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1.
Preconcentration techniques for uranium(VI) and thorium(IV) prior to analytical determination-an overview 总被引:1,自引:0,他引:1
The need for the preconcentration of trace and ultratrace amounts of uranium(VI) and thorium(IV) in conjunction with various detection techniques was clearly brought out in the introductory part. Subsequently, various off-line and on-line procedures developed for uranium(VI) and thorium(IV) prior to their analytical determination since 1990 were critically reviewed in terms of enrichment factor, retention/sorption capacity, validation using certified reference materials and application to complex real samples. The relative merits and demerits of various preconcentration and/or separation of uranium(VI) and thorium(IV) prior to quantitation by a plethora of analytical techniques are discussed in concluding part of the review article. 相似文献
2.
A simple and effective method is presented for the separation and preconcentration of thorium(IV) and uranium(VI) by solid phase extraction on Duolite XAD761 adsorption resin. Thorium(IV) and uranium(VI) 9-phenyl-3-fluorone chelates are formed and adsorbed onto the Duolite XAD761. Thorium(IV) and uranium(VI) are quantitatively eluted with 2 mol L−1 HCl and determined by inductively coupled plasma-mass spectrometry (ICP-MS). The influences of analytical parameters including pH, amount of reagents, amount of Duolite XAD761 and sample volume, etc. were investigated on the recovery of analyte ions. The interference of a large number of anions and cations has been studied and the optimized conditions developed have been utilized for the trace determination of uranium and thorium. A preconcentration factor of 30 for uranium and thorium was achieved. The relative standard deviation (N = 10) was 2.3% for uranium and 4.5% for thorium ions for 10 replicate determinations in the solution containing 0.5 μg of uranium and thorium. The three sigma detection limits (N = 15) for thorium(IV) and uranium(VI) ions were found to be 4.5 and 6.3 ng L−1, respectively. The developed solid phase extraction method was successively utilized for the determination of traces thorium(IV) and uranium(VI) in environmental samples by ICP-MS. 相似文献
3.
A study on the feasibility of preparing cellulose from sugarcane bagasse, by means of chemical procedures including acid hydrolysis and alkaline treatment was conducted. The extracted purified cellulose was further used to prepare a cost-effective additive via alkalization and etherification for Coal-water slurry (CWS). The degree of substitute (DS) and intrinsic viscosity of the prepared sodium carboxymethyl cellulose (SCMC1) were determined and its structure was also characterized by means of FT-IR and TGA, with another sample of SCMC2 produced from microcrystalline cellulose and a commercial SCMC3 as references. Results showed SCMC1 had a DS of 0.857 which was 32.7% and 44.7% higher than SCMC2 and SCMC3, respectively. The higher intrinsic viscosity of SCMC1 indicated it had a higher molecular mass. The SCMC samples were used as additives to prepare CWS of which the rheological behavior and static stability were measured to evaluate their applied performances. The data showed that CWS with SCMC1 had a lower apparent viscosity and higher static stability than others, which was due to the higher DS and higher molecular mass of SCMC1. For SCMC1 could provide stronger electrostatic repulsive forces and steric repulsive forces between the coal particles via adsorption. 相似文献
4.
You-Shao Wang Ai-Ping Yang Ge-Fei Zhou Xu-Fang Tan 《Journal of Radioanalytical and Nuclear Chemistry》2000,246(2):419-422
Five kinds of solid coordination complexes of uranium(VI) and thorium(IV) with the diamide (N,N,N,N-tetrabutylmalon-amide (TBMA), N,N,N,N-tetrabutylsuccinylamide (TBSA), N,N,N,N-tetrabutylglutaramide (TBGA), N,N,N,N-tetrabutyl-adipicamide (TBAA)) were synthesized. All these complexes of UO2(NO3)2·TBMA, UO2(NO3)2· TBSA, [UO2(NO3)2·(TBGA1/2)2]
x
, UO2(NO3)2·TBAA and Th(NO3)4·2TBMA were characterized by elemental analysis, UV spectra, IR spectra and 13C NMR spectra. The coordination form and proposed structures of the complexes are also discussed. 相似文献
5.
