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1.
The complexes formed between IE11 and Cd(II), Cr(III), Cu(II), Mn(II) and Pb(II) were identified and confirmed by IR, UV and pH-metric titration. The uptake behavior of porous silica modified with N-propylsalicylaldimine (IE11) and these metal ions were studied. Log k(d) was found to be within the range 2.19-5.16 depending on pH and time of stirring. IE11 was used in the separation and preconcentration of Cd(II), Cr(III, VI), Cu(II), Mn(II, VII) and Pb(II) from some natural water samples. Data were compared with those obtained by the solvent extraction method APDC/MIBK. The proposed methodology allows to verify an improvement in the water quality of Nile River probably attributed to high to moderate floods in the last few years. The method was found to be accurate and not subject to random error, i.e. precise.  相似文献   
2.
Free silanol groups of silica-gel functionalized with quercetin (QSG) were blocked with TiO2 or ZrO2 to produce TiO2-QSG and ZrO2-QSG, respectively. The silica materials were characterized by infrared, Raman spectra, thermogravimetric, elemental analyses, magic angle spinning 13C-nuclear magnetic resonance, BET specific surface area measurements and inductively coupled plasma—optical emission spectrometry-monitored silica hydrolysis. Siloxane groups are reinforced in the blocked QSG samples without affecting the hydrophilic nature or the porosity of silica. Quercetin is unaffected by the titania layer in contrary to zirconia. Also, the stability of silica against hydrolysis in TiO2-QSG and ZrO2-QSG was remarkably improved in the range of pH 3.5–9.1, attributed to the interruption of the intramolecular interaction of silanol groups with the amino groups. The hydrolyzed silica of TiO2-QSG and ZrO2-QSG decreased to 46.6 and 18.5%, of that of QSG and to 7.6 and 3.1%, of that of 3-aminopropylsilica gel at pH 9.1, respectively. TiO2-QSG was applied for the extraction of Hg(II) with separation efficiency of 99.0 ± 0.6% at pH 8.5. The capacity loss of TiO2-QSG per recovery cycle of Hg(II) was lowered in comparison with the uncovered material. It was successfully applied for the recovery of Hg(II) from spiked water and referenced samples.  相似文献   
3.
MnO2 was chemically prepared from birnessite (CMD2D) and from spinel-like LiMn2O4 (CMD3D) by acid leaching. X-ray diffractometry, FTIR spectrometry, chemical and thermal analyses were used to determine the structure and chemical disorder. On the basis of cation vacancy model, the structural water was found to be mainly due to Coleman protons in both samples. Both samples were found to be of very close structure belonging to γ-MnO2 type I according to Chabre and Pannetier classification with de Wolff disorder (Pr) of 0.19 and 0.30 and microtwinning (Tw) of 9.9 and 17%, respectively. The activation energy of structural water release calculated from thermal analysis was apparently higher than that of other γ-MnO2 types (150 and 156.6 kJ/mol, respectively).A high reduction capacity in aqueous and non-aqueous batteries was delivered for both samples except for the electro- chemical lithium insertion of CMD2D, which was attributed to the different oxygen packing.  相似文献   
4.
A novel tetrachlorothallate (III) (TCT)-selective membrane sensor consisting of tetrachlorothallate (III)-2,3,5-triphenyl-2-H-tetrazolium ion pair dispersed in a PVC matrix plasticized with dioctylphthalate is described. The electrode shows a stable, near-Nernstian response for 1×10−3-4×10−6 M thallium (III) at 25 °C with an anionic slope of 56.5±0.5 over the pH range 3-6. The lower detection limit and the response time are 2×10−6 M and 30-60 s, respectively. Selectivity coefficients for Tl(III) relative to a number of interfering substances were investigated. There is negligible interference from many cations and anions; however, iodide and bromide are significantly interfere. The determination of 0.5-200 μg ml−1 of Tl(III) in aqueous solutions shows an average recovery of 99.0% and a mean relative standard deviation of 1.4% at 50.0 μg ml−1. The direct determination of Tl(III) in spiked wastewater gave results that compare favorably with those obtained by the atomic absorption spectrometric method. The electrode was successfully applied for the determination of thallium in zinc concentrate. Also the tetrachlorothallate electrode has been utilized as an end point indicator electrode for the determination of thallium using potentiometric titration.  相似文献   
5.
