 × 10−2 mol L−1 with a good Nernstian slopes of 20.12 ± 0.30 mV decade−1 and 20.63 ± 0.66 mV decade−1 and limits of detection of 9.0 × 10−7 and 8.5 × 10−7 mol L−1 for electrode (I) and electrode (II), respectively. Both electrodes showed a fast response time and reasonable thermal stability. The potentiometric response of the DPC-based electrodes was independent on the pH of the tested solutions in ranges of 2.5–5 and 2.5–5.5 for electrode (I) and electrode (II), respectively. The two electrodes can be also used in partially non-aqueous medium containing up to 20% (v/v) acetone or methanol with no significant changes in the working concentration ranges or the slopes. The proposed electrodes showed fairly good discriminating ability toward Al(III) ions in comparison with many other metal ions. The electrodes were applied successfully for Al(III) ions determination in drainage water, spiked tap water and pharmaceutical preparation samples. Furthermore, the electrode surfaces were characterized using energy-dispersive X-ray (EDX) and scanning electron microscopic (SEM) as surface characterization techniques and Fourier Transform Infrared (FT-IR) technique to confirm the interaction between Al(III) and DPC.

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12.
A sensitive and straightforward liquid–liquid–liquid microextraction method was developed to preconcentrate and cleanup antidepressants, including mirtazapine, venlafaxine, escitalopram, fluoxetine, and fluvoxamine, from biological samples before analyzing with high-performance liquid chromatography. The essential novelty of this study is using magnetic ionic liquids as the extraction phase in the lumen of hollow fiber and preparing a liquid magnetic stir bar. In this method, polypropylene hollow fiber was utilized as the permeable membrane for the analyte extraction. Six magnetic ionic liquids consisting of the transition metal and rare earth compounds were synthesized and then hollow fiber lumen was injected as acceptor phase to extract the antidepressants. Besides, 3-pentanol as a water-immiscible solvent was impregnated in the hollow fiber wall pores. The effective factors in the method were optimized with the central composition design. The resultant calibration curves were linear over the concentration range of 0.8–400.0 ng mL−1 (R2 ≥ 0.996). The method displayed the proper detection limit (0.11–0.24 ng mL−1), the reasonable limit of quantification (≤0.79 ng mL−1), wide linear ranges, high preconcentration factors (≥294.3), and suitable relative standard deviation (2.31–5.47%) for measuring antidepressant medications. Analysis of human milk and urine samples showed acceptable recoveries of 96.5–103.8% with excellent relative standard deviations lower than 5.95%.  相似文献   

13.
A new and fast hollow fiber based liquid phase microextraction (HF-LPME) method using volatile organic solvents coupled with high-performance liquid chromatography (HPLC) was developed for determination of aromatic amines in the environmental water samples. Analytes including 3-nitroaniline, 3-chloroaniline and 4-bromoaniline were extracted from 6 mL basic aqueous sample solution (donor phase, NaOH 1 mol L−1) into the thin film of organic solvent that surrounded and impregnated the pores of the polypropylene hollow fiber wall (toluene, 20 μL), then back-extracted into the 6 μL acidified aqueous solution (acceptor phase, HCl 0.5 mol L−1) in the lumen of the two-end sealed hollow fiber. After the extraction, 5 μL of the acceptor phase was withdrawn into the syringe and injected directly into the HPLC system for the analysis. The parameters influencing the extraction efficiency including the kind of organic solvent and its volume, composition of donor and acceptor phases and the volume ratio between them, extraction time, stirring rate, salt addition and the effect of the analyte complexation with 18-crown-6 ether were investigated and optimized. Under the optimal conditions (donor phase: 6 mL of 1 mol L−1 NaOH with 10% NaCl; organic phase: 20 μL of toluene; acceptor phase: 6 μL of 0.5 mol L−1 HCl and 600 m mol L−1 18-crown-6 ether; pre-extraction and back-extraction times: 75 s and 10 min, respectively; stirring rate: 800 rpm), the obtained EFs were between 259 and 674, dynamic linear ranges were 0.1-1000 μg L−1 (R > 0.9991), and also the limits of detection were in the range of 0.01-0.1 μg L−1. The proposed procedure worked very well for real environmental water samples with microgram per liter level of the analytes, and good relative recoveries (91-102%) were obtained for the spiked sample solutions.  相似文献   