The determination of the two species of uranium(VI and IV) present in 6 uranium ores was studied in relation to the chemical and mineralogical composition, humidity, and pH of the samples taken over from the mine. X‐ray diffraction studies, performed on the uranium ores in powder form allowed to establish their mineralogical composition. Thechemical analysis pointed out the presence, besides the two uranium species, of some microelements able to influence the UVI/UIV ratio in minerals and to leach out UVI as uranyl ions from the corresponding minerals. 相似文献
6.
V. Brandel 《Journal of solid state chemistry》2005,178(4):1054-1063
A new uranium (IV) phosphate of proposed formula U2(PO4)2HPO4·H2O, i.e. uranium phosphate-hydrogenphosphate hydrate (UPHPH), was synthesized in autoclave and/or in polytetrafluoroethylene closed containers at 150 °C by three ways: from uranium (IV) hydrochloric solution and phosphoric acid, from uranium dioxide and phosphoric acid and by transformation of the uranium hydrogenphosphate hydrate U(HPO4)2·nH2O. The new product appears similar to the previously published thorium phosphate-hydrogenphosphate hydrate Th2(PO4)2HPO4·H2O (TPHPH). From preliminary studies, it was found that UPHPH crystallizes in monoclinic system (, , , β=91.67(3)° and ). Heated under inert atmosphere, this compound is decomposed above 400 °C into uranium phosphate-triphosphate U2(PO4)P3O10, uranium diphosphate α-UP2O7 and diuranium oxide phosphate U2O(PO4)2.Crystallized cerium (IV) phosphate-hydrogenphosphate hydrate Ce2(PO4)2HPO4·H2O (CePHPH) was also synthesized from (NH4)2Ce(NO3)6 and phosphoric acid solutions by the same method (monoclinic system: , , , β=91.98(1)° and ). When heating above 600 °C, cerium (IV) is reduced into Ce (III) and forms a mixture of CePO4 (monazite structure) and CeP3O9. 相似文献
7.
This paper reports a simple and highly selective method for the separation, preconcentration, and determination of trace amounts of thorium and uranium in some complex samples via staircase flotation. The method is based on the initial flotation of the Th(IV)‐arsenazo III complex in the presence of U(VI) from a solution of 5 mol dm?3 HCl, then reduction of U(VI) to U(IV) and repetition of the flotation step. In both steps, the floated complex was dissolved in a 5‐mL portion of methanol and its absorbance was measured at 655 nm, spectrophotometrically. For a 30‐mL portion of the sample, Beer's law was obeyed over the concentration ranges of 3.40 × 10?7to 3.06 × 10?6 mol dm?3 for Th(IV) and3.40 × 10?7 to 3.40 × 10?6 mol dm?3 for U(IV) with the apparent molar absorptivity of 4.20 × 105 dm3 mol?1 cm?1 and 3.59 × 105 dm3 mol?1 cm?1, respectively. The RSDs (n = 7) corresponding to 1.7 × 10?6 mol dm?3 of Th(IV) and U(IV) were obtained as 1.7% and 1.87%. The detection limits (7 blanks) for both the metal ions were found to be 1.7 × 10?7 mol dm?3. The important benefit of the method is that the determinations are free from the interference of almost all cations and anions found in the complex matrixes, such as seawater samples. The proposed method was also applied to reference materials, and the determinations were shown to have good agreement with the certified values. 相似文献
8.
本文报道了傅烷基磷酸钍的结构分析,证实了该材料具有类似于α-磷酸锆的层状结构;并将其应用于气相色谱固定相,较好地实现了硫醇类、含氯烃类及芳香烃类混合样品的分离。 相似文献
9.
Summary Thorium(IV) facilitates the reduction of bismuth(III)-ethylenediaminetetraacetate chelate in weakly acidic medium and gives a new wave at a more positive potential, because the EDTA anion liberated by the reduction will be caught immediately by thorium(IV) ion. The height of the substitution reduction wave is proportional to the concentration of thorium(IV) between 0.1 and 0.6 mM. Properties of the wave and the electrode process were investigated.
