Foam Separation of Cadmium From Waste Water

Foam separation techniques are evaluated to determine if they would be feasible for removing cadmium (II) from waste water. Variables such as pH, ionic strength, collector concentration, and interfering ions were studied to determine their effects on separation. Sodium laury sulfate, sodium sterate, and hexadecyltrimethyl-ammonium bromide were chosen as the collector; Fe(OH)₃ and Al(OH)₃ were used as the adsorbing colloid, and sodium tripolyphosphate was used as modifier. It was found that cadmium could be effectively removed using various foam separation techniques. Cadmium levels were reduced from 5 ppm to 0.003 ppm in 60 minutes foaming with sodium laury sulfate. Foam separation of cadmium sterate with hexadecyltrimethyl-ammonium bromide was effective even at very high ionic strength, such as 1.0M NaNO₃.     

Ion and Adsorbing Colloid Flotation of Auramine

Auramine, a cationic dye, was removed from synthetic wastewater by ion flotation of auramine‐sodium lauryl sulfate complex. Over 98% of auramine was removed from the solution in 15 min. A stoichiometric amount of surfactant (1 mol of surfactant to 1 mol of dye) was found to be most effective for auramine removal. The rate of separation and ultimate removal of auramine increased with increasing the rate of air flow and decreased with increasing concentration of NaNO₃. Auramine was also removed by adsorbing colloid flotation technique using ferric hydroxide as the coagulant. Sodium lauryl sulfate was used as the collector, and over 95% of auramine was removed in 10 min. The separation efficiency decreased with increasing ionic strength of the solution. The deleterious effect of neutral salt was compensated somewhat with the aid of aluminum ions as the activator. Both ion flotation and adsorbing colloid flotation are promising approaches for the removal of cationic dye from wastewater.     

Removal of Safranine from Aqueous Solution by Using Adsorptive Bubble Separation Techniques

Safranine, a cationic dye, was removed from synthetic wastewater by ion flotation. Over 98% of safranine was removed from the solution in 10 min. A stoichiometric amount of surfactant (1 mol of surfactant to 1 mol of dye) was found to be most effective for safranine removal. The separation efficiency of safranine decreased with increasing concentration of NaNO3. Safranine was also removed by adsorbing colloid flotation technique using Fe(OH)3 as the coagulant. Sodium lauryl sulfate was used as the collector, and over 97% of safranine was removed in 5 min. The separation efficiency decreased with increasing ionic strength of the solution. The deleterious effect of neutral salt was compensated somewhat with the aid of Al^3 as the activator. Both ion flotation and adsorbing colloid flotation may be applicable in the removal of safranine from wastewater.     

Separation of Co(II) from dilute aqueous solutions by precipitate and adsorbing colloid flotation

Ion, precipitate and adsorbing colloid flotation of cobalt(II) have been investigated at different pH values, using N-dodecylpyridinium chloride (DPCl), A strong cationic surfactant, and sodium lauryl sulfate (NaLS), a strong anionic surfactant, as collectors. In case of adsorbing colloid flotation, hydrous manganese dioxide was used as an adsorbent. The precipitate flotation curves experimentally obtained with the two tested collectors were compared with the corresponding theoretical one calculated from the data published for Co(II) hydrolysis. The effects of the collector concentration, ageing of the water-MnO₂–Co(II) system, bubbling time period, cobalt(II) concentration and foreign salts on the percent removal of Co(II) by adsorbing colloid flotation using DPCl as collector were determined. Removals approaching 100% could be achieved under the optimum conditions.     

Electrosorption of manganese dioxide on electrochemically modified carbon fiber nonwoven materials

Electrosorption of manganese dioxide on an electrochemically activated carbon fiber nonwoven electrode was studied as influenced by the current density, solution flow-through rate, and concentration of the MnO(OH)₂ colloid solution. It was found that manganese hydroxide can be deposited onto electrochemically activated fibers of fibrous carbon materials by different methods: (1) electrosorption of MnO(OH)₂ from its colloid solution, (2) synthesis of MnO(OH)₂ directly on the fibrous carbon material sample, and (3) impregnation with an MnO(OH)₂ colloid solution.     

