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Publications (64)
Oxidation behaviour of (U1−yGdy)O2.00; (y = 0.05, 0.10, 0.15 and 0.20) was examined under controlled oxygen partial pressures ranging from 101.3 to 0.2 kPa. Stoichiometric gadolinium (Gd3+)-doped UO2 was synthesized by a gel combustion method followed by reduction at 1673 K in Ar–8%H2 atmosphere. Thermogravimetry (TG) measurements of (U1−yGdy)O2.00...
Thermo physical properties of potassium, rubidium and cesium thorium phosphate compounds were investigated. All compounds were synthesized by conventional solid state method. Formation of orthorhombic AMThP3O10, tetragonal AM2Th(PO4)2 and monoclinic AMTh2(PO4)3; [AM=K, Rb and Cs] was confirmed using Powder X‐ray diffraction (XRD) technique. Structu...
Sub solidus phase relations in pseudo ternary SrO–La2O3–P2O5 system were determined experimentally at 1523 K in air. To confirm the formation of phases at this temperature, ternary and quaternary compounds in SrO–P2O5, SrO–La2O3, La2O3–P2O5 and SrO–La2O3–P2O5 systems were synthesized by solid state route. Powder X-ray diffraction (XRD) technique wa...
The title complex [PdCl(L)] (1), is obtained from the reaction of SCS pincer ligand HL (where, HL = N,N'-di-tert-butylbenzene-1,3-dicarbothioamide) with lithium tetrachloropalladate (II) in methanol. The compound 1 is characterized by elemental analysis, FTIR, ¹H, and ¹³C-NMR spectroscopy, UV-Vis spectroscopy, powder X-ray diffraction and X-ray cry...
A series of compositions covering the complete range in SrTh(PO4)2–SrU(PO4)2 system were synthesized by conventional solid state (dry) route at 1473 K in argon atmosphere. The products were examined by powder X-ray diffraction (XRD) technique. X-ray diffraction (XRD) patterns of thorium rich Sr(Th1-xUx)(PO4)2 with compositions x ≤ 0.15 showed chera...
In this study the coordination chemistry of three ligands, C5H4NOCONRR’ (where, R, R’ = ⁱC3H7 (L1); R, R’ = ⁱC4H9 (L2); and R = H, R’ = tC4H9 (L3) composed of N-oxide and carboxamide groups have been explored with uranyl nitrate and some selected lanthanide (La, Sm, and Eu) nitrates. All the synthesized ligands as well as their complexes (1-12) of...
Synthesis, X-ray, chemical analysis and thermal properties of Nd doped (U, Th)O2 mixed oxides of the formula [(U0.3Th0.7)1-yNdy]O2+x; (Where y = 0–0.4) are reported in this work. The Nd doped mixed (U, Th)O2 oxides were synthesized using gel combustion method followed by heating the precursors at 1673 K in reduced atmosphere. Powder X-ray Diffracti...
Structure of monoclinic CaU(PO4)2, synthesized in argon atmosphere at 1473 K, was derived from powder X−ray diffraction (XRD) data using Rietveld refinement method. Thermogravimetric (TG) Curve recorded up to 1573 K in argon atmosphere showed thermal as well as structural stability of CaU(PO4)2. When heated in air, TG curve of CaU(PO4)2 showed weig...
Electrochemical investigations and extraction of Pu(IV) was investigated employing a new bifunctional ligand system (N,N-dialkyl carbamoyl methyl) (2-pyridyl-N-Oxide) sulfide C5H4NOSCH2CONR2, (where R = octyl) (NOSCO) dissolved in 1-butyl-3-methylimidazolium bis (trifluoromethanesulphonyl) imide ([Bmim][NTf2]). The extraction efficiency was found t...
For the first time, oxidation behavior of (U1-yCey)O2.00; (y = 0.21, 0.28 and 0.44) was examined under various oxygen potentials ranging from 0 to −58 kJ/mol. Thermogravimetry (TG) and powder X-ray powder diffraction (XRD) were used as prime techniques for determination of oxygen stoichiometry and identification of different compounds formed. Rietv...