The stability of aminopropyl-silica gel (AP-SG) against hydrolysis was investigated after modification by 2,3-butanedione monoxime (BDMO), 8-hydroxyquinoline-2-carboxaldehyde (HQC) or isatin (Is) by Schiff’s base condensation reaction. The hybrid modified silica gel (HMSG) compounds; BDMO-SG, HQC-SG and Is-SG were characterized by IR, thermogravimetric and elemental analyses, magic angle spinning-13C-nuclear magnetic resonance, pH-metric titration and inductively coupled plasma–optical emission spectrometry-monitored silica hydrolysis. The stability of the HMSG’s was found to be dependant on the type of the functionalization group, which may protect the silica surface via; (1) the delocalization of the free lone pair of electrons on nitrogen of the propylamine group in the aromatic rings, which reduces local basicity experienced on the silica surface, (2) the hydrophobic nature of the organic substrates, which hinders the attack of hydroxide ions and water molecules, and (3) the bulky organic substrate, which hinders nucleophilic attack on silicon. HQC-SG is recommended as an optimal modification to meet the requirements of stability, capacity and separation efficiency of Hg(II) at pH 4.1.  相似文献   
6.
Silica gel was firstly functionalised with aminopropyltrimethoxysilane obtaining the aminopropylsilica gel (APSG). The APSG was reacted subsequently with morin yielding morin-bonded silica gel (morin-APSG). The structure was investigated and confirmed by elemental and thermogravimetric analyses, IR and (13)C NMR spectral studies. Morin-APSG was found to be highly stable in common organic solvents, acidic medium (<2molL(-1) HCl, HNO(3)) or alkaline medium up to pH 8. The separation and preconcentration of Ag(I), Au(III), Pd(II), Pt(II) and Rh(III) from aqueous medium using morin-APSG was studied. The optimum pH values for the separation of Ag(I), Au(III), Pd(II), Pt(II) and Rh(III) on the sorbent are 5.7, 2.2, 3.7, 3.7 and 6.8, giving rise to separation efficiencies of 43.9, 85.9, 97.7, 60.9 and 91.0%, respectively, where the activity was found to be >90% in the presence of acetate ion. The ion sorption capacity of morin-APSG towards Cu(II) at pH 5.5 was found to be 0.249mmolg(-1) where the sorption capacities of Ag(I) and Pd(II) were 0.087 and 0.121mmolg(-1) and 0.222 and 0.241mmolg(-1) at pH 2.2 and 5.7, respectively. This indicates a 1:1 and 1:2 morin/metal ratios at pH 2.2 and 5.7, respectively. Complete elution of the sorbed metal ions was carried out using 10mL (0.5molL(-1) HCl+0.01molL(-1) thiourea) in case of Au(III), Pd(II), Pt(II) and Rh(III) and 10mL 0.5molL(-1) HNO(3) in case of Ag(I). Morin-APSG was successfully employed in the separation and preconcentration of the investigated precious metal ions from some spiking water samples yielding 100-folds concentration factor. The relative standard deviation (R.S.D.) and the T-test (|t|(1)) were calculated.  相似文献   
7.