Measurement of the Hydrolysis of Tin Tetraacetate by Proton and Carbon-13 NMR Spectroscopy

Solid-state ^l3C CP/MAS spectral analysis of the hydrolysis products of Sn(OAc)₄ allowed the hydrolysis intermediates, Sn(OH)(OAc)₃, Sn(OH)₂(OAc)₂ and Sn(OH)₃(OAc), to be identified. The results show that the hydrolysis consists of three steps; the first and second steps are consecutive reactions and the third is reversible. Intermolecular exchange between hydrolysis products (i.e. Sn(OAc)⁴, Sn(OH)(OAc)₂, Sn(OH)₂(OAc)₂ and Sn(OH)₃(OAc),) and acetic acid was observed from the measurement of ¹H and ¹³C solution spectra at varied temperatures in CD₂Cl₂ with ΔG^?₃₄₈ 50.5 kJ mol^?1.     

Hydroxoverbindungen. 10. Über die Natriumoxohydroxostannate(II) Na4[Sn4O(OH)10] und Na2[Sn2O(OH)4]

Hydroxo Compounds. 10. The Sodium Oxohydroxostannates(II) Na₄[Sn₄O(OH)₁₀] and Na₂[Sn₂O(OH)₄] Na₄[Sn₄O(OH)₁₀] = Na₄[Sn(OH)₃]₂[Sn₂O(OH)₄] ( I ) and Na₂[Sn₂O(OH)₄] ( II ) have now been doubtlessly characterized as the first Na-hydroxostannates(II). I crystallizes monoclinic in P2₁/n (a = 1522.4(5) pm, b = 830.0(2) pm, c = 1276.0(3) pm, β = 104.8(2)°, Z = 4, R = 0.047, 1137 I_hkl); II crystallizes orthorhombic in P2₁2₁2₁ (a = 1450(2) pm, b = 1665(2) pm, c = 590.7(8) pm, Z = 8, R = 0.042, 1208 I_hkl). II is identical with the compound which was described up to now as “Na[Sn(OH)₃]”. The new compounds contain the complex anions [Sn(OH)₃]^? and [Sn₂O(OH)₄]^2?, whose structures are now proved. The oxotetrahydroxo-distannate(II) anion [Sn₂O(OH)₄]^2? exhibits a syn-conformation with respect to the projection along the (Sn? Sn) vector. The two compounds crystallize with pronounced layer structures, which show direct topotactical relations with one another as well as with SnO. This relates closely to the fast formation of SnO from crystals of I and II .     

Electrochemical determination of Sn(IV)/Sn(II) ratio in tin sol formed in copper–tin sulphate solution containing laprol 2402C

The electrochemical method was applied to determine Sn(IV)/Sn(II) molar ratio in negatively charged colloid which forms in bronze plating sulphate solution containing laprol 2402C as a surface-active substance. An analysis of characteristic voltammetric minimum the onset of which is highly sensitive to Sn²⁺ concentration was used for this purpose. The Sn(IV)/Sn(II) ratio was found to be constant for completely formed colloid and independent on Cu(II) concentration in the solution. Particles involving Sn(IV) are supposed to be the main component responsible for stability of the sol.     

New Insights into the Formation and Reactivity of Molecular Organostannonic Acids

