Selective determination of beryllium(II) ion at picomole per decimeter cubed levels by kinetic differentiation mode reversed-phase high-performance liquid chromatography with fluorometric detection using 2-(2'-hydroxyphenyl)-10-hydroxybenzo[H]quinoline as precolumn chelating reagent

A highly sensitive and selective method for the determination of the Be(II) ion has been developed by the use of reversed-phase high-performance liquid chromatography (HPLC) with fluorometric detection using 2-(2'-hydroxyphenyl)-10-hydroxybenzo[h]quinoline (HPHBQ) as a precolumn (off-line) chelating reagent. The reagent HPHBQ has been designed to form the kinetically inert Be chelate compatible with high fluorescence yield, which is appropriate to the HPLC-fluorometric detection system. The Be-HPHBQ chelate is efficiently separated on a LiChrospher 100 RP-18(e) column with a methanol (58.3 wt %)-water eluent containing 20 mmol kg(-1) of tartaric acid and is fluorometrically detected at 520 nm with the excitation at 420 nm. Under the conditions used, the concentration range of 20-8,000 pmol dm(-3) of Be(II) ion can be determined without interferences from 10 micromol dm(-3) each of common metal ions, typically Al(III), Cu(II), Fe(III), and Zn(II), and still more coexistence of Ca(II) and Mg(II) ions at 0.50 mmol dm(-3) and 5.0 mmol dm(-3), respectively, is tolerated. The detection limit (3a baseline fluctuation) is 4.3 pmol dm(-3) (39 fg cm(-3)). The extraordinarily high sensitivity with toughness toward the matrix influence was demonstrated with the successful application to environmental Be analyses, such as determination of Be in rainwater and tap water.     

Ion-Pair Extraction of Metalloporphyrins into Acetonitrile for Determination of Copper(II)

Equilibrium study of ion-pair extraction of a cationic water-soluble porphyrin [5,10,15,20-tetrakis(1-methylpyridinium-4-yl)porphyrin, H(2)tmpyp(4+)] and its metalloporphyrins (MP) into the acetonitrile layer, separated by addition of sodium chloride (4.00 mol dm(-)(3)) to a 1:1 (v/v) acetonitrile-water mixed solvent, was carried out to develop a new and useful method for the determination of a subnanogram amount of copper(II). M denotes Zn(2+), Cu(2+), Co(3+), Fe(3+), and Mn(3+), and P(2)(-) is porphyrinate ion. The extraction and dissociation constants of the ion-pair complexes, defined by K(ex) = [MP(ClO(4))(4)](org)[MP(4+)](aq)(-)(1)[ClO(4)(-)](aq)(-)(4), K(dis,1) = [MP(ClO(4))(3)(+)](org)[ClO(4)(-)](org)[MP(ClO(4))(4)](org)(-)(1), and K(dis,2) = [MP(ClO(4))(2)(2+)](org)[ClO(4)(-)](org)[MP(ClO(4))(3)(+)](org)(-)(1), were determined by taking into account the partition constant of sodium perchlorate (K(D) = 1.82 ± 0.01). The equilibrium constants were found to be K(ex)K(dis,1) = (7.2 ± 1.3) × 10(4), (6.4 ± 0.9) × 10(4), (1.35 ± 0.13) × 10(5), (4.8 ± 0.6) × 10(3), (1.23 ± 0.05) × 10(4), and (1.42 ± 0.07) × 10(3) at 25 °C for the free base porphyrin (H(2)tmpyp(4+)) and the metalloporphyrins of zinc(II), copper(II), cobalt(III), iron(III), and manganese(III), respectively. The K(dis,2) values were (2.9 ± 1.4) × 10(-)(2), (3.1 ± 1.1) × 10(-)(2), (8.0 ± 4.9) × 10(-)(3), and (5.1 ± 2.2) × 10(-)(2) for the free base porphyrins and the metalloporphyrins of zinc(II), copper(II), and cobalt(III), respectively. The results were developed for determination of a trace amount of copper(II) (3 × 10(-)(8)-4 × 10(-)(6) mol dm(-)(3)) in natural water samples using H(2)tmpyp(4+) with a molar absorptivity of 3.1 × 10(5) mol(-)(1) dm(3) cm(-)(1) at a precision of 1.3% (RSD). The determination of copper(II) was not interfered by the presence of 10(-)(4) mol dm(-)(3) of Mn(2+), Co(2+), Ni(2+), Hg(2+), Cd(2+), Ag(+), Cr(3+), V(5+), Al(3+), Mg(2+), Ca(2+), Br(-), I(-), SCN(-), and S(2)O(3)(2)(-) and 10(-)(5) mol dm(-)(3) of Fe(3+), Zn(2+), and Pd(2+).     

