Effects of the mineral phase and valence of vanadium on vanadium extraction from stone coal

The influence of roasting on the leaching rate and valence of vanadium was evaluated during vanadium extraction from stone coal. Vanadium in stone coal is hard to be leached and the leaching rate is less than 10% when the raw ore is leached by 4 mol/L H₂SO₄ at 90℃ for 2 h. After the sample is roasted at 900℃ for 2 h, the leaching rate of vanadium reaches the maximum, and more than 70% of vanadium can be leached. The crystal of vanadium-bearing mica minerals decomposes and the content of V(V) increases with the rise of roasting temperature from 600 to 900℃, therefore the leaching rate of vanadium increases significantly with the decomposition of the mica minerals. Some new phases, anorthite for example, form when the roasting temperature reaches 1000℃. A part of vanadium may be enwrapped in the sintered materials and newly formed phases, which may impede the oxidation of low valent vanadium and make the leaching rate of vanadium drop dramatically. The leaching rate of vanadium is not only determined by the valence state of vanadium but also controlled by the decomposition of vanadium-bearing minerals and the existence state of vanadium to a large extent.     

Gas chromatographic method for the determination of hexaconazole residues in black tea

A highly reliable, quantitative and sensitive analytical method for determining the residues of the fungicide, hexaconazole in black tea is described. The proposed method is based on liquid-liquid extraction followed by gas chromatographic determination, using nitrogen phosphorus detector （GC-NPD） for the identification and quantitation of hexaconazole. The most appropriate solvent mixture for extracting hexaconazole residues from black tea was n-hexane：acetone at 1 ：1 （v/v）. The extract was cleaned up by adsorption column chromatography using activated florisil. Performance of the method was assessed by evaluating quality parameters such as recovery value, repeatability, reproducibility, linearity and limits of detection and quantitation. When the method was assessed for repeatability, the percentage of recovery ranged between 86% and 96% while the relative standard deviation was between 0.30% and 2.35%. In studies on reproducibility the recovery ranged from 81% to 85% and relative standard deviation from 1.68% to 5.13%, implying that the method was reliable. A field trial was conducted to verify the application of this method with real samples. Results prove that the validated method was suitable for extracting hexaconazole residues.     

Influence of chitosan characteristics on the properties of biopolymeric chitosan–montmorillonite

Chitosan–montmorillonite is a modified montmorillonite in which the sodium ions in montmorillonite layers are replaced by biopolymeric chitosan. The effects of characteristics of chitosan (i.e. molecular weight and degree of deacetylation) and the chitosan/montmorillonite mass ratio on the properties of chitosan–montmorillonite were investigated. Thermogravimetric analysis, zeta potential and X-ray diffraction results confirmed intercalation of chitosan into montmorillonite layers. An interaction between chitosan and montmorillonite was revealed by FTIR and the zeta potential. The amount of chitosan intercalated into the montmorillonite layers depended on the characteristics of chitosan, with the largest amounts of intercalated chitosan achieved by addition of chitosan with a molecular weight of 71,000 g/mol or a degree of deacetylation of 80% at a fixed chitosan/montmorillonite mass ratio of 2:1. The resulting chitosan–montmorilllonite had good adsorbent properties, especially for adsorption of cationic dyes, and also inhibited E. coli by almost 100%. The chitosan–montmorillonite may be useful as a functional material for dye adsorption and antibacterial applications.     

Binding of vanadium compounds perturbs conformation and aggregation state of insulin

The interactions between zinc-free insulin and vanadium compounds, NaVO3, VO(acac)2 and VO(ma)2, have been investigated by fluorescence spectroscopy, circular dichroism (CD) and Fourier-transformed infrared (FT-IR) spectroscopy. The results showed that binding of vanadium compounds produced a static quenching of the intrinsic fluorescence of insulin. The apparent association constants were determined to be (0.17±0.01)×104 L*mol-1 for NaVO3, (2.8±0.2)×104 L*mol-1 for VO(acac)2, and (4.0±0.1)×104 L*mol-1 for VO(ma)2, respectively. The light scattering intensity of insulin decreased upon incubation with the vanadium compounds, suggesting the disaggregation of insulin. The attenuation of the band at 273 nm of insulin CD spectra also supported the disaggregation of insulin observed above. A new band at 1650～1653 cm-1 appeared in the FT-IR spectra of insulin upon incubation with the vanadium compounds, indicating the formation of an α-helix structure at B (9-19) motif. This α-helix structure suggests a structural change of insulin from an extended conformation (T state) to a helical conformation (R state), which is essential for binding of insulin to its receptor. In conclusion, binding of vanadium compounds results in conformational changes and disaggregation of insulin. These changes might account for the enhancement of binding affinity for insulin to its receptor in the presence of vanadium compounds.     