14.
《Comptes Rendus Chimie》2017,20(4):415-423
The optical and colorimetric properties of a new chemosensor 4-((2,4-dichlorophenyl)diazenyl)-2-(3-hydroxypropylimino)methyl)phenol (L) for cyanide ions were investigated by the naked-eye detection and UV–vis spectroscopy. This receptor reveals visual changes toward CN anions in aqueous media. No significant color changes were observed upon the addition of any other anions. The cyanide recognition properties of the receptor through proton-transfer were monitored by UV–vis titration and 1H NMR spectroscopy. The binding constant (Ka) and stoichiometry of the formed host–guest complex were calculated by the Benesi–Hildebrand (B–H) plot and Job's plot method, respectively. The detection limit of the probe towards CN was 1.03 × 10−6 mol L−1, which is lower than the maximum value of cyanide (1.9 × 10−6 mol L−1) permitted by the World Health Organization in drinking water. Thus, this chemosensor was sensitive enough to detect cyanide in aqueous solutions. 1H NMR experiments were conducted to investigate the nature of interaction between the receptor and CN anions. Notably, the designed sensor can be applied for the rapid detection of cyanide anions in the basic pH range and also under physiological conditions, for practical purposes for a long duration. The sensing behavior of the receptor was further emphasized by computational studies. Quantum-chemical calculations and molecular studies via Density Functional Theory (DFT) were carried out to supplement the experimental results.  相似文献   

15.

In this research, electrospun polycaprolactam nanofibers were collected on a fine stainless steel mesh sheet without a binder, and a layer of conductive polyaniline was chemically deposited on the nanofibers. The polyaniline immobilized on the polycaprolactam nanofibers provided high electrical conductivity, acceptable mechanical stability, and a large surface area. This assembly was then used as a working electrode in electrochemically controlled solid-phase microextraction (EC-SPME), a fast and environmentally friendly method. The polymer layers were characterized by SEM and FTIR techniques. Significant factors affecting the EC-SPME efficiency were investigated, including the desorption conditions, the sorbent used, the pH of the sample solution, the extraction voltage, the extraction time, and the ionic strength. Under the optimum conditions, the limits of detection and quantification for the target analytes were 0.9–1.8 μg L−1 and 3.0–6.1 μg L−1, respectively. The linear dynamic range was 5–2000 μg L−1, with R2 > 0.993. The method was coupled with HPLC analysis and applied to the determination of angiotensin ΙΙ receptor antagonists (ARA-ΙΙs) in human plasma, and relative recoveries of 91.1–104.3% with RSDs of ≤8.3% were obtained.

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16.

The extraction behavior of Nd(III) and Eu(III) with 0.05 mol dm−3 furosemide in benzyl alcohol as single acidic extractant and then with equimolar (0.05 mol dm−3) synergic mixture of furosemide as acidic extractant and tribenzylamine as neutral donor in benzyl alcohol has been studied from aqueous solutions of pH 1 to 6. The effect of various parameters and of various cations and anions on the extraction of these metal ions was investigated. The composition of the extracted adducts was determined by slope analysis method that came out to be [(M(FS)2)+ (CH3COO)] and [M(FS)3·3TBA] where M = Nd(III) and Eu(III).

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17.

A new electrochemical biosensor is developed for the detection of diazinon. For this purpose, a glassy carbon electrode is modified with MWCNTs and poly-l-lysine to immobilize a double-strain DNA (ds-DNA) on the surface of the electrode. In the first step, the interaction of diazinon with ds-DNA is transduced by electrochemical impedance spectroscopy and UV–Vis spectroscopy to monitor the intercalation of diazinon with DNA helix. This interaction leads to reduced interfacial charge-transfer resistance (Rct). The difference in the Rct before and after the interaction is considered as a suitable signal for diazinon detection. The proposed biosensor has a low detection limit (0.3 nmol L−1), a wide linear dynamic range (0.001‒100 µmol L−1), and high selectivity for the determination of diazinon. Finally, the performance of the biosensor for detecting of diazinon is verified in real samples such as river water, agricultural wastewater, lettuce juice, and tomato juice.