Controlled-pore silica glass modified with N-propylsalicylaldimine (SCPSG) has been investigated as a surface-active matrix for the separation of some metal ions. The porous silica glass base was confirmed to have better stability towards hydrolysis in aqueous solution buffered at pH=9 in comparison to silica gel, which showed twice the surface area of controlled-pore silica glass. The different analytical parameters affecting the batch mode separation and preconcentration of trace Al(II), Ag(I) and Hg(II) in environmental samples using SCPSG, prior to their determination using inductively coupled plasma mass spectrometry (ICP-MS), were studied. The optimum conditions are pH 9.0 +/- 0.1, time of stirring 30 min and the eluent concentration 0.5 mol dm(-3) HNO3. The ion-exchange capacity of SCPSG with respect to Al(III), Ag(I) and Hg(II) was 0.27, 0.18 and 0.23 mmol g(-1), respectively. The recovery values for the metal ions were 96.8 +/- 0.86, 98.1 +/- 0.60 and 96.2 +/- 1.06%, and the analytical detection limits were 26.1, 1.49 and 0.44 pg cm(-3), respectively, for a preconcentration factor of 100. The method has been applied to the determination of the investigated metal ions in natural water samples as well as certified and reported samples and the results were found to be accurate.  相似文献   
8.
The electrochemical behaviour of some hydrated layered manganese dioxides previously prepared and characterised was investigated by galvanostatic and potentiostatic studies at different conditions of temperature, type of electrolyte and counter electrode, number of cycles and depth of reduction.

Reversible range was found to be a homogeneous reaction, which is limited up to 0.23 e/f.u., whereas the major theoretical capacity is consumed in two heterogeneous reduction reactions yielding Mn(OH)2 at the end. Spinel-like phases such as hausmannite and hetaerolite are formed during the heterogeneous stage. The formation of the spinel-like phases was found to decrease at low temperature in the absence of aggressive ions such as Zn2+ and at shallow depth of reduction.

The mechanism of the electrochemical reduction of the heterogeneous stage is suggested to proceed via an intermediate with the hydrotalcite structure, which undergoes conversion to Mn3O4. The chemical reduction of manganese dioxides was also investigated and was found to support this suggestion.  相似文献   

9.
A new sensitive chromogenic reagent, 9,10-phenanthaquinone monoethylthiosemicarbazone (PET), has been synthesized and used in the spectrophotometric determination of Tl(III). In HNO3, H2SO4 or H3PO4 acids, PET can react immediately at room temperature with Tl(III) to form a red 2:1 complex with a maximum absorption at 516 nm. The different analytical parameters affecting the extraction and determination processes have been examined. The calibration curve was found to be linear over the range 0.2-10 microg cm(-3) with a molar absorptivity of 2.2 x 10(4) dm3 mol(-1) cm(-1). Sandell's sensitivity was found to be 0.0093 microg cm(-2). No interference from macroamounts of foreign ions was detected, except for Pd(II). However, Pd(II) does not affect the determination process, because its complex with PET has its lambda(max) at 625 nm. The proposed method has been applied to the determination of Tl(I and III) in synthetic and natural samples after separation by flotation (in oleic acid/kerosene) and solid-phase extraction (on polyurethane foam) techniques. The two methods were found to be accurate and not subject to random error, but solid-phase extraction was preferred because it is cheap, simpler and there is no contamination risk coming from flotation reagents.  相似文献   
10.
Silanol groups of n-aminopropyl silica gel (APSG) were blocked with TiO2 or ZrO2 to produce Ti-APSG and Zr-APSG, respectively. The silica materials were characterized by infrared, Raman spectra, thermogravimetric, elemental analyses, magic angle spinning 13C-nuclear magnetic resonance, specific surface area measurements, pH-metric titration and inductively coupled plasma—optical emission spectrometry—monitored silica hydrolysis. The stability of APSG against hydrolysis was found to be mainly affected by the specific surface area and the basicity of the n-aminopropyl groups which acquire additional strength from their intramolecular interaction with the silanol groups. The hydrolysis of silica in Ti-APSG and Zr-APSG remarkably decreased in the range of pH 1.0–9.1 due to the interruption of that intramolecular interaction. The hydrolyzed silica of Ti-APSG and Zr-APSG was decreased to 22.7 and 29.9%, respectively, of that of APSG at pH 4.5. Capacity and stability of Ti-APSG and Zr-APSG were improved in comparison with APSG upon application in the extraction of Cu2+ for 20 cycles of extraction and regeneration.  相似文献   
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