A new approach for the extraction of plutonium and americium from aqueous media containing complexing ligands has been investigated using a new extractant N,N′-dioctyl-α-hydroxy acetamide. Studies have been carried out on the extraction of Am(III) and Pu(IV) by this extractant from media containing complexing ligands such as PO4³⁻, C2O4²⁻ and F⁻ wh...
X-ray diffraction, chemical and thermal studies of [(U0.2Th0.8)1-yLay]O2+x (LUTL) and [(U0.3Th0.7)1-yLay]O2+x (UTL); compounds (where y ≤ 0.4) were carried out. These compounds were synthesized by gel combustion method followed by heating in reduced atmospheres at 1673 K. To co-relate lattice parameters with metal and oxygen concentrations, reduced...
A new bifunctional ligand system (N, N-dialkyl carbamoyl methyl) (2-pyridyl-N-Oxide) sulfide C5H4NOSCH2CONR2, (where R = isopropyl (L1), isobutyl (L2) and butyl (L3) and octyl (L4)) have been synthesized. The coordination chemistry of this ligand system with UO2(NO3)2.6H2O has been carried out. All the ligands and complexes were characterized by CH...
Compounds SrU(PO4)2 (SUP) and BaU(PO4)2 (BUP) were synthesized by solid state method in high purity argon atmosphere at 1473 K. Structures of both the compounds were derived using Rietveld method from powder X–ray diffraction (XRD) data. Compound SUP is orthorhombic and has ordered cheralite type structure with alternate layers of SrO10 and UO8 pol...
The sub–solidus phase relations in BaBiVO quaternary system were determined at 1123 K in air. To confirm the formation and stability of reported phases at this temperature, ternary and quaternary compounds in BaOBi2O3, Bi2O3V2O5, BaOV2O5 and BaOBi2O3V2O5 systems were synthesized by solid state route. BaCO3, Bi2O3 and NH4VO3 were reacted in desired...
The separation of different metal ions can be successfully accomplished by using picolinamide-based ligands. We herein report the first X-ray structure of picolinamide-based ligands of the type C5H4NCONR2 (where R = ⁱC3H7 (L1) and ⁱC4H9 (L2)) and C5H4NCONHR (R = tC4H9 (L3)) with palladium(II) ion. We have synthesized and characterized the structure...
Sr7U(PO4)6 (I) and Ba7U(PO4)6 (II) are prepared by solid state reaction of stoichiometric amounts of SrCO3 or BaCO3, UO2, and NH4H2PO4 under Ar (1.
The crystal structure of Sr2WO5 has been refined using powder X-Ray diffraction (XRD) and neutron diffraction (ND) data. The corner connected WO6 octahedra forms infinite cis-bridged chains along b axis which are further connected by the layer of Sr atoms to give a three dimensional network. Thermogravimetric study revealed that Sr2WO5 on storage p...
Compounds Sr7U(PO4)6 (1) and Ba7U(PO4)6 (2) were prepared by the solid state reaction route, by mixing appropriate molar proportions of alkaline earth metal carbonates (Sr and Ba), UO2 and NH4H2PO4 (ADHP) and heating in high purity Ar atmosphere at 1373 K for 10 h with intermittent grinding. Powder X-ray Diffraction (XRD) was done to ascertain the...
Thermal stability and expansion behavior of ThW2O8 and UWO6 were studied using thermogravimetry and high-temperature X-ray diffraction techniques. ThW2O8 and UWO6 showed positive thermal expansion in vacuum from ambient to 1273 and 1073 K, respectively. Heat capacity for ThW2O8(s) and UWO6(s) was measured in argon atmosphere using heat flux-type di...
