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1.
The adsorption of transition metal cations and inorganic anions from aqueous solutions on microdispersed sintered detonation nanodiamond (MSDN) is systematically studied. The selectivity series Fe3+ > Al3+ > Cu2+ > Mn2+ > Zn2+ > Cd2+ > Co2+ > Ni2+ with maximum adsorption capacity between 2 and 5 µmol g?1 is obtained. It is found that anions may significantly contribute to the adsorption of transition metal cations, so the adsorption of CH3COO?, Cl?, B4O7 2?, ClO4 ?, I?, SO4 2?, C2O4 2?, PO4 3? is also studied. For the first time, dominating adsorption of anions over cations is demonstrated for detonation nanodiamond. The maximum anion-exchange capacity of 50–150 µmol g?1 is found for MSDN. Beside of electrostatic interactions, the formation of complexes with hydroxyl groups and interaction with metal impurities contribute to the adsorption of B4O7 2? and PO4 3?, respectively. Therefore, anion exchange selectivity of MSDN is different from that observed for common anion exchange resins. In all cases, the adsorption on MSDN obeys Langmuir law. The pH effect on the adsorption of SO4 2?, PO4 3? and B4O7 2? is different from that observed for other anions due to specific interactions.  相似文献   

2.
Trace element impurities in high-purity antimony were determined employing three different methods for the removal of matrix; on Dowex 50WX 8 by adsorption from 0.1 mol/L HF and elution with 4 mol/L HNO3; on Chelex-100 resin (in NH4 + form) Bi, Cd, Co, Cu, and Pb were separated in the presence of tartaric acid at a pH of 9.0 ± 0.1 with subsequent elution with 2 mol/L HCl; these determinations were carried out by GFAAS. The separation of trace impurities from Sb by volatilization of the matrix from H2SO4 and HBr medium was also investigated. ICP-MS was used for the determination in these cases. All the three procedures showed that the removal of the antimony matrix was nearly quantitative (> 99.99%). The recoveries of trace elements were found to be > 95%. The relative standard deviations were in the range 2–7%. Standard addition calibrations were used. The levels of process blanks indicate that with careful optimization, the volatilization procedure coupled with ICP-QMS can be used for trace impurity characterization of 6N+ Sb.  相似文献   

3.
Trace element impurities in high-purity antimony were determined employing three different methods for the removal of matrix; on Dowex 50WX 8 by adsorption from 0.1 mol/L HF and elution with 4 mol/L HNO3; on Chelex-100 resin (in NH4 + form) Bi, Cd, Co, Cu, and Pb were separated in the presence of tartaric acid at a pH of 9.0 ± 0.1 with subsequent elution with 2 mol/L HCl; these determinations were carried out by GFAAS. The separation of trace impurities from Sb by volatilization of the matrix from H2SO4 and HBr medium was also investigated. ICP-MS was used for the determination in these cases. All the three procedures showed that the removal of the antimony matrix was nearly quantitative (> 99.99%). The recoveries of trace elements were found to be > 95%. The relative standard deviations were in the range 2–7%. Standard addition calibrations were used. The levels of process blanks indicate that with careful optimization, the volatilization procedure coupled with ICP-QMS can be used for trace impurity characterization of 6N+ Sb. Received: 25 May 1998 / Revised: 23 September 1998 / Accepted: 26 September 1998  相似文献   

4.
Glassy tin arsenate, Sn(HAsO4)2·2.7H2O (SnAs) was prepared and characterized. The uptake of lanthanide ions La3+, Sm3+, Eu3+, and Yb3+ was followed on the glassy tin arsenate in HNO3 solution at pH 1,2 and 4. The radiotracers are140La,153Sm,152mEu, and175Yb. 500 μl (4.0·10−5 mmole) of each solution of the tracer as a mixture plus 7.5 ml HNO3 solution at the desired pH were equilibrated with 0.1g of SnAs. The selectivity order (K d values) was found to be dependent on the pH. At pH 2 theK d values were high for all the studied metal ions [Yb (2065.4)>La (1976.1)>Sm (1826.4)>Eu (1754.4)]. TheK d values at pH 1 and 4 are quite low for all the metal ions studied. At pH 1 they range from ≈144 to 156 and at pH 4 they range from ≈70 to 79.  相似文献   