Tast-Polarographische Bestimmung von Thorium(IV) mit Hilfe der Substitutionsreduktion des Wismut(III)-Äthylendiamintetraacetat-Chelats
Zusammenfassung Thorium(IV) erleichtert die Reduktion des Wismut(III)-ÄDTE-Chelats in schwach sauerem Medium und gibt eine neue Welle bei positiverem Potential, da das durch die Reduktion freigesetzte ÄDTE-Anion vom Thorium(IV)-Ion sofort ergriffen wird. Die Höhe der Substitutionsreduktionswelle ist zwischen 0,1 und 0,6 mM der Thorium(IV)-Konzentration proportional. Eigenschaften der Welle und der Elektrodenvorgang wurden untersucht.相似文献
10.
Ahmed M. Donia Asem A. Atia Tarik E. Amer Mona N. El-Hazek Mohamed H. Ismael 《Journal of Dispersion Science and Technology》2013,34(11):1673-1681
A glycidyl methacrylate/divinylbenzene resin containing triethylenetetramine functional group was synthesized. The adsorption behavior of the obtained resin toward U(VI), Th(IV), and La(III) in aqueous solutions was investigated by batch and column techniques at different experimental conditions. Kinetic and thermodynamic characteristics of the adsorption process have been investigated. The regeneration of the loaded resin was also studied. 相似文献
11.
Complexes of uranium in its IV oxidation state, using cysteine, glycine, serine and aspartic acid as ligands, have been synthesized. Semi-microanalysis of the complexes indicate 1:1 metal to ligand ratio for all the synthesized complexes. Infrared spectra of solid complexes have been employed to establish the groups, coordinated to the metal ion. Effective magnetic moment of the complexes were also estimated. 相似文献
12.
Jeyakumar S Mishra VG Das MK Raut VV Sawant RM Ramakumar KL 《Journal of separation science》2011,34(6):609-616
The retention behavior of U and Th as their 2,6-pyridine dicarboxylic acid (PDCA) complexes on a cation exchange column was investigated under low pH conditions. Based on the observed retention characteristics, an ion chromatographic method for the rapid separation of uranium and thorium in isocratic elution mode using 0.08 mM PDCA and 0.24 M KNO(3) in 0.22 M HNO(3) as the eluent was developed. Both uranium and thorium were eluted as their PDCA complexes within 2 min, whereas the transition and lanthanide metal cations were eluted as an unresolved broad peak after thorium. Under the optimized conditions both U and Th have no interference either from alkali and alkaline earth elements up to a concentration ratio of 1:500 or from other elements up to 1:100. The detection limits (LOD) of U and Th were calculated as 0.04 and 0.06 ppm, respectively (S/N=3). The precision in the measurement of peak area of 0.5 ppm of both U and Th was better than 5% and a linear calibration in the concentration range of 0.25-25 ppm of U and Th was obtained. The method was successfully applied to determine U and Th in effluent water samples. 相似文献
13.
Xiao-qing Liu Fang Kong Jia-li Liao Song-dong Ding Yuan-you Yang Huang Huang Shun-zhong Luo Guo-ping Liu Xing-liang Li Ji-jun Yang Jun Tang Ning Liu 《Journal of Radioanalytical and Nuclear Chemistry》2014,302(3):1069-1076
The extraction kinetics of uranium(VI) and thorium(IV) with Tri-iso-amyl phosphate (TiAP) from nitric acid medium has been investigated using a Lewis Cell. Especially, dependences of the extraction rate on stirring speed, temperature, interfacial area were firstly measured to elucidate the extraction kinetics regimes. The experimental results demonstrated that extraction kinetic of U(VI) is governed by chemical reactions at interface with an activation energy, Ea, of 43.41 kJ/mol, while the rate of Th(IV) extraction is proved to be intermediate controlled, of which the Ea is 23.20 kJ/mol. Reaction orders with respect to the influencing parameters of the extraction rate are determined, and the rate equations of U(VI) and Th(IV) at 293 K have been proposed as $$ {\text{r}} = - {\text{dcUO}}_{ 2} \left( {{\text{NO}}_{ 3} } \right)_{ 2} /{\text{dt}} = 1. 80 \times 10^{ - 3} \left[ {{\text{UO}}_{ 2} \left( {{\text{NO}}_{ 3} } \right)_{ 2} } \right]^{ 1.0 1} \left[ {\text{TiAP}} \right]^{0. 5 5} , $$ $$ {\text{r}} = - {\text{dcTh }}\left( {{\text{NO}}_{ 3} } \right)_{ 4} /{\text{dt}} = 1. 8 8\times 10^{ - 3} \left[ {{\text{Th }}\left( {{\text{NO}}_{ 3} } \right)_{ 4} } \right]^{ 1.0 4} \left[ {\text{TiAP}} \right]^{ 1. 7 7} \left[ {{\text{HNO}}_{ 3} } \right]^{0. 3 8} , $$ respectively. 相似文献
14.