Four novel rubidium uranium (IV) molybdate compounds, Rb4U5(MoO4)12, Rb2U(MoO4)3, Rb4U(MoO4)4 and Rb8U(MoO4)6 have been prepared by solid state route, reacting Rb2MoO4, UMoO5 and MoO3 in desired molar proportions in evacuated sealed quartz ampoules at 823 K and characterized by powder X-ray diffraction (XRD) and thermal analysis techniques. Thermal...
Th (MO4)2: Eu3+ (M = Mo, W) phosphor materials have been synthesized via high temperature solid state route and characterized systematically using by X-ray diffraction (XRD) and photoluminescence (PL) spectroscopy. X-ray diffraction data of Th(WO4)2 and Th(Mo1−xWxO4)2 were refined and structures were derived for the first time using Th(MoO4)2 as an...
Phase relations and defect structures in (U0.2Th0.8)O2-DyO1.5 quaternary system were studied at 1673 K by heating the oxides in different atmospheres. Lattice parameter and O/U of the mixed oxides were determined from X-ray diffraction (XRD) and chemical analysis, respectively. The cubic lattice parameter of [(U0.2Th0.8)1−yDyy]O2+x; (0 ≤ y ≤ 0.37)...
Uranyl complexes containing diphenyl(2-pyridyl)phosphine oxide, with the formulae [UO2(NO3)2({C6H5}2POC5H4N)2] (1) and [UO2(DBM)2({C6H5}2POC5H4N)] (2) (where DBM = C6H5COCHCOC6H5), were prepared and characterized by IR, NMR spectroscopic and elemental analysis methods. The structures of the compounds were determined by X-ray diffraction methods and...
The complex chemistry of piperidine based amide ligands with uranyl chloride, bromide, nitrate and β-diketonates shows that the ligands bond through the amido oxygen atom to the uranyl group. The structures of the uranyl halides, nitrate and bis(β-diketonates) show octahedral, hexagonal bipyramidal and pentagonal bipyramidal geometries around the u...
Dithio-diglycolamide ligands of the types [(CH2SCH2CONR2)(2)] (where R = (C3H7)-C-1, C4H9, (C4H9)-C-i, C8H17) and [C7H6(SCH2CONR2)(2)] (where R = (C4H9)-C-i) were prepared and characterized. The complex chemistry of these ligands with uranyl nitrate was studied using IR, NMR and ESI-MS techniques and elemental analysis. The structures for two of th...
A monoamide, N,N'-dioctyl, α-hydroxy acetamide, shows unusual extraction properties towards trivalent lanthanide and actinide ions above 3 M HNO3. The extracted ions could be quantitatively back extracted using 0.5 M HNO3. This amide shows negligible extraction towards Sr(ii) and Ru(iii) ions, making it advantageous over other reported extractants....
A new compound BiCrTeO6 in Bi–Cr–Te–O system was prepared by solid state reaction of Bi2O3, Cr2O3 and H6TeO6 in oxygen and characterized by X-ray diffraction (XRD) method. It could be indexed on a trigonal lattice, with the space group P-31c, unit cell parameters a = 5.16268(7) Å and c = 9.91861(17) Å. The crystal structure of BiCrTeO6 was determin...
In Cs–Mo–O system, Cs2MonO3n+1 (n = 1, 3, 5 and 7) were prepared by solid state route and n = 7 was established as the highest stable analog. Differential thermal analysis of the compound Cs2MoO4 (n = 1) in air showed a reversible phase transition followed by melting whereas compounds with n = 3, 5 and 7 did not show any phase transition up to thei...
Carbamoyl pyrazole compounds of palladium(II) chloride of the type [PdCl2L2] (where L = C3H3N2CONR2 or C5H7N2CONR2; R = CH3, C2H5 or iC3H7) have been synthesized and characterized by IR, 1H NMR, ES-MS, elemental analysis and single crystal X-ray diffraction methods. The centrosymmetric structure of [PdCl2(C3H3N2CON{C2H5}2)2] (2) shows that the pall...