5.
The removal of Th4+ ions from aqueous solutions was investigated using single-layer graphene oxide (GO) as a sorbent which was prepared by the modified Hummers’ method through batch adsorption experiments at room temperature. Structural characterizations of the sorbent were also investigated. The influences of the pH value of solution, contact time, sorbent dose, ionic strength, the initial metal ion concentration and temperature on the adsorption of Th4+ were also investigated. These results indicated that the adsorption of Th4+ was dependent on the pH and independent on the ionic strength. The sorbent provided significant Th4+ removal (>98.7 %) at pH 3.0 and the adsorption equilibrium was achieved after only 10 min. The Langmuir adsorption isotherm fit the absorption profile very closely, and indicated that a maximum adsorption capacity of 1.77 mmol g?1 of GO (411 mg g?1) after 2 h. The thermodynamic parameters showed that this adsorption process was endothermic and spontaneous. Moreover, the desorption level of Th4+ from GO, by using 0.1 mol L?1 H2SO4 as a stripping agent, was 84.2 ± 1.2 %, and that of 0.5 mol L?1 HNO3 as a stripping agent, was 79.8 ± 3.0 %.  相似文献   

6.
Uptake of lead by carbonaceous adsorbents developed from tire rubber   总被引:1,自引:0,他引:1  
The adsorption of lead in aqueous solution by discarded tire rubber (TR) and by carbonaceous adsorbents (CAs) prepared from it by thermal and chemical treatments is studied. TR was heated at 400 or 900?°C for 2 h in N2 atmosphere or treated chemically with H2SO4, HNO3, H2SO4/HNO3, HCl, NaOH, HCl-NaOH or NaOH-HCl for 24 h. TR and CAs were characterized physico-chemically with regard to their texture, elemental composition and surface chemistry. The adsorption of lead was studied, mainly from the kinetic standpoint, using 4×10?3 mol?L?1 Pb2+ solutions at initial pH 2.0, 5.7 and 12.6. TR is practically a non-porous material. The heat treatment of TR mainly develops meso- and macroporosity. The effect on macroporosity is stronger when HNO3 and H2SO4/HNO3 are used. For all adsorbents, the adsorption of lead is not measurable when adsorptive solution at pH 2 is used. With an increase of pH from 5.7 to 12.6, the kinetics of adsorption becomes faster and the amount of lead adsorbed significantly increases. For the solution at pH 12.6 and an adsorption time of 8 h, the adsorption percentage is 36 wt% for TR. For the CAs prepared by heat treatment of TR, it is higher than 50 wt%. For longer adsorption times, the kinetics is much slower for the product of TR treatment with HNO3. However, the corresponding adsorption percentage is as high as 93 wt% for an adsorption time of 264 h. TR and the CAs, in particular the product heated at 400?°C, are good adsorbents to be used in the rapid removal of a significant amount of lead from aqueous solution.  相似文献   

7.