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18.
Carrier-mediated three-phase hollow fiber microextraction combined with high-performance liquid chromatography-ultra violet detection (HPLC-UV) was applied for the extraction and determination of propylthiouracil in biological samples. Propylthiouracil (PTU) was extracted from 7.5 mL of the basic solution (the source phase) with pH 12 into an organic phase (n-octanol containing 6% (w/v) of Aliquat 336 as the carrier) impregnated in the pores of a hollow fiber, and finally was back extracted into 24 μL of the acidic solution located inside the lumen of the hollow fiber (the receiving phase). The extraction was performed through the gradient of counter ion from the source to the receiving phase. The effects of different variables on the extraction efficiency were studied simultaneously using an experimental design. A half-fractional factorial design was employed for screening to determine the variables significantly affecting the extraction efficiency. Then, the factors with significant effect were optimized using a central composite design (CCD) and the response surface equations were developed. The optimal experimental conditions obtained from this statistical evaluation included: source phase, pH 12; temperature, 25 °C; extraction time, 40 min; counter ion concentration, 2 mol L−1 of NaClO4; organic solvent 6% of Aliquat in octanol and without salt addition in the source phase. Under the optimized conditions, the preconcentration factors were between 125 and 198 and also the limit of detections (LODs) ranged from 0.1 μg L−1 to 0.4 μg L−1 in different biological samples. The calibration curve was linear (r2 = 0.998) in the concentration range of 0.5-1000 μg L−1. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of PTU in human plasma and urine as well as the bovine milk and meat samples in microgram per liter, and suitable results were obtained (RSDs < 6.3%).  相似文献   

19.
Behavior of cadmium(II) in aqueous solutions irradiated by accelerated electrons was studied. A concentration of 8.8 × 10−4 mol L−1 of cadmium dissolved from Cd(NO3)2 requires dose of 15 kGy to be effectively removed from the system containing 1 × 10−2 mol L−1 of HCOOK as a scavenger of OH radicals. The positive effect of deaeration with N2O or N2 was observed in the range of lower doses. The addition of solid modifiers (bentonite, active carbon, zeolite, Cu2O, NiO, TiO2 and CuO) reduced the effectivity of radiation removal of cadmium. Product of irradiation is CdCO3. On the contrary, in the system with cadmium dissolved from CdCl2 radiation reduction takes place. Systems contained organic complexants (ethylene diamine tetraacetic acid–EDTA, citric acid) were also studied. The solutions of Cd(NO3)2 containing initial concentration 2.37 × 10−4 mol L−1 of CdII were mixed with 3 × 10−4 mol L−1 EDTA. In this system the efficient degradation proceeds up to 90% at a dose of 45 kGy with addition of 5 × 10−3 mol L−1 carbonate (pH 10.5). The product of irradiation is CdCO3. The presence of 1 × 10−2 mol L−1 of HCOOK in the solution is necessary for radiation removal of cadmium complexed with citric acid (1 × 10−3 mol L−1) at pH 8. With increasing concentration of HCOOK (up to 5 × 10−2 mol L−1) decreases the pH value necessary for the radiation induced precipitation of cadmium. The best result was obtained in the system containing zeolite as a solid modifier.  相似文献   

20.
A viscometric study of two polyelectrolytes, chitosan (CH, with 94% deacetylation degree, in a solute-mixture of acetic acid (0.1 mol L−1) and sodium chloride (0.2 mol L−1) and sodium alginate (SA, with 62% M-units, in sodium chloride (0.1 mol L−1), was performed at 25 °C. Five different equations were applied to calculate intrinsic viscosity [η]: Huggins, Kraemer and Schulz-Blaschke (SB) by graphical extrapolation; Solomon-Ciuta, Deb-Chanterjee and again SB, by faster single-point determination. Viscometric constants were calculated employing graphical extrapolation equations. Average molar mass (‾Mv) values were determined by applying the Mark-Houwink-Sakurada equation. For the samples analyzed, Huggins equation was the most suitable to calculate [η] and‾Mv by graphical extrapolation for chitosan, while Schulz-Blaschke and Solomon-Ciuta were adequate for single-point determinations of sodium alginate. Viscometric constants indicated that the aqueous mixture of acetic acid and sodium chloride is a poor solvent for chitosan, while sodium alginate is well solvated by aqueous sodium chloride.  相似文献   

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