The controlled base hydrolysis of 2,6‐Mes₂C₆H₃SnCl₃ ( 1 ; Mes=mesityl) provided 2,6‐Mes₂C₆H₃Sn(OH)Cl₂?H₂O ( 2 ) and the trinuclear organostannonic acid trans‐[2,6‐Mes₂C₆H₃Sn(O)OH]₃ ( 3 ), respectively. In moist C₆D₆, 3 reversibly reacts with water to give the monomeric organostannonic acid 2,6‐Mes₂C₆H₃Sn(OH)₃ ( 3a ). The reaction of 3 with (tBu₂SnO)₃, Ph₂PO₂H, and NaH, gives rise to the multinuclear hypercoordinated organostannoxane clusters [tBu₂Sn(OH)OSnR(OH)₂OC(OSntBu₂OH)₂(O)SnR(OH)(H₂O)]₂ ( 5 ), [RSn(OH)₂(O₂PPh₂)]₂ ( 6 ), and Na₃(RSn)₄O₆(OH)₃ ( 7 ), respectively (R=2,6‐Mes₂C₆H₃). The characterization of the new compounds is achieved by multinuclear NMR spectroscopy and electrospray mass spectrometry in solution and ¹¹⁹Sn MAS NMR spectroscopy, IR spectroscopy, and X‐ray crystallography in the solid‐state.     

Preparation and thermal analysis of synthetic malachite CuCO3·Cu(OH)2

The synthesis of malachite CuCO₃·Cu(OH)₂ or Cu₂CO₃(OH)₂ was studied through titrations of copper(II) salt solutions with a solution of sodium carbonate at different temperatures. The precipitates were characterized by TG, IR and chemical analysis. The composition varies depending on thepH of the solution and the temperature. Purer malachite was synthesized by simple mixing of a solution of copper(II) nitrate or sulfate with a solution of sodium carbonate at 50°C.The kinetics of the thermal decomposition of synthetic malachite was described by eitherR ₃ orA _m(m=1.2–1.4) law, according to TG analysis, both isothermal and nonisothermal. The Arrhenius parameters determined using three different integral methods showed the kinetic compensation effect, which is correlated to the working temperature interval analyzed.The authors thank Mr. H. Takemoto for analyzing kinetics of the thermal decomposition of synthetic malachite.     

Methylation of tin(II) by methyl iodide: influences of different environmental factors on the efficiency and reaction kinetics

The methylation reaction of Sn(II) with methyl iodide (MeI) in water has been studied using sensitive GC-QSIL-FPD technology. The pH value, amount of MeI and salinity (S) are the three important factors that influence the methylation reaction in an aquatic environment. In all experiments, monomethyltin (MMT) is the only methylation product of the tin(II) reacting with MeI observed. At the 95% confidence level, the pH, MeI and S are significant for the MMT yield. The concentration of MMT in the reactor increases with increase in pH within the selected pH range of 4–9 because four different species of Sn(II)–Sn²⁺, SnOH⁺, Sn(OH)₂⁰ and Sn(OH)₃⁻–have different reaction activities with MeI. The methylation activity of Sn(II) was found to be highest at a salinity of 0.1 M at three different pH levels: 5, 7 and 9. Higher concentration of Cl⁻ (as a relatively weak nucleophilic ion) will obstruct nucleophilic attack of Sn(II) on MeI. MMT production also increases with rising volume of MeI. Moreover, first-order reaction rates have been calculated at different pH, salinity and MeI, and found to be in the range 0.0018–0.0199 h⁻¹. The reaction rate also varies largely under different reaction conditions. One probable mechanism for the methylation reaction of Sn(II) with MeI is a S_N2 nucleophilic attack on the methyl group of MeI by Sn(II), via a process of oxidative methyl-transfer. Copyright © 2006 John Wiley & Sons, Ltd.     

Adsorptive Bubble Separation of Dinitrophenol

Dinitrophenol was removed from aqueous solution by various adsorptive bubble separation techniques. Foam fractionation of dinitrophenol with hexadecyltrimethylammonium bromide(HTA) was most effective with over 99% removal in 15 min. The addition of a surfactant in greater than stoichiometric amounts was required for effective separation. Solvent sublation of the dinitrophenol-HTA complex was also effective. The separation efficiency of solvent sublation of dinitrophenol-HTA was similar to that of foam fractionation. The separation by solvent sublation of dinitrophenol without adding any surfactant was very poor. Adsorbing colloid flotation with Fe(OH)₃ was not effective in removing dinitrophenol from aqueous solution.     