Ni(2+) and H(2)PO(4)(-) uptake properties of compounds in the CaTiO(3)-CaFeO(2.5) system

A batch method was used to investigate the uptake of heavy metal cations and anions by the compounds in the CaTiO(3)-CaFeO(2.5) system, in which a series of oxygen vacancies was systematically introduced into a perovskite structure as the x-value of Ca(Fe(x)Ti(1-x))O(3-x/2) was increased. Samples of CaTiO(3), CaFe(0.1)Ti(0.9)O(2.95), CaFe(0.5)Ti(0.5)O(2.75), CaFe(0.67)Ti(0.33)O(2.67) and CaFeO(2.5) were prepared by solid mixing (SM), co-precipitation (CP) and gel evaporation (GE) methods. The resulting samples were calcined at temperatures between 400 and 1000 °C. The target crystalline phases differed according to the preparation method, but in most cases were formed at 700-800 °C. The Ni(2+) sorption isotherms of all the samples were fitted better by the Langmuir model than by the Freundlich model, while in the case of H(2)PO(4)(-) sorption isotherms, these were better fitted by the latter model. The uptake ability increased with increasing x value of the samples. The maximum values for the saturated sorption of Ni(2+) (Q(0)(Ni(2+)) = 2.83 mmol/g) and H(2)PO(4)(-) (K(F)(H(2)PO(4)(-)) = 2.95 mmol/g) were achieved for x = 1 (i.e. CaFeO(2.5)) sample.     

Poly(vinyl) chloride membrane copper-selective electrode based on 1-phenyl-2-(2-hydroxyphenylhydrazo)butane-1,3-dione

1-Phenyl-2-(2-hydroxyphenylhydrazo)butane-1,3-dione (H(2)L) was used as an effective ionophore for copper-selective poly(vinyl) chloride (PVC) membrane electrodes. Optimization of the composition of the membrane and of the conditions of the analysis was performed, and under the optimized conditions the electrode has a detection limit of 6.30×10(-7) M Cu(II) at pH 4.0 with response time 10s and displays a linear EMF versus log[Cu(2+)] response over the concentration range 2.0×10(-6) to 5.0×10(-3) M Cu(II) with a Nernstian slope of 28.80±0.11 mV/decade over the pH range of 3.0-8.0. The sensor is stable for 9 weeks and exhibits good selectivity with respect to alkali, alkali earth and transition metal ions (e.g. Na(+), K(+), Ba(2+), Ca(2+), Zn(2+), Cd(2+), Co(2+), Mn(2+), Ni(2+), Fe(2+), Al(3+)) in the 3.0-8.0 pH range. It was successfully applied for the direct determination of copper(II) in zinc, aluminum and nickel based alloys, in soils polluted by oil, and as an indicator electrode for potentiometric titration of copper ions with EDTA.     

Electrochemical studies of the interaction of metal chelates with DNA. 4. Voltammetric and electrogenerated chemiluminescent studies of the interaction of tris(2,2'-bipyridine)osmium(II) with DNA

Cyclic voltammetric and electrogenerated chemiluminescent data were used to study the binding of tris(2,2'-bipyridine)-osmium(II), Os(bpy)3(2+), an electrostatic binder, to calf thymus DNA. The oxidized form of the osmium complex, Os(bpy)3(3+), has a stronger association to DNA than the reduced form, Os(bpy)3(2+), as indicated by the negative shift of E0' of the CV waves (K3+/K2+ = 3.35). The calculated binding constant, K2+, and binding site size, s, for the Os(byp)3(2+)-DNA system depended slightly on whether a mobile or a static equilibrium was assumed. In 10 mM NaCl, 10 mM Tris pH 7, K2+ = (7.3 +/- 0.4) x 10(3) M-1 and s = 3 base pairs (mobile) and K2+ = (5.0 +/- 0.2) x 10(3) M-1 and s = 3 base pairs (static). Electrogenerated chemiluminescence (ECL) was produced upon oxidation of Os(bpy)3(2+) at a Pt electrode in a solution containing 10 mM C2O4(2-) and 10 mM phosphate at pH 5. Addition of DNA caused a decrease in the emission intensity (I); a plot of I vs relative DNA concentration yielded K2+ = (6.5 +/- 0.5) x 10(3) M-1 and s = 3 base pairs. The osmium complex produced ECL when bound to the DNA molecule with an efficiency of 30% that of the unbound chelate.     