THE TRANSFER BEHAVIOUR OF SOME CATIONS AT WATER／NITROBENZENE INTERFACE BY SEMIDIFFERENTIAL CYCLIC VOLTAMMETRY

The transfer of Sr~(2+) and Ba~(2+) ion, facilitated by 18-Crown-6 present in the aqueous phase, and of succinylcholine ion at w/nb interface were investigated by semi-differential cyclic voltammetry. A good polarographic curve of succinylcholine ion dissolved in water was obtained in the system of 0.01 mol/l LiCl (w)——0.01 mol/l TBATPB (nb). The peak current is directly proportional to the concentration of SC~(2+) ion. It can be used for the determination of SC and the detection limit is 1.05×10~(-5) mol/l.The apparent D~w and D~(nb) have been estimated. The transfer of Sr~(2+) and of Ba~(2+) at the interface are facilitated by 18-Crown-6 present in the aqueous phase and the peak current is directly proportional to the concentration of 18-Crown-6 in water. This method can be used for the determination of the complexing agent and for the stability constant of the complex formed in the aqueous phase.All the experimental results are in keeping with the theoretical.     

HPLC Determination of Ascorbic Acid Using Luminol-Cu(Ⅱ) Chemiluminescence-Application to the Analysis of Juice Beverage

The chemiluminescence (CL) of luminol-Cu(Ⅱ) was applied to HPLC determination of ascorbic acid, which was separated by a C18 reverse-phase column with a mobile phase of 0.25 mol/L HAc. The eluted ascorbic acid was mixed with 0.3 mmol/L luminol and 0.05 mol/L CuSO4. The light emission from the reaction of Cu(Ⅱ) oxidized ascorbic acid and luminol was detected by a modified luminometer. The detection limit was 3.6×10-6 mol/L for ascorbic acid at a S/N ratio of 3, and the linear calibration range was 2×10-4- 2×10-3 mol/L. The relative standard deviation for 5 replicate injections of 1×10-3 mol/L ascorbic acid was calculated as 4.3 %. The method was successfully applied to determination of ascorbic acid in juice beverage.     

Determination of sulfonamides with fluorescent inclusion complex of carbonic anhydrase and dansylamide

A new fluorimetric method for determination of sulfonamides was described based on the formation of a fluorescent inclusion complex of carbonic anhydrase(CA) with dansylamide(DNSA). The binding of DNSA to CA resulted in an enhancement in the fluorescence emission at 460 nm with excitation at 280 nm. Dissociation constants were determined for the carbonic anhydrase sulfonamide complexes. Linear calibration graphs of sulfonamides were obtained within a concentration range of 0- 0.058 μg/mL for DNSA; 0-0.344 μg/mL for sulfanilamide (SAN) and 0-0.286 μg/mL for P toluenesulfonamide (PTSN). The relative standard deviations were within 1.8%-4.2%. Limits of detection for DNSA, SAN and PTSN were 0.84, 19.5 and 6.1 ng/mL, respectively. The method was applied to the determination of sulfonamides in cow milk at ng/mL level.     

Preconcentration and Separation of Trace Copper in Water Samples with Nanometer-Size TiO2 Colloid and Determination by FAAS

A new absorbent of nanometer-size TiO2 colloid for Cu(Ⅱ) was studied in this work. The adsorption rate could reach above 99% when the pH values were at the range of 5-6. The adsorption balance time, adsorption capacities, and the eluent were investigated. A novel method of trace Cu(Ⅱ) preconcentration and separation with nanometer-size titanium dioxide colloid and determination by flame atomic absorption spectrometry (FAAS) was advanced. The detection limit (3σ) of the method was 1.15 μg· L~(-1) , and the relative standard deviation (R.S.D) was 1.53% (n=6). Environmental sample experiments were also conducted to test the feasibility of the method, and it came out that the recovery rates were between 95.9% and 97.8%.     