Preparation and Characterization of Ceramic Hollow Microspheres for Heavy Metal Ion Removal in Wastewater

Ceramic hollow microspheres (CHMSs) were prepared to use as supports for the removal of heavy metal ions from industrial waste-water. A water extraction sol–gel technique was used to prepare porous CHMS by extracting water from an emulsion of LUDOX (silica colloid; SiO₂, Aldrich Co.) and 2-ethyl-1-hexanol. Experiments were conducted to control pore size, wall thickness, and separation yield by examining the ratio of precursors (LUDOX and 2-ethyl-1-hexanol), catalyst (NH₄OH), sintering temperature, surfactant (SPAN 80), extractant (n-butanol), stirring speed, and concentration of precursor (LUDOX). The results revealed that the optimum conditions were 20 ml of a 10 wt% solution of LUDOX, 10 ml of NH₄OH, a sintering temperature of 500°C, 0.4 ml of SPAN 80, 200 ml of n-butanol, and a stirring speed of 730 rpm/100 ml of 2-ethyl-1-hexanol. CHMSs were impregnated in Cyanex 272 and examined for their ability to remove heavy metal ions from a solution. Based on an experiment involving the removal of metal ions using CHMSs that were prepared under optimum conditions, Zn ion was removed at a level of 0.354 mmol/g at pH 4, which was about twice the adsorption capacity of CHMSs prepared by Wilcox (Mater. Res. Soc. Symp. Proc.346, 201 (1994)).     

Speciation and NMR Spectrometric Studies of Interaction of Di- and Tri-organotin(IV) Moieties with 5′-Guanosine Monophosphate and Guanosine in Aqueous Solution

Potentiometric studies of the interaction of (Me₂Sn)²⁺ and (Me₃Sn)⁺ with 5′-guanosine monophosphate [(5′-HGMP)^2?, abbreviated as (HL-1)^2?] and guanosine [(HGUO), abbreviated as (HL-2)] in aqueous solution (I = 0.1 mol·dm^?3 KNO₃, 298.15 ± 0.1 K) were performed, and the speciation of various complex species was evaluated as a function of pH. The species that exist at physiological pH ~7.0 are Me₂Sn(HL-1)/[Me₂Sn(HL-2)]²⁺ (87.0/88.8 %), [Me₂Sn(HL-1)(OH)]^?/[Me₂Sn(HL-2)(OH)]⁺ (3.0/0 %) and [Me₂Sn(HL-1H_?1)]/[Me₂Sn(HL-2H_?1)]²⁺ (9.4/6.6 %) for 1:1 dimethyltin(IV):5′-guanosine monophosphate/dimethyltin(IV): guanosine systems, whereas for the corresponding 1:2 systems, the species are Me₂Sn(HL-1)/[Me₂Sn(HL-2)]²⁺ (44.0/92.0 %), [Me₂Sn(HL-1H_?1)]/[Me₂Sn(HL-2H_?1)]²⁺ (5.0/6.0 %), Me₂Sn(OH)₂ (49.0/0 %), [Me₂Sn(HL-1)(OH)]^?/[Me₂Sn(HL-2)(OH)]⁺ (1.5/2.0 %), and [Me₂Sn(OH)]⁺ (1.0/0 %). For 1:1 trimethyltin(IV):5′-guanosine monophosphate/trimethyltin(IV):guanosine systems, only [Me₃Sn(HL-1)]^?/[Me₃Sn(HL-2)]⁺ (99.9 %) are found at pH = 7.0, whereas for 1:2 systems, [Me₃Sn(HL-1)]^?/[Me₃Sn(HL-2)]⁺ (49.8/100 %), Me₃Sn(OH) (15.0/0 %) and [Me₃Sn(HL-1)(OH)]^2?/Me₃Sn(HL-2)(OH) (0.2/0 %) are the species found. No polymeric species were detected. Beyond pH = 8.0, significant amounts of [Me₂Sn(OH)]⁺, Me₂Sn(OH)₂, [Me₂Sn(OH)₃]^? and Me₃Sn(OH) are formed. Multinuclear (¹H, ¹³C and ¹¹⁹Sn) NMR studies at different pHs indicated a distorted octahedral geometry for the species Me₂Sn(HL-1)/[Me₂Sn(HL-2)]²⁺ in dimethyltin(IV)-(HL-1)^2?/(HL-2) systems and a distorted trigonal bipyramidal/distorted tetrahedral geometry for the species [Me₃Sn(HL-1)]^?/[Me₃Sn(HL-2)]⁺ in trimethyltin(IV)-(HL-1)^2?/(HL-2) systems.     