The aim of this study is to prepare magnetic beads which can be used for the removal of heavy metal ions from synthetic solutions. Magnetic poly(ethylene glycol dimethacrylate‐vinyl imidazole) [m‐poly(EGDMA‐VIM)] beads were produced by suspension polymerization in the presence of magnetite Fe3O4 nano‐powder. The specific surface area of the m‐poly(EGDMA‐VIM) beads was found to be 63.1 m2/g with a size range of 150–200 µm in diameter and the swelling ratio was 85%. The average Fe3O4 content of the resulting m‐poly(EGDMA‐VIM) beads was 12.4%. The maximum binding capacities of the m‐poly(EGDMA‐VIM) beads were 32.4 mg/g for Cu2+, 45.8 mg/g for Zn2+, 84.2 mg/g for Cd2+and 134.5 mg/g for Pb2+. The affinity order on mass basis is Pb2+>Cd2+>Zn2+>Cu2+. Equilibrium data agreed well with the Langmuir model. pH significantly affected the binding capacity of the magnetic beads. Binding of heavy metal ions from synthetic wastewater was also studied. The binding capacities were 26.2 mg/g for Cu2+, 33.7 mg/g for Zn2+, 54.7 mg/g for Cd2+ and 108.4 mg/g for Pb2+. The magnetic beads could be regenerated up to about 97% by treating with 0.1 M HNO3. These features make m‐poly(EGDMA‐VIM) beads a potential candidate for support of heavy metal removal under magnetic field.  相似文献   

8.
The chemical and electrochemical properties of technetium metal were studied in 1–6 M HX and in 1 M NaX (pH 1 and 2.5), X = Cl, NO3. The chemical dissolution rates of Tc metal were higher in HNO3 than in HCl (i.e. 8.63 × 10?5 mol cm?2 h?1 in 6 M HNO3 versus 2.05 × 10?9 mol cm?2 h?1 in 6 M HCl). The electrochemical dissolution rates in HNO3 and HCl were similar and mainly depended on the electrochemical potential and the acid concentration. The optimum dissolution of Tc metal was obtained in 1 M HNO3 at 1 V/AgAgCl (1.70 × 10?3 mol cm?2 h?1). The dissolution potentials of Tc metal in nitric acid were in the range of 0.596–0.832 V/AgAgCl. Comparison of Tc behavior with Mo and Ru indicated that in HNO3, the dissolution rate followed the order: Mo > Tc > Ru, and for dissolution potential the order: E diss(Ru) > E diss(Tc) > E diss(Mo). The corrosion products of Tc metal were analyzed in HCl solution by UV–Visible spectroscopy and showed the presence of TcO4 ?. The surface of the electrode was characterized by microscopic techniques; it indicated that Tc metal preferentially corroded at the scratches formed during the polishing and no oxide layer was observed.  相似文献   

9.
Ammonium dinitramide (ADN) has attracted great interest as a potential oxidizer for next generation rocket propellants. It is a halogen-free alternative to ammonium perchlorate, which is currently in wide used as a solid propellant oxidizer. However, in ADN synthesis, N-nitration is necessary to form the N-(NO2)2 group. Using a reaction calorimeter, the thermal behavior of nitration of sulfamates (K, Na, and NH4) using a mixture of acids (HNO3/H2SO4 and HNO3/AcOH) as the nitration agent was examined. The heat of decomposition of potassium sulfamate at ?10 °C was greater than that at 20 °C. The heat of decomposition decreased in the following order: K salt>Na salt>NH4 salt in HNO3/H2SO4. The dipole moments of the sulfamates were calculated, and the results revealed that the electronic states of nitrogen were different. Thus, the dipole moments of sulfamates affect the decomposition heat of sulfamates. The heat of decomposition in HNO3/AcOH was larger than that in HNO3/H2SO4.  相似文献   

10.
The order of extraction of Mo(VI) from 1M acid solutions by 5% (v/v) LIX 622 (HL) in benzene is HCl>HNO3>HClO4>H2SO4, and extraction decreases with increasing concentration of HCl and H2SO4, and increases slightly with increasing concentration of HNO3 and HClO4. The extracted species is shown to be MoO2L2 as established by IR data of organic extracts and the extracted species in the solid form. Extraction is almost quantitative at and above 10% LIX 622, and is found to be independent of [Mo(VI)] in the range of 10–4 to 10–3 M. The diluents CCl4, CHCl3 and C6H6 are found to be superior to solvents of high dielectric constant for extraction of Mo(VI). Extraction of uranium(VI) by 10% (v/v) LIX 622 in benzene was found to increase with increasing equilibrium pH (3.0 to 6.0), and becomes quantitative at pH 5.9. Tributyl phosphate acts as a modifier up to 2% (v/v). Thorium(IV) is almost not extracted by LIX 622 or its mixture. Separation of Mo(VI) and U(VI) is feasible.  相似文献   