Phase-transition temperatures and piezoelectric properties of (Bi1/2Na1/2)TiO3-(Bi1/2Li1/2)TiO3-(Bi1/2K1/2)TiO3 lead-free ferroelectric ceramics.

The phase-transition temperatures and piezoelectric properties of x(Bi(1/2)Na(1/2))TiO3-y(Bi(1/2)Li(1/2))TiO3-z(Bi(1/2)K(1/2))TiO3 [x + y + z = 1] (abbreviated as BNLKT100(y)-100(z)) ceramics were investigated. These ceramics were prepared using a conventional ceramic fabrication process. The phase-transition temperatures such as depolarization temperatures T(d), rhombohedraltetragonal phase transition temperature T(R-T), and dielectric-maximum temperature T(m) were determined using electrical measurements such as dielectric and piezoelectric properties. The X-ray powder diffraction patterns of BNLKT100(y)-100(z)) show the morphotropic phase boundary (MPB) between rhombohedral and tetragonal at approximately z = 0.20, and the piezoelectric properties show the maximum at the MPB. The electromechanical coupling factor k(33), piezoelectric constant d(33) and T(d) of BNLKT4-20 and BNLKT8-20 were 0.603, 176 pC/N, and 171 degrees C, and 0.590, 190 pC/N, and 115 degrees C, respectively. In addition, the relationship between d33 and Td of tetragonal side and rhombohedral side for BNLKT4-100z and BNLKT8-100z were presented. Considering both high Td and high d(33), the tetragonal side of BNLKT4-100z is thought to be the superior composition. The d(33) and T(d) of BNLKT4-28 were 135 pC/N and 218 degrees C, respectively. Moreover, this study revealed that the variation of T(d) is related to the variation of lattice distortion such as rhombohedrality 90-alpha and tetragonality c/a.     

Heterobimetallic Ru(II)-Eu(III) complex as chemodosimeter for selective biogenic amine odorants detection in fish sample

Gaseous biogenic amines such as putrescine, spermidine, aniline, and trimethylamine are important biomolecules that play many crucial roles in metabolism and medical diagnostics. A chemodosimetric detection assay has been developed for those gaseous amines by Ru(II)-Eu(III) heterobimetallic complexes, K{[Ru(II)((t)Bubpy)(CN)(4)](2)Eu(III)(H(2)O)(4)} (where (t)Bubpy = 4,4'-di-tert-butyl-2,2'-bipyridine). Synthesis, X-ray crystal characterization, and spectroscopic properties of this Ru(II)-Eu(III) heterobimetallic complex were reported. Binding properties of the Ru(II)-Eu(III) complex with common gases revealed that this complex is very selective to gaseous amine molecules. Sensitivity of this complex toward the amines was found as ～log k() = 4.5-4.8. Real time monitoring of gaseous biogenic amines was applied to real fish samples (Atlantic mackerel) by studying the spectrofluorimetric responses of the Ru(II)-Eu(III) complex toward different biogenic amine concentration. GC/MS studies were also used as a reference for the studies. A linear spectrofluorimetric response was found toward biogenic amine concentration in real fish samples. This complex was found to respond specifically to those biogenic amines down to 10 ppb.     