Trapping Dimethyltin Cations by Bipyridine‐N,N′‐Dioxide Ligands

N,N′‐dioxide ligands such as 2, 2′‐bipyridine‐N,N‐dioxide (BPDO‐I) and 4, 4′‐bipyridine‐N,N‐dioxide (BPDO‐II) were used to trap the hydrated dimethyltin cations under controlled hydrolysis. The use of the chelating ligand BPDO‐I leads to the isolation of the discrete monocation [Me₂Sn(BPDO‐I)(OH₂)(NO₃)]⁺[NO₃]^– ( 2 ), whereas the linear ligand BPDO‐II directs the construction of cationic polymers, [{Me₂Sn(OH₂)₂(μ‐BPDO‐II)}²⁺{NO₃^–}₂ · 2H₂O]_n ( 3· 2H₂O) and [{Me₂Sn(μ‐OH)(BPDO‐II)}₂²⁺{NO₃^–}₂ · H₂O]_n ( 4· H₂O) under different reaction conditions.     

Production of <Superscript>122</Superscript>Sb for the study of environmental pollution

This article presents, ¹²²Sb (T _1/2 = 2.723 days, I _β- = 97.59%) was produced via the ^natSn(p,xn) nuclear process at the AMIRS (Cyclone-30, IBA, Belgium). The electrodeposition experiments were carried out by potassium stannate trihydrate (K₂Sn(OH)₆) and potassium hydroxide. The optimum conditions of the electrodeposition of tin were as follows: 40 g/L ^natSn, 20 g/L KOH, 115 g/L K₂Sn(OH)₆, DC current density of 5 A/dm² with a bath temperature of 75 °C. The electroplated Tin-target was irradiated with 26.5 MeV protons at current of 180 μA for 20 min. Solvent extraction of no-carrier-added ¹²²Sb from irradiated Tin-natural target hydrochloric solution was investigated using di-n-butyl ether (C₈H₁₈O). Yields of about 3.61 MBq/μAh were experimentally obtained.     

New Insights in Asymmetric Tetraorganodistannoxane Ladder Formation. A NMR‐Spectroscopic and Crystallographic study

The syntheses of the asymmetrically substituted tetraorganodistannoxanes [t‐Bu₂(X)SnOSn(Y)(CH₂SiMe₃)₂]₂ ( 1 , X = Y = OH; 2 , X = Cl, Y = OH; 3 , X = Y = Cl) are reported and their structures in solution and in the solid state are characterized by multinuclear NMR spectroscopy and single crystal X‐ray analyses. In toluene, the tetrahydroxy‐substituted derivative 1 is in equilibrium with the organotin oxides cyclo‐[t‐Bu₂Sn{OSn(CH₂SiMe₃)₂}₂O] ( 4 ), cyclo[(Me₃SiCH₂)₂Sn(OSnt‐Bu₂)₂O] ( 5 ), and cyclo‐(t‐Bu₂SnO)₃, and some additional, undefined species containing pentacoordinated tin atoms. In contrast, the dihydroxydichloro‐substituted derivative 2 is inert in solution.     