11.
175, 181Hafnium(IV) was extracted by HDBP in 2-ethylhexanol from 1–10M solutions of HClO4, HCl and HNO3, and 1–8M H2SO4. As with low polar organic phase diluents, the acidity dependence of the distribution ratio of Hf, D, passes through a minimum for HClO4, HCl, and H2SO4 whereas only an increase of D can be observed with increasing HNO3 concentration. From the slope analysis the following complexes were found to be extracted (HDBP=HA): HfA4 at <4M HClO4 and <5M HCl, lg Kextr=9, HfX4(HA)4 (X=ClO 4 , Cl or NO 3 ) at >5M HClO4, >7M HCl and 1–10M HNO3, Hf(SO4)A2(HA)3–4 at <3M H2SO4, and Hf(SO4)2 (HA)4 at >6M H2SO4. Coextraction of sulphate with hafnium from H2SO4 solutions was evidenced in experiments with macro concentrations of Hf(IV) and35SO 4 2− . Part XX: Coll. Czech. Chem. Commun., 40 (1975) 3617.  相似文献   

12.
The present study deals with the characterization of halotolerant protease produced by Bacillus aquimaris VITP4 strain isolated from Kumta coast, Karnataka, India. The studies were performed at 40 °C and pH 8 in Tris buffer. Metal ions such as Mn2+ and Ca2+ increased the proteolytic activity of the enzyme by 34 and 30 %, respectively, at 10 mM concentration. Cu2+ at 1 mM concentration was found to enhance the enzyme activity by 16 %, whereas inhibition was observed at higher concentration (>5 mM). Slight inhibition was observed even with lower (>1 mM) concentrations of Zn2+, Hg2+, Fe3+, Ni2+, and Co2+.The activity of protease was completely inhibited by phenylmethylsulfonyl fluoride, indicating that the VITP4 protease is a serine protease. The presence of ethylenediaminetetraacetic acid and 1,10-phenanthroline (>5 mM) moderately inhibited the activity, suggesting that the enzyme is activated by metal ions. The protease was purified to homogeneity with a purification fold of 15.7 with ammonium sulfate precipitation and 46.65 with gel filtration chromatography using Sephadex G-100, resulting in a specific activity of 424?±?2.6 U mg?1. The VITP4 protease consists of a single polypeptide chain with a molecular mass of 34.7 kDa as determined by sodium dodecyl sulfate–polyacrylamide gel electrophoresis and matrix-assisted laser desorption/ionization–time of flight. Among the different substrates used (casein, egg albumin, gelatin, and bovine serum albumin), the activity was higher with casein with V max, K m, and k cat values of 0.817 mg ml min?1, 0.472 mg ml?1, and 2.31 s?1, respectively. Circular dichroism studies revealed that the VITP4 protease has a predominantly β-sheet structure (51.6 %) with a temperature for half denaturation of 85.8 °C in the presence of 1 mM CaCl2. Additionally, the VITP4 protease was found to retain more than 70 % activity in the presence of 10 mM concentration of different detergents (CTAB, urea, and sodium dodecyl sulfate) and surfactants (Triton X-100, Tween-20, and Tween-80), and the results of wash performance test with various commercial detergents confirmed that it can be used in detergent formulations.  相似文献   