Raman and infrared spectroscopic investigations on aqueous alkali metal phosphate solutions and density functional theory calculations of phosphate-water clusters

Phosphate (PO(4)(3-)) solutions in water and heavy water have been studied by Raman and infrared spectroscopy over a broad concentration range (0.0091-5.280 mol/L) including a hydrate melt at 23 degrees C. In the low wavenumber range, spectra in R-format have been constructed and the R normalization procedure has been briefly discussed. The vibrational modes of the tetrahedral PO(4)(3-)(aq) (T(d) symmetry) have been assigned and compared to the calculated values derived from the density functional theory (DFT) method for the unhydrated PO(4)(3-)(T(d)) and phosphate-water clusters: PO(4)(3-).H(2)O (C(2v)), PO(4)(3-).2H(2)O (D(2d)), PO(4)(3-).4H(2)O (D(2d)), PO(4)(3-).6H(2)O (T(d)), and PO(4)(3-).12H(2)O (T), a cluster with a complete first hydration sphere of water molecules. A cluster with a second hydration sphere of 12 water molecules and 6 in the first sphere, PO(4)(3-).18H(2)O (T), has also been calculated. Agreement between measured and calculated vibrational modes is best in the case of the PO(4)(3-).12H(2)O cluster and the PO(4)(3-).18H(2)O cluster but far less so in the case of the unhydrated PO(4)(3-) or phosphate-water cluster with a lower number of water molecules than 12. The asymmetric, broad band shape of v(1)(a(1)) PO(4)(3-) in aqueous solutions has been measured as a function of concentration and the asymmetric and broad band shape was explained. However, the same mode in heavy water has only half the full width at half-height compared to the mode in normal water. The PO(4)(3-) is strongly hydrated in aqueous solutions. This has been verified by Raman spectroscopy comparing v(2)(H(2)O), the deformation mode of water, and the stretching modes, the v(1)OH and v(3)OH of water, in K(3)PO(4) solutions as a function of concentration and comparison with the same modes in pure water. A mode at approximately 240 cm(-1) (isotropic R spectrum) has been detected and assigned to the restricted translational mode of the strong hydrogen bonds formed between phosphate and water, P-O...HOH. In very concentrated K(3)PO(4) solutions (C(0) > or = 3.70 mol/L) and in the hydrate melt, formation of contact ion pairs (CIPs) could be detected. The phosphate in the CIPs shows a symmetry lowering of the T(d) symmetry to C(3v). In the less concentrated solutions, PO(4)(3-)(aq) solvent separated ion pairs and doubly solvent separated ion pairs exist, while in very dilute solutions fully hydrated ions are present (C(0) < or = 0.005 mol/L). Quantitative Raman measurements have been carried out to follow the hydrolysis of PO(4)(3-)(aq) over a very broad concentration range. From the hydrolysis data, the pK(3) value for H(3)PO(4) has been determined to be 12.45 at 23 degrees C.     

Photosensitized degradation in water of the phenolic pesticides bromoxynil and dichlorophen in the presence of riboflavin, as a model of their natural photodecomposition in the environment

Within the context of environmentally friendly methods for the elimination of surface-water pollutants, the photodegradation of the phenolic pesticides bromoxynil (BXN) and dichlorophen (DCP) under simulated natural conditions has been studied. The work was done in the presence of the visible-light absorber photosensitizer riboflavin (Rf), usually present in trace quantities in natural waters. Under aerobic conditions, an efficient photooxidation of both pesticides was observed. The relatively intricate photochemical mechanism involves pesticide and oxygen consumption and, to a lesser extent, Rf degradation. The kinetic and mechanistic study supports that both H(2)O(2) and singlet molecular oxygen, O(2)((1)Δ(g)), are involved in the process. Kinetic data for the O(2)((1)Δ(g))-mediated oxidation indicate that BXN and DCP are photodegraded with this species faster than the parent compound phenol, very frequently employed as a model for aquatic contaminants, likely due to their lower pK(a) values. This observation allows the design of phenolic pesticides with different photodegradation rates under environmental conditions.     

Catalytic effect of nanogold on Cu(II)-N2H4 reaction and its application to resonance scattering immunoassay