New tri-functional ligands of the type R2NCOCH2SCH2CONR2 (where R = iso-propyl, n-butyl or iso-butyl) were prepared and characterized. The coordination chemistry of these ligands with uranyl and lanthanum(III) nitrates was studied by using the IR, 1HNMR and elemental analysis methods. Structures for the compounds [UO2(NO3)2(iPr2NCOCH2SCH2CONiPr2)] [UO2(NO3)2(iBu2NCOCH2SCH2CONiBu2)], [La(NO3)3(iPr2NCOCH2SCH2CONiPr2)2] and [La(NO3)3(iBu2NCOCH2SCH2CONiBu2)2] were determined by single crystal X-ray diffraction. These structures show that the ligand acts as a bidentate chelating ligand and bonds through both the carbamoyl groups to the uranyl and lanthanum(III) nitrate groups. Solvent extraction studies show that the ligand can extract the uranyl ion from the nitric acid medium but does not show any ability to extract the americium (III) ion. 相似文献
15.
G. M. Hussein Nabawia A. Gomaa Mohamed R. Shehata Wafaa M. Hosny 《Journal of Dispersion Science and Technology》2017,38(8):1204-1210
In the present study, the use of 5% Aliquat-336/kerosene was evaluated in the liquid–liquid extraction of Uranium(VI) and some impurities of Thorium(IV) and rare earth elements (REEs(III)). Experiments were carried out to determine the factors affecting U(VI) and some impurities of Th(IV) and REEs(III) extraction. McCabe–Thiele diagram was constructed to define the theoretical stages for extraction mixer settler process. The effect of stripping factors from the loaded extractant was also tested. Uranium cake was finally obtained from the strip solution and a workable flow sheet was then formulated. 相似文献
16.
Poly(acrylamidoxime-co-2-acrylamido-2-methylpropane sulfonic acid) (PAMSA) hydrogel was prepared by copolymerization of acrylonitrile and 2-acrylamido-2-methylpropane sulfonic acid as monomer, N,N′-methylenebis(acrylamide) as crosslinking agent and potassium peroxodisulfate as initiator. Amidoximated copolymer network was prepared by the reaction of copolymer network with hydroxylamine hydrochloride. A batch procedure was used for the determination of the characteristics of the U(VI) solid phase extraction from the amidoximated hydrogel. The determination of U(VI) was performed by spectrophotometric method using arsenazo-III as complexing agent. Optimal pH value for the quantitative preconcentration was 3, and full desorption was achieved with 3 mol L−1 HClO4. The adsorption process can be well described by the pseudo-second-order kinetic model, and the equilibrium adsorption isotherm was closely fitted with the Langmuir model. A preconcentration factor of 20 and the three sigma detection limit of 2.8 μg L−1 (n = 20) were achieved for uranium(VI) ions. The PAMSA hydrogel was used for separating and preconcentrating the uranyl ion existing in sea water samples, thermal spring water samples and the certified reference materials (TMDA 64; fortified lake water sample). 相似文献
17.