Na4(ThxU1-x)(MoO4)4(x = 0.5,0.8) type
of compounds were synthesized by reacting
(ThxU1-x)(MoO4)2 and Na2MoO4
in appropriate molar ratio at 873 K in an evacuated quartz ampoule for
25 h. The crystal structure of
Na4(ThxU1-x)(MoO4)4 was refined from
X-ray powder diffraction data in the tetragonal system (space group:
I41/a) by Rietveld method and has...
A new phase Pu(VO3)4 in PuO2–V2O5 system was prepared by heating an appropriate amount of pre-dried PuO2 and V2O5 at 640 °C. The structural and thermal properties of Pu(VO3)4 were investigated by powder X-ray diffraction and thermogravimetry (TG). Structural analyses revealed that Pu(VO3)4 crystallizes in tetragonal (space group: I41/a) lattice wit...
New bifunctional pyrazole based ligands of the type [C(3)HR(2)N(2)CONR'] (where R = H or CH(3); R' = CH(3), C(2)H(5), or (i)C(3)H(7)) were prepared and characterized. The coordination chemistry of these ligands with uranyl nitrate and uranyl bis(dibenzoyl methanate) was studied with infrared (IR), (1)H NMR, electrospray-mass spectrometry (ES-MS), e...
A 1,1′ bis(diphenyl phosphino ferrocene) dioxide complex of the uranyl dichloride was synthesized and characterized by elemental analysis, 1H, 31P{1H} NMR and X-ray diffraction methods. The structure of the compound shows that the uranium(VI) ion is surrounded by four oxygen and two chlorine atoms in an octahedral geometry. Two oxygen atoms from th...
Thermal expansion behavior of U2MoO8, β-UMo2O8, UMo5O16, UMo7O22 and UMo10O32 was studied in vacuum between 298 K and 873 K using high temperature X-ray diffractometer. The compounds were synthesized by solid state route, reacting UO2, MoO2 and/or MoO3 in required molar proportions in sealed evacuated quartz ampoules at desired temperatures. Studie...
The sub-solidus phase relations in Sr–Th–P–O quaternary system were determined at 1223K in air. To confirm the formation and stability of reported phases, ternary and quaternary compounds in Sr–Th–O, Sr–P–O, Th–P–O and Sr–Th–P–O systems were synthesized by solid state reactions of SrCO3, ThO2 and NH4H2PO4 in desired molar proportions at 1223K. A ps...
A new tri-functional ligand iBu2NCOCH2SO2CH2CONiBu2 (L) was prepared and characterized. The coordination chemistry of this ligand with uranyl nitrate was studied with IR, 1HNMR, ES-MS, TG and elemental analysis methods. The structure of the compound [UO2(NO3)2L] was determined by single crystal X-ray diffraction techniques. In the structure the ura...
A new tri-functional ligand iBu2NCOCH2SOCH2CONiBu2 was prepared and characterized. The coordination chemistry of this ligand with uranyl nitrate was studied with IR, 1H NMR, electrospray mass–spectrometry, thermogravimetry, and elemental analysis. The structure of [UO2(NO3)2(iBu2NCOCH2SOCH2CONiBu2)] was determined by single-crystal X-ray diffractio...
A 1,1′ bis(diphenylphosphino ferrocene)dioxide complex of uranyl nitrate was synthesized and characterized by IR, 1H and 31P{1H} NMR spectroscopic and X-ray diffraction methods. The structure of the compound shows that the uranium atom is surrounded by eight oxygen atoms in a hexagonal bi-pyramidal geometry. Two oxygen atoms from 1,1′ bis(diphenylp...
The extraction behavior of new bi-functional ligands containing sulfoxide and amide groups viz. N,N'-dibutyl carbamoyl methyl phenyl sulfoxide (L1) and N,N'-dibutyl carbamoyl methyl benzyl sulfoxide (L2) towards the U(VI), Pu(IV) and Am(III) ions from nitric acid was studied. Both of these extractants showed appreciable extractions for U(VI) and Pu...
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)] [U...