In the medium of EDTA-NaOH, nanogold strongly catalyzed the slow reaction between hydrazine (N2H4) and Cu(II) to form Cu particles, which exhibited a strong resonance scattering (RS) peak at 602 nm. The increased RS intensity at 602 nm (DeltaI(RS)) was linear to the nanogold concentration in the range of 0.008-2.64 nM, with a detection limit of 1.0 pM Au. The rate equation obtained by the initial rate procedure was V(Cu) = K(Cu)[C(Cu(II))](2)C(OH)(1)C(Au)(1)C(N2)H4(1), with an apparent activation energy of 38 kJ x mol(-1), and the catalytic reaction mechanism was also discussed. An immunonanogold-catalytic resonance scattering spectral (RSS) assay was established for detection of microalbumin (Malb), using 10 nm nanogold to label goat antihuman Malb to obtain an immunonanogold probe (AuMalb) for Malb. In pH 5.0 citric acid-Na2HPO4 buffer solution, the AuMalb aggregated nonspecifically. Upon addition of Malb, it reacted with the probe to form dispersive AuMalb-Malb immunocomplex in the solution. After centrifugation, the supernatant containing AuMalb-Malb was obtained, and exhibited a catalytic effect on the reaction of N2H4-Cu(II) to produce large Cu particles that resulted in the I(602 nm) increasing. The increased RS intensity at 602 nm (DeltaI(602 nm)) was linear to Malb concentration (C(Malb)) in the range of 0.4 to 460 pg x mL(-1), with the regression equation of DeltaI(602 nm) = 0.3713 C(Malb) + 7.2, correlation coefficient of 0.9981 and detection limit of 0.1 pg x mL(-1) Malb. The proposed method was applied to detect Malb in healthy human urine samples, with satisfactory results.     

Complete set of material properties of [011](c) poled 0.24Pb(In(1/2)Nb(1/2))O(3)-0.46Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) single crystal

A complete set of elastic, piezoelectric, and dielectric constants of [011](c) poled multidomain 0.24Pb(In(1/2)Nb(1/2))O(3)-0.46Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) ternary single crystal has been determined using resonance and ultrasonic methods and the temperature dependence of the dielectric permittivity has been measured at 3 different frequencies. The experimental results revealed that this [011](c) poled ternary single crystal has very large transverse piezoelectric coefficient d(32) = -1693 pC/N, transverse dielectric constant ε(11)/ε(0) ~ 7400 and a high electromechanical coupling factor k(32) ~ 90%. In addition, its coercive field is 2 times of that of the corresponding binary 0.7Pb(Mg(1/3)Nb(2/3))O(3)-0.30PbTiO(3) single system with much better temperature stability. Therefore, the crystal is an excellent candidate for transverse mode electromechanical devices.     

Density functional theory calculations for [C(2)H(4)N(2)O(6)]((n)) (n=0, +1, -1)

The structural and electronic properties of neutral and mono ionic structures of isolated ethylene glycol dinitrate (EGDN) [C(2)H(4)N(2)O(6)]((n)) (n=0, +1, -1) have been investigated by performing density functional theory calculations at B3LYP level. The optimum geometry, vibrational frequencies, electronic structure and some thermo dynamical values of the structures considered have been obtained in their ground states. The calculations reveal that as the charge develops the bond lengths and angles change. In the anionic case charge accumulation causes NO(2) elimination as a result of esteric O-N bond cleavage.     

Adsorption of arsenic(V) into modified lamellar Kenyaite

The synthetic Kenyaite sample was used for organofunctionalization process with N-propyldiethylenetrimethoxysilane and bis[3-(triethoxysilyl)propyl]tetrasulfide. The resulted materials were submitted to process of adsorption with arsenic solution at pH 2.0 and 298+/-1K. The adsorption isotherms were adjusted using a modified Langmuir equation with regression non-linear; the net thermal effects obtained from calorimetric titration measurements were adjusted to a modified Langmuir equation. The adsorption process was exothermic (Delta(int)H=-4.08 to -5.94 kJ mol(-1)) accompanied by increase in entropy (Delta(int)S=41.29-62.09 J K(-1)mol(-1)) and Gibbs energy (Delta(int)G=-22.33 to -24.45 kJ mol(-1)). The energetic effect caused by metal cation adsorption was determined through calorimetric titration at the solid-liquid interface and gave a net thermal effect that enabled the calculation of the exothermic values and the equilibrium constant.     