13.
A new ion chromatographic (IC) system, in which n-tetradecylphosphocholine (TDPC, a phosphobetaine type of zwitterionic surfactant) was used as the stationary phase, pure water as the mobile phase, and conductivity as the method of detection, has been developed for the determination of inorganic acids. Five model acids, HCl, HNO3, HClO4, H2SO4, and H3PO4, were separated to baseline and eluted in the order H3PO4 > HCl > HNO3 > H2SO4 > HClO4. When peak areas were plotted against the concentrations of the acids in samples, linear calibration curves were obtained. Ultimate determination limits were approximately 1 mmol L–1, but the discrimination of the method between solutions of different concentration was better than 10 μmol L–1 for those model analytes. Salts of divalent cations could also be separated, but they were eluted faster than the acids. No separation was observed for the salts of monovalent cations. This newly proposed approach is applicable to the simultaneous determination of the inorganic acids (produced by reactions of NOx, SOx, and HCl with water) in aerosols.  相似文献   

14.
The separation procedure for Ag, B, Cd, Dy, Eu and Sm as impurities in Gd matrix using ICP-AES technique with an extraction chromatographic column has been developed. The spectral interference of the Gd matrix on the elements was eliminated using a chromatography technique with 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (PC-88A) as the mobile phase and XAD-16 resin as the stationary phase. Ag+, B4O72−, and Cd2+ were eluted with 0.1 M HNO3, while rare earth ions were not. The best eluent for separating Eu and Sm in the Gd matrix was 0.3 M HNO3. The limit of quantitation for these elements was 0.6-3.0 ng mL−1. The recovery of Ag, B, and Cd was 90-104% using 0.1 M HNO3 as the eluent, while that of Eu, Gd, and Sm ranged from 100 to 102% with 0.3 M HNO3. Dy was recovered quantitatively with 4 M HNO3. The relative standard deviation of the methods for a set of three replicates was between 1.0 and 15.4% for the synthetic and standard Gd solutions. The proposed separation procedure was used to measure Ag, B, Cd, Dy, Eu, and Sm in a standard Gd solution.  相似文献   

15.
The extraction of HCl, HBr, HNO3, HClO4, H2SO4 and CH3COOH into solutions of 4-(5-nonyl)pyridine (NPy) and 2-hexylpyridine (HPy) dissolved in benzene has been studied. The results show that the larger, less basic anions extract better (ClO 4 >CH3COO≥NO 3 >Br>Cl>HSO 4 ) due to their low aqueous hydration. The ionization constants of NPyH+ and HPyH+ as determined spectrophotometrically were found to be 5.97±0.06 and 5.94±0.05, respectively, at 25°C.  相似文献   

16.
The sorption of nickel on synthetic hydroxyapatite was investigated using a batch method and radiotracer technique. The hydroxyapatite samples used in experiments were a commercial hydroxyapatite and hydroxyapatite of high crystallinity with Ca/P ratio of 1.563 and 1.688, respectively, prepared by a wet precipitation process. The sorption of nickel on hydroxyapatite was pH independent ranging from 4.5 to 6.5 as a result of buffering properties of hydroxyapatite. The adsorption of nickel was rapid and the percentage of Ni sorption on both samples of hydroxyapatite was >98 % during the first 15–30 min of the contact time for initial Ni2+ concentration of 1 × 10?4 mol dm?3. The experimental data for sorption of nickel have been interpreted in the term of Langmuir isotherm and the value of maximum sorption capacity of nickel on a commercial hydroxyapatite and hydroxyapatite prepared by wet precipitation process was calculated to be 0.184 and 0.247 mmol g?1, respectively. The sorption of Ni2+ ions was performed by ion-exchange with Ca2+ cations on the crystal surface of hydroxyapatite under experimental conditions. The competition effect of Co2+ and Fe2+ towards Ni2+ sorption was stronger than that of Ca2+ ions. NH4 + ions have no apparent effect on nickel sorption.  相似文献   