A method for haplotype inference in general pedigrees without recombination

The abundance of single nucleotide polymorphisms (SNPs) makes the haplotype-based method instead of single-maker-oriented method the main approach to association studies on QTL mapping. The key problem in haploptype-based method is how to reconstruct haplotypes from genotype data. Directly assaying haplotypes in diploid individuals by experimental methods is too expensive, therefore the in silico haplotyping-determination methods are the major choice at the present. This paper presents a rapid and reliable algorithm for haplotype reconstruction for tightly linked SNPs in general pedigrees. It is based on six rules and consists of three steps. First, the parental origins of alleles in offspring are assigned conditional on genotypes in parent-offspring trios; second, the redundant haplotypes are eliminated based on the six rules; and finally, the most likely haplotype combinations are chosen via maximum likelihood method. Our method was verified and compared with PEDPHASE by simulated data with different pedigree sizes, numbers of loci, and proportions of missing genotypes. The result shows that our algorithm was superior to PEDPHASE in terms of computing time and accuracy of haplotype estimation. The computing time for 100 runs was 10―15 times less and the accuracy was 4%―10% higher than PEDPHASE. The result also indicates that our method was very robust and was hardly affected by pedigree size, number of loci, and proportion of missing genotypes.     

A simple spectroscopic method for the quantification of gold nanoparticle number concentration in water and fetal bovine serum solutions

In this work,we developed a facile and low-cost method with sufficient sensitivity for the quantitative determination of gold nanoparticles(GNPs)number concentration in water and fetal bovine serum solutions.The Au(III)digested from GNPs was reduced to Au(I)presumably by the thiol group of 2-mercaptobenzimidazole,then the Au(I)–thiolate complex was formed,the concentration of which is determined by absorbance at 300 nm.The number concentration of GNPs can be converted using microscopic images and simple calculations.The interference of serum can be avoided in this method.The limit of detection(LOD)of GNPs was calculated as 2.1 910-12mol/L in water solution and 1.3 9 10-11mol/L in fetal bovine serum(FBS)solution.This method provides a simple and fast way to determine the concentration of GNPs,which can be in carried out in the routine laboratory practice.     

Roasting and leaching behaviors of vanadium and chromium in calcification roasting–acid leaching of high-chromium vanadium slag

Calcification roasting–acid leaching of high-chromium vanadium slag (HCVS) was conducted to elucidate the roasting and leaching behaviors of vanadium and chromium. The effects of the purity of CaO, molar ratio between CaO and V₂O₅ (n(CaO)/n(V₂O₅)), roasting temperature, holding time, and the heating rate used in the oxidation–calcification processes were investigated. The roasting process and mechanism were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), and thermogravimetry–differential scanning calorimetry (TG–DSC). The results show that most of vanadium reacted with CaO to generate calcium vanadates and transferred into the leaching liquid, whereas almost all of the chromium remained in the leaching residue in the form of (Fe_0.6Cr_0.4)₂O₃. Variation trends of the vanadium and chromium leaching ratios were always opposite because of the competitive reactions of oxidation and calcification between vanadium and chromium with CaO. Moreover, CaO was more likely to combine with vanadium, as further confirmed by thermodynamic analysis. When the HCVS with CaO added in an n(CaO)/n(V₂O₅) ratio of 0.5 was roasted in an air atmosphere at a heating rate of 10℃/min from room temperature to 950℃ and maintained at this temperature for 60 min, the leaching ratios of vanadium and chromium reached 91.14% and 0.49%, respectively; thus, efficient extraction of vanadium from HCVS was achieved and the leaching residue could be used as a new raw material for the extraction of chromium. Furthermore, the oxidation and calcification reactions of the spinel phases occurred at 592 and 630℃ for n(CaO)/n(V₂O₅) ratios of 0.5 and 5, respectively.     

Enhancement of transfection efficiency for HeLa cells via incorporating arginine moiety into chitosan