Efficacy of modified distillation sludge of rose (Rosa centifolia) petals for lead(II) and zinc(II) removal from aqueous solutions

Removal of lead(II) and zinc(II) from aqueous solutions was studied using chemically modified distillation sludge of rose (Rosa centifolia) petals by pretreatment with NaOH, Ca(OH)(2), Al(OH)(3), C(6)H(6), C(6)H(5)CHO and HgCl(2). The adsorption capacity of biomass was found to be significantly improved. NaOH pretreated biomass showed remarkable increase in sorption capacity. Maximum adsorption of both metal ions was observed at pH 5. When Freundlich and Langmuir isotherms were tested, the latter had a better fit with the experimental data. The overall adsorption process was best described by pseudo second order kinetics. The thermodynamic assessment of the metal ion-Rosa centifolia biomass system indicated the feasibility and spontaneous nature of the process and DeltaG degrees was evaluated as ranging from -26.9501 to -31.652 KJmol(-1) and -24.1905 to -29.8923KJmol(-1) for lead(II) and zinc(II) sorption, respectively, in the concentration range 10-640mgL(-1). Distribution coefficient (D) showed that the concentration of metal ions at the sorbent-water interface is higher than the concentration in the continuous aqueous phase. Maximum adsorption capacity of biomass tends to be in the order Pb(II) (87.74mgg(-1))>Zn(II) (73.8mgg(-1)) by NaOH pretreated biomass.     

Physical Properties and Electronic Structure Study of the 1-(2-aminoethyl) Piperaziniumtrichlorocuprate (II) Monohydrate

The [(C₆H₁₆N₃)CuCl₃] compound crystallizes in the monoclinic system with P21/n space group. The copper (II) ion is five-coordinated by two nitrogen atoms form the bidentate 1-(2-aminoethyl) piperazinium cation and three chloride ions in a distorted square-pyramidal environment. Magnetic susceptibility and hysteresis-loop measurements are reported. The magnetic susceptibility shows a maximum around 4?K and decreases gradually. Below this temperature, the system is antiferromagnetic with a weak moment. The electronic structure calculation based on the Full potential Linearized Augmented Plane Wave (FLAPW) method is also performed to shed light on magnetic and electronic structures. The experimental results are in agreement with theoretical studies.     

Identification of produced powerful radicals involved in the mineralization of bisphenol A using a novel UV-Na(2)S(2)O(8)/H(2)O(2)-Fe(II,III) two-stage oxidation process

A two-stage oxidation (UV-Na(2)S(2)O(8)/H(2)O(2)-Fe(II,III)) process was applied to mineralize bisphenol A (BPA) at pH(i) (initial pH) 7. We take advantage of the high oxidation potential of sulfate radicals and use persulfate as the 1st-stage oxidant to oxidize BPA to less complex compounds (stoichiometric ratio: [S(2)O(8)(2-)](0)/[BPA](0)=1). Afterwards, the traditional photo-Fenton process was used to mineralize those compounds to CO(2). To the best of our knowledge, this is the first attempt to utilize the two processes in conjunction for the complete degradation of BPA. During the 2nd-stage reaction, other oxidants (H(2)O(2) and Iron alone) were also employed to observe the extent of enhancement of photo-Fenton. Further, qualitative identification of both hydroxyl and sulfate radicals was performed to evaluate their dominance under different conditions. The BPA degradation in this UV/persulfate process formulated a pseudo-first-order kinetic model well, with a rate constant of approximately 0.038 min(-1) (25 degrees C), 0.057 min(-1) (35 degrees C), and 0.087 min(-1) (50 degrees C), respectively. The much lower activation energy (DeltaE = 26 kJ mol(-1)) was further calculated to clarify that the thermal-effect of an illuminated system differs from single heat-assisted systems described in other research. Final total organic carbon (TOC) removal levels of BPA by the use of such two-stage oxidation processes were 25-34%, 25%, and 87-91% for additional Fe(II,III) activation, H(2)O(2) promotion, and Fe(II,III)/H(2)O(2) promotions, respectively.     

1，3-双（叠氮乙酰氧基）-2-乙基-2-硝基丙烷的合成与性能

以2-乙基-2-硝基-1,3-丙二醇为原料,经酯化、叠氮化两步反应,合成出了1,3-二(叠氮乙酰氧基)-2-乙基-2-硝基丙烷(ENPEA),总收率为83%。利用红外光谱、核磁共振、元素分析对ENPEA的结构进行了表征。探讨了叠氮化反应的影响因素,确定其最佳反应条件为:n(Na N3)n(ENPE)为2.21.0,混合溶剂中水占总体积的13%~20%,反应时间2 h;性能测试得到ENPEA的玻璃化转变温度为-43.4℃,热分解峰温为252.4℃,密度为1.34 g/cm3,特性落高为120.2 cm(落锤2 kg),爆炸概率为4%(摆角66°)。     