17.
Formation of complexes between the lanthanide ions and N,N′-bis(salicylidene)-4-methyl-1,3-phenylenediamine ligand was studied in solution by pH potentiometry. The potentiometric titration was performed at 25.00 °C in 0.1 mol·dm?3 NaClO4 ionic strength and in DMSO:water (30:70 v:v) solvent mixture. N,N′-bis(salicylidene)-4-methyl-1,3-phenylenediamine ligand (H2L) occurs in three forms: fully or partially deprotonated and unionized. Computer analysis of potentiometric data indicated that in solution the lanthanide (Ln) complexes exist as LnL2, Ln(HL)2 and Ln(H2L)2 species. This observation appears to be in contrast to the solid-state behavior of these complexes prepared in a self-assembly process and structurally defined. Stability constants for La3+, Eu3+, Gd3+, Tb3+, Ho3+ and Lu3+ (Ln3+) complexes were determined. The order of stabilities of LnL2 species in terms of metal ions is La3+ > Eu3+ ≈ Gd3+ = Tb3+ < Ho3+ < Lu3+ with a prominent “gadolinium break”.  相似文献   

18.
Series of maleate monoester and diester monomers based on poly(ethylene glycol) monomethyl ether (MPEG) were copolymerized using the ionizable 2‐acrylamido‐2–methyl propane sulfonic acid (AMPS) via different dose rate of electron‐beam irradiation (40–150 kGy). The crosslinking of the copolymers were carried out in aqueous acidic solutions at pH 1 or in the presence of 1% N,N‐methylene bisacrylamide (MBA) as crosslinking agent. The final equilibrium water content and swelling capacities for the prepared hydrogels were determined in aqueous solutions at pH 1, 6.8, and 12 and in aqueous salt solutions at 298 K. Swelling equilibria for prepared hydrogels were determined in different molar salt solutions of NaCl, KCl, CaCl2, Na2SO4, K2SO4, and CaSO4. The swelling ratios of gels in pure water and in the salt solutions were found to depend on the counterion species in the increasing sequence of Ca2+, Na+ and K+. Copyright © 2002 John Wiley & Sons, Ltd.  相似文献   

19.
A 100-fold preconcentration procedure based on rare-earth elements (REEs) separation from water samples with an extraction chromatographic column has been developed. The separation of REEs from matrix elements (mainly Fe, alkaline and alkaline-earth elements) in water samples was performed loading the samples, previously acidified to pH 2.0 with HNO3, in a 2 ml column preconditioned with 20 ml 0.01 M HNO3. Subsequently, REEs were quantitatively eluted with 20 ml 7 M HNO3. This solution was evaporated to dryness and the final residue was dissolved in 10 ml 2% HNO3 containing 1 μg l−1 of cesium used as internal standard. The solution was directly analysed by inductively coupled plasma mass spectrometry (ICP-MS), using ultrasonic nebulization, obtaining quantification limits ranging from 0.05 to 0.10 ng l−1. The proposed method has been applied to granitic waters running through fracture fillings coated by iron and manganese oxy-hydroxides in the area of the Ratones (Cáceres, Spain) old uranium mine.  相似文献   

20.
《Analytical letters》2012,45(5):890-901
Abstract

A highly selective polyvinyl chloride (PVC) membrane electrode, based on N,N′‐(aminoethyl)ethylenediamide bis(2‐benzoideneimine) binuclear copper(II) complex [Cu(II)‐AEBB] as neutral carrier, was prepared for thiocyanate (SCN?) determination, which displays an anti‐Hofmeister selectivity sequence for a series of anions in the following order: SCN?>ClO4 ?>Sal? > I?>NO3 ?>Br?> Cl?>NO2 ?>SO3 2?>F?>H2PO4 ?>SO4 2?. The electrode exhibited near‐Nernst response for SCN? with a slope of –59.0 mV/decade over a wide concentration range (8.5×10?7~6.8×10?1 mol/L) with a detection limit of –5.0×10?7 mol/L in pH 5.0 phosphate buffer solution at 25°C. Alternating current (AC) impedance and equivalent circuits were used to investigate the thiocyanate response mechanism of the membrane doped with [Cu(II)‐AEBB].  相似文献   

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