Arginine-rich peptides have attracted considerable attention due to their distinct internalization mechanism. It was reported that arginine and guanidino moieties were able to translocate through cell membranes and played a critical role in the process of membrane permeation. In this work, arginine was conjugated to the backbone of chitosan to form a novel chitosan derivative, arginine modified chitosan (Arg-CS). Arg-CS/DNA complexes were prepared according to the method of coacervation process. The physicochemical properties of Arg-CS and Arg-CS/DNA complexes were characterized and the transfection activity and efficiency mediated by Arg-CS/DNA complexes were investigated taking HeLa cells as target cells. Arg-CS was characterized by FTIR and 13C NMR. Arg-CS/DNA polye- lectrolyte complexes were investigated by agarose gel retardation, dynamic light scattering (DLS) and atomic force microscopy (AFM). The results revealed that the Arg-CS/DNA complexes started to form at N/P ratio of 2:1, and the size of particles varied from 100 to 180 nm. The cytotoxicity of Arg-CS and their complexes with plasmid DNA were determined by MTT assay for HeLa cells, and the results suggested that Arg-CS/DNA complexes were slightly less toxic than Arg-CS. Moreover, the derivative alone and their complexes showed significantly lower toxicity than PEI and PEI/DNA complexes, respectively. Taking HeLa cells as target cells and using pGL3-control as reporter gene, the luciferase expression mediated by Arg-CS was greatly enhanced to about 100 folds compared with the luciferase expression mediated by chitosan at different pH media. These results suggest that Arg-CS is a promising candi- date as a safe and efficient vector for gene delivery and transfection.     

Folate-Polyethyleneimine Grafted Polymer Multilayer Hollow Microcapsules as a Slow-Release Carrier of Doxorubicin

A novel biodegradable and biocompatible multilayer hollow microcapsules,modified by folate-conjugated polyethyleneimine(PEI),as targeted and sustained release carriers of doxorubicin(DOX),were successfully synthesized using the sequential layer-by-layer electrostatic assembly technique from the sacrificial microtemplates(CaCOj/CMC,spherical,1.7 μm) with chitosan(CS) and sodium carboxymethyl cellulose(CMC) as the polycation and polyanion polyelectrolyte.Scanning electron microscope(SEM) observation showed that the diameter of the seven assembly multilayer microparticles was about 2.0 μm with relatively regular sphere.After the microparticle cores was removed by complexation with ethylene diamine tetraacetic acid(EDTA) for calcium ions,the range of 200- 300 nm wall thickness of microcapsules was built,and it made the forming microcapsules to be stable.Thermogravimetric analysis confirms the deposition and modification total amount of polymer on the microtemplates is about33.5%.The assembly microparticles were modified by introducing PEI,and the grafting rate of folate could reach 20.0%.It was 4times that of traditional method.The high grafting rate helped to improve targeting action of microcapsules.The deposition of DOX was prominent and the encapsulation efficiency was 96.9%,and the plateaued release of loaded drug reached 78%in pH 7.4 buffer solution,and then in pH 5.7 showed significantly a slow release.     

Determination of Four Chiral Pesticides in Soil by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

The enantiomer residues of metalaxyl, napropamide, triticonazole and metconazole were detected in soil by Qu EChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The soil sample was extracted with acetonitrile containing 1% acetic acid and purified using Qu ECh ERS method. Quantitative analysis for the enantiomers of these four chiral pesticides was performed in MS in multi-response monitoring(MRM) mode by external standard method. All enantiomers showed good linearity in the range of 0.5 to 50 μg/L. The average recoveries of enantiomers in soil were 81.74% to 105.79% with relative standard deviations(RSDs) from 3.69% to 7.86%. The method quantitative limit(MQL) was 5.3-30.3 ng/kg. The method can be used for rapid screening and determination of chiral pesticides in soil.     

An improved implementable process for the synthesis of zeolite 4A from bauxite tailings and its Cr<Superscript>3+</Superscript> removal capacity

A simple and practical method for the synthesis of zeolite 4A from bauxite tailings is presented in this paper. Systematic investigations were carried out regarding the capacity of zeolite 4A to remove Cr(Ⅲ) from aqueous solutions with relatively low initial concentrations of Cr(Ⅲ) (5–100 mg·L-1). It is found that the new method is extremely cost-effective and can significantly contribute in decreasing environmental pollution caused by the dumping of bauxite tailings. The Cr(Ⅲ) removal capacity highly depends on the initial pH value and concentration of Cr(Ⅲ) in the solution. The maximum removal capacity of Cr(Ⅲ) was evaluated to be 85.1 mg·g-1 for zeolite 4A, measured at an initial pH value of 4 and an initial Cr(Ⅲ) concentration of 5 mg·L-1. This approach enables a higher removal capacity at lower concentrations of Cr(Ⅲ), which is a clear advantage over the chemical precipitation method. The removal mechanism of Cr(Ⅲ) by zeolite 4A was examined. The results suggest that both ion exchange and the surface adsorption-crystallization reaction are critical steps. These two steps collectively resulted in the high removal capacity of zeolite 4A to remove Cr(Ⅲ).     