Multi‐Pyrene Assemblies Supported on Stannoxane Frameworks: Synthesis,Structure and Photophysical Studies

Organostannoxanes have been used as scaffolds for the preparation of multi‐chromophore assemblies. A single‐step synthesis procedure allows the preparation of compounds in which the number of chromophore units can be varied from two to six. Thus, the reactions of pyrene sulfonic acid (PySO₃H) or C₁₆H₉CHNC₆H₃(COOH)₂ (LH₂) with various organotin precursors gave pyrene‐containing organostannoxanes, that is, [Ph₃SnPySO₃]₆ ( 1 ), [{(Me₂Sn)₂(μ₃‐O)(μ‐OH)PySO₃}₂{(Me₂Sn)₂(μ₃‐O)(μ‐OH)H₂O}₂ ? 2 PySO₃] ( 2 ), [{tBu₂Sn(OH)PySO₃}₂] ( 3 ), [{(nBuSn)₁₂(O)₁₄(OH)₆{PySO₃}₂] ( 4 ), and [{(nBu₂Sn)L}₃]₂ ? C₆H₅CH₃ ( 5 ). Compounds 1 – 5 were characterized by using X‐ray crystallography. Compounds 1 and 5 are 24‐membered macrocycles. Macrocycle 1 possesses intramolecular π–π stacking interactions. An unusual co‐crystal of two tetrameric ladders in 2 was observed in which one of the components of the co‐crystal is neutral whereas the other is dicationic and two pyrenesulfonate counterions are present to balance the overall charge. In the solid state these compounds reveal rich supramolecular structures. Photophysical studies on 1 – 5 reveal that interactions in the solid state lead to considerable broadening of the emission bands.     

Mössbauer and infrared spectroscopic studies of some organotin(IV) schiff base complexes

Several organotin(IV) complexes with quadri- and terdentate anionic Schiff base ligands have been investigated in the solid state using ¹¹⁹Sn Mössbauer and IR spectroscopies, Mössbauer parameters derived from both zero-field and magnetically perturbed spectra suggest that the R₂Sn(Salen)(R = Me, Et, Ph) and Me₂Sn(Saldap-2OH) complexes have similarly distorted trans-octahedral structures. However, in Ph₂Sn(HSaldap-2-O) the ligand appears to be only terdentate, leading to a penta-coordinate structure similar to those of the R₂Sn(Sal-N-2-OC₆H₄) derivatives (R = Me, Ph). For Ph₃Sn(Sal-N-2-OC₆H₄) the asymmetry parameter of the electric field gradient is close to unity, confirming a mer-octahedral configuration for this complex.     

Speciation and Multinuclear NMR Spectroscopic Studies of Di- and Trimethyltin(IV) Moieties with MESNA in Aqueous Medium

The interaction of Me₂Sn(IV)²⁺ and Me₃Sn(IV)⁺ with a prodrug, sodium 2-mercaptoethane sulfonate (HSCH₂CH₂SO₃Na, MESNA) abbreviated as (HL), has been studied potentiometrically in aqueous solution (I = 0.1 mol·L^?1 KNO₃, 298 K). The concentration distribution of various species formed in the solution was studied with changes in pH (~3–11). A strong coordination of MESNA with metal through the S atom of thiol group has been found. In the Me₂Sn(IV)–HL system, the species [Me₂Sn(L)]⁺ (53.1–75.6%) is predominant at acidic pH (3.73 ± 0.02) and the species [Me₂Sn(L)₂OH]^? (29.4–38.5%) is predominant at basic pH (10.32 ± 0.08). In contrast, for the Me₃Sn(IV)⁺ system, [Me₃SnL] (37.0–57.4%) is the major species at pH 7.65 ± 0.03 and [Me₃Sn(OH)] (49.9–67.2%) and [Me₃Sn(L)(OH)]^? (30.2–46.5%) are the major species at pH 11.05 ± 0.01. However, at physiological pH (7.01 ± 0.32), in both (1:1) and (1:2) Me₂Sn(IV)–HL systems, the species [Me₂Sn(L)(OH)] (67.2–89.9%) is predominant, whereas for Me₃Sn(IV)–HL (1:1) and (1:2) systems, [Me₃Sn(OH)] (53.5%) and [Me₃SnL] (56.8%) are the respective predominant species. In order to characterize the possible geometry of the proposed complex species, multinuclear (¹H, ¹³C and ¹¹⁹Sn) NMR studies were carried out at different pHs. No polymeric species were detected in the experimental pH range.