Benedicte Chapelet-Arab Guy Nowogrocki Stephane Grandjean 《Journal of solid state chemistry》2005,178(10):3046-3054
A new ammonium uranium (IV) oxalate (NH4)2U2(C2O4)5·0.7H2O (1) and three mixed uranium (IV)-lanthanide (III) oxalates, (N2H5)2.6U1.4M0.6(C2O4)5·xH2O (M=Nd (2) and M=Sm (3)), Na2.56U1.44Nd0.56(C2O4)5·7.6H2O (4) and Na3UCe(C2O4)5·10.4H2O (5), have been prepared. The crystal structures of compounds 1, 4 and 5 have been determined by single-crystal X-ray diffraction. The crystal structures were solved by the direct methods and Fourier difference techniques, and refined by a least square method on the basis of F2 for all unique reflections. Compounds 2 and 3 are isotypic with 1. Crystallographic data: 1, hexagonal, space group P63/mmc, a=19.177(3), c=12.728(4) Å, Z=6, R1=0.0575 for 52 parameters with 1360 reflections with I?2σ(I); 2, hexagonal, space group P63/mmc, a=19.243(4), c=12.760(5) Å, Z=6; 3, hexagonal, space group P63/mmc, a=19.211(3), c=12.274(4) Å, Z=6; 4, orthorhombic, space group Pbcn, a=18.79(3), b=11.46(1), c=12.77(2) Å, Z=4, R1=0.0511 for 183 parameters with 3026 reflections with I?2σ(I); 5, monoclinic, space group C2/c, a=18.878(6), b=11.684(4), c=12.932(4) Å, β=95.97(1)°, Z=4, R1=0.0416 for 213 parameters with 4060 reflections with I?2σ(I). The honeycomb-like structure of the five compounds is built from the same three-dimensional arrangement of metallic and oxalate ions. Similar hexagonal rings of alternating metallic and oxalate ions form layers parallel to the (001) plane that are pillared by another oxalate ion. Indeed, some torsions or rotations of the bridging oxalate ligands led to modifications of the network symmetry. The monovalent cations and the water molecules occupy the hexagonal tunnels running down the [001] direction. Starting from the uranium (IV) compound A2U2(C2O4)5·0.7H2O with A=NH4+ (1), the mixed U(IV)/Ln(III) oxalates are obtained by partial substitution of U(IV) by Ln(III) in a ten-coordinated site, the charge deficit being compensated by intercalation of supplementary monovalent ions within the tunnels. The distortion of the arrangement in the [001] direction for the Na-containing compounds allows the accommodation of a greater number of water molecules that insure an octahedral coordination of the Na atoms. 相似文献
18.
Uranium extraction using DEHCNPB (butyl-1-[N,N-bis(2-ethylhexyl)carbamoyl]nonyl phosphonic acid, a bifunctional cationic extractant) has been studied to better understand mechanism differences depending on the original acidic solution (phosphoric or sulfuric). Solvent extraction batch experiments were carried out and the organic phases were probed using 31P-NMR. This technique enabled to demonstrate that phosphoric acid is poorly extracted by DEHCNPB ([H3PO4]org < 2mM), using direct quantification in the organic phase by 31P-NMR spectra integration. Moreover, in the presence of uranium in the initial phosphoric acid solution, uranyl extraction by DEHCNPB competes with H3PO4 extraction.Average stoichiometries of U(VI)-DEHCNPB complexes in organic phases were also determined using slope analysis on uranium distribution data. Uranium seems to be extracted from a phosphoric medium by two extractant molecules, whereas more than three DEHCNPB on average would be necessary to extract uranium from a sulfuric medium. Thus, uranium is extracted according to different mechanisms depending on the nature of the initial solution. 相似文献
19.
《Journal of Saudi Chemical Society》2020,24(6):451-460
The present work describes the synthesis and characterization of thorium (IV) and dioxouranium (VI) coordination compounds with three Schiff bases derived from 1-furfurylaldehyde. All coordination compounds were characterized by elemental analysis, ultraviolet–visible spectroscopy, Fourier transform infrared spectroscopy, fluorescence spectroscopy, and thermal analysis. The structural pattern, the geometry of the complexes and the coordination number of the metal ions were assigned on the basis of physico-chemical parameters, such as FTIR and UV–Vis spectra. The elemental analyses show a 1:1 stoichiometry for thorium coordinative compounds and 1:2 stoichiometry for uranyl ion, respectively. The obtained coordination compounds are stable in air, soluble in some organic solvents (DMF, acetonitrile, DMSO) and show fluorescent properties. The coordination compounds have high molar conductance that indicates their electrolytes nature. On the basis of the obtained experimental results, combined with theoretical studies, the structures of the compounds under study were proposed. 相似文献