Synthesis, structure, and properties of [Be(H2O)4][UO2(CH3COO)3]2

Crystals of previously unknown compound [Be(H₂O)₄][UO₂(CH₃COO)₃]₂ were prepared and studied by X-ray diffraction analysis. The compound crystallizes in the tetragonal system, unit cell parameters (at 100 K): a = 10.3647(3), c = 23.4127(8) Å, V = 2515.16(13) ų, space group I4₁/a, Z = 4, R = 0.0194. The structure consists of mononuclear complexes [Be(H₂O)₄]²⁺ and [UO₂(CH₃COO)₃]^? linked with each other by electrostatic interactions and hydrogen bonds formed by water molecules and O atoms of acetate anions. The compound was also studied by methods of thermal analysis and IR spectroscopy.     

Azadirachta indica (Neem) leaf powder as a biosorbent for removal of Cd(II) from aqueous medium

A biosorbent, Neem leaf powder (NLP), was prepared from the mature leaves of the Azadirachta indica (Neem) tree by initial cleaning, drying, grinding, washing to remove pigments and redrying. The powder was characterized with respect to specific surface area (21.45 m2g(-1)), surface topography and surface functional groups and the material was used as an adsorbent in a batch process to remove Cd(II) from aqueous medium under conditions of different concentrations, NLP loadings, pH, agitation time and temperature. Adsorption increased from 8.8% at pH 4.0 to 70.0% at pH 7.0 and 93.6% at pH 9.5, the higher values in alkaline medium being due to removal by precipitation. The adsorption was very fast initially and maximum adsorption was observed within 300 min of agitation. The kinetics of the interactions was tested with pseudo first order Lagergren equation (mean k(1)=1.2x10(-2)min(-1)), simple second order kinetics (mean k2=1.34x10(-3) gmg(-1)min(-1)), Elovich equation, liquid film diffusion model (mean k=1.39x10(-2)min(-1)) and intra-particle diffusion mechanism. The adsorption data gave good fits with Langmuir and Freundlich isotherms and yielded Langmuir monolayer capacity of 158mgg(-1) for the NLP and Freundlich adsorption capacity of 18.7 Lg(-1). A 2.0 g of NLP could remove 86% of Cd(II) at 293 K from a solution containing 158.8 mg Cd(II) per litre. The mean values of the thermodynamic parameters, DeltaH, DeltaS and DeltaG, at 293 K were -73.7 kJmol(-1), -0.24 Jmol(-1)K(-1) and -3.63 kJmol(-1), respectively, showing the adsorption process to be thermodynamically favourable. The results have established good potentiality for the Neem leaf powder to be used as a biosorbent for Cd(II).     

Nonlinear dielectric response of AgNb(1-x)Ta(x)O3 in the vicinity of diffuse phase transitions

Linear and nonlinear dielectric studies of AgNb(1-x)Ta(x)O(3) (ATN) ceramics (x ≤ 0.6) were carried out in the temperature range of 80 to 673K. The temperature dependences of third-order nonlinear electric susceptibility X3'(T) exhibit two distinct maxima: at the temperature of the weak ferroelectric phase appearance, M(1)-M(2) transition, and at the temperature of the Nb/Ta ion dynamics freezing, Tf. For AgNbO3, they appear at 325K and 448K, respectively. With increasing Ta concentration, both maxima shift toward lower temperature: 4K/%Ta (M(1)-M(2)) and 5.6K/%Ta (T(f)). The X3' (T) maxima indicate changes of the Nb/Ta ion dynamics and their contribution to electric susceptibility. At T(f), a partial freezing of the Nb/Ta ion displacements to the disordered antipolar, antiferroelectric array takes place. At the M(1)-M(2) transition, further freezing of Nb/Ta displacements to polar weak relaxor ferroelectric or dipolar glass transition occurs. This polar state coexists with the ground antiferroelectric state. Studies of the aging process showed that below T(f) the aging influence on electric susceptibility is substantial, whereas above Tf it may be neglected. This means that for ATN ceramics in the concentration range used for applications, there is no aging process in the room temperature region, which is an additional advantage of this system.