Chemiluminescence Determination of Tetracycline and Oxytetracycline in Pharmaceutical Preparations Using Ru(bipy)32+-Cerium(Ⅳ) System

A new chemiluminescence (CL) method for the determination of tetracycline and oxytetracycline is developed, based on the CL reaction of tetracycline and oxytetracycline with Ru(bipy)32+ and Ce (Ⅳ). In sulfuric acid medium, the CL emission is generated upon continuous oxidation of Ru(bipy)32+ by cerium (Ⅳ).The emission intensity is greatly enhanced when tetracycline and oxytetracycline are introduced into the reaction system after acid degradation. Under the optimum conditions, the calibration curves are linear over therange of 8. 0× 10-8～4. 0× 10-6 mol/L for tetracycline and of 2. 0× 10-7～4. 0× 10-5 mol/L for oxytetracycline, with the detection limits are 4. 2 × 10-8 mol/L for tetracycline and 1.5 × 10-7 mol/L for oxytetracydine, respectively. The proposed method was used for the determination of tetracycline and oxytetracycline in pharmaceutical formulations with good results.     

Measurement of the Average Molecular Weight of Cotton Cellulose Crosslinked by a Polycarboxylic Acid at Different pH Using Multiple Angle Light Scattering Photometer in a DMAc/LiCl Solvent System

Durable press finishing of cotton fabrics with polycarboxylic acid increases fabric wrinkle-resistance at the expense of its mechanical strength. Severe tensile strength loss is the major disadvantage for wrinkle resistant cotton fabrics. Tensile strength loss of cotton fabric crosslinked by a polycarboxylic acid can be attributed to depolymerization and crosslink of cellulose molecules. Measurement of the molecular weight of cotton fabric before and after crosslinked by polycarboxylic acids can offer a possibility of direct understanding of the depolymerization. In this research, a multiple angle laser light scattering photometer was used to determine the absolute molecular weight of cotton fabric treated with BTCA at different pH and then hydrolyzed with 0.5 M NaOH solution at 50℃ for 144 h. The results indicate that average molecular weights of cotton fabric treated with polycarboxylic acids at different pH are almost the same.     

Sintering behaviour of feldspar and influence of electric charge effects

The characterization of feldspar for electric porcelain and the behaviour of these materials after heating at 1230℃ were studied. X-ray diffraction (XRD) and scanning electronic microscopy (SEM) were used to identify the present phases and the densification level. Feldspar sand was treated by flotation. The floated feldspar is constituted by microcline, quartz, and minor amounts of albite. The microstructure of sintered feldspar at 1230℃ is essentially vitreous with open microporosities. The dielectrical properties of composites were characterized by using the induced courant method (ICM), which indicates that the charge trapping capacity depends on the mineralogical and chemical composition of feldspar.     

Behaviors of helium in vanadiu m: Stabil ity, diffusi on, vacancy trapping and ideal tensi le strength

The behaviors of helium in vanadium including stability,diffusion,and its interaction with vacancy as well as its effects on the ideal tensile strength was investigated by a frst-principles method.The activation energy barrier of helium was calculated to be 0.09 eV,which is consistent with the experimental result.The results indicated that the vacancy can lead to a directed helium segregation into the vacancy to form a helium cluster since the vacancy provides a "lower atomic and electron density region" as a large driving force for helium binding.It is easy for a mono-vacancy to trap helium and form a Hen V complex.The frst-principles computational tensile test demonstrates that helium obviously decreased the tensile strength of vanadium.     

Synthesis and Characterization of Magnetic SiO_2 Nanoparticles Loaded with Naproxen for Anti-inflammatory Therapy

The aim of this study is to synthesize of magnetic SiO2 nanoparticles(MSNPs)loaded with Naproxen(NAP-MSNPs)for targeting anti-flammatory therapy.The Fe3O4 nanoparticles were coated with a thin layer of silica by stber method and the drug was encapsulated in it simultaneously.The optimal conditions were investigated for the synthesis of MSNPs.The shape,size,and phase structure of NAP-MSNP were characterized by transmission electron micrographs(TEM)and X-ray diffraction(XRD).The drug encapsulation efficiency was confirmed by FT-IR and measured by UV spectrometry.The NAP-MSNPs show the response at the external magnetic field and the drug could be released readily from NAP-MSNPs.All of these facts suggest the NAP-MSNPs could be applied in a promising drug release-controlling system for targeting anti-inflammatory therapy.