The crystal structures for two of the ligands C6H5CH2SOCH2CONHCH2C6H5 (1) and C6H5SOCH2CON(iC3H7)2 (2) have been determined by X-ray diffraction. These compounds crystallize in orthorhombic system with space groups and cell parameters, Pca21(no. 29), a = 8.4600(5) Å, b = 5.3534(5) Å, c = 32.136(2) Å, V = 1455.42(15) Å3 and Pna21(no. 33) a = 17.5563...
The coordination chemistry of iso-butyramide based ligands such as: iC3H7CON(iC3H7)2, iC3H7CON(C4H9)2 and iC3H7CON(iC4H9)2 with [UO2(NO3)2·6H2O], [UO2(OO)2·2H2O] {where OO=C4H3SCOCHCOCF3 (TTA), C6H5COCHCOCF3 (BTA) and C6H5COCHCOC6H5 (DBM)}, [Th(NO3)4·6H2O] and [La(NO3)3·6H2O] has been evaluated. Structures for the compounds [UO2(NO3)2(iC3H7CON{iC4H...
In continuation with the earlier work for phase studies of Rb–Sr–U–O and Cs–Sr–U–O systems, the subsolidus phase relations in Na–Sr–U–O quaternary system were determined at 850 °C in air atmosphere. A novel quaternary phase Na8Sr2U6O24 in the Na–Sr–U–O system was synthesized by heating the respective oxides at 850 °C in air. XRD data of Na8Sr2U6O24...
The bi-functional carbamoyl methyl pyrazole ligands, C5H7N2CH2CONBu2 (L1), C5H7N2CH2CONiBu2 (L2), C3H3N2CH2CONBu2 (L3), C3H3N2CH2CONiBu2 (L4) and C5H7N2CH2CON(C8H17)2 (L5) were synthesized and characterized by spectroscopic and elemental analysis methods. The selected coordination chemistry of L1 to L4 with [UO2(NO3)2·6H2O], [La(NO3)3·6H2O] and [Ce...
Carbamoyl methyl pyrazole compound of palladium(II) chloride of the type [PdCl2L2] (where L = C5H7N2CH2CON(C4 H9)2, C5H7N2CH2CON(i C4H9)2, C3H3N2CH2CON(C4 H9)2, or C3H3N2CH2CON(i C4H9)2) has been synthesized and characterized by IR and 1H NMR spectroscopy. The structure of the compound [PdCl2{C3H3N2CH2C ONiBu2}2] has been determined by single cryst...
The carbamoyl methyl sulfoxide compounds of uranyl bis(β-diketonate) of the types [UO2(DBM)2CMSO] and [{UO2(DBM)2}2CMSO] (where HDBM=C6H5COCH2COC6H5; CMSO=C6H5CH2SOCH2CONHC6H5 or C6H5SOCH2CONiPr2) have been synthesized and characterized by IR and NMR spectroscopic techniques and elemental analysis. Spectral studies show that CMSO acts as a monodent...
The bifunctional carbamoyl methyl sulfoxide ligands, PhCH(2)SOCH(2)CONHPh (L1), PhCH(2)SOCH(2)CONHCH(2)Ph (L2), PhSOCH(2)CON(i)Pr(2)(L3), PhSOCH(2)CONBu(2)(L4), PhSOCH(2)CON(i)Bu(2)(L5) and PhSOCH(2)CON(C(8)H(17))(2)(L6) have been synthesized and characterized by spectroscopic methods. The selected coordination chemistry of L1, L3, and L5with [UO(2...
In the title compound, [UO2(C15H9O2)2(C17H18O)] or [UO2(DBM)2(DBA)], where DBM is dibenzoyl methanate and DBA is dibenzylacetone, the UVI atom is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry. The diphenylpropane-1,3-dionate system acts as a chelating ligand and coordinates through both of its ketonate O atoms, wh...
In the title compound, [UO2(C15H9O2)2(C17H18O)] or [UO2(DBM)2(DBA)], where DBM is dibenzoyl methanate and DBA is dibenzylacetone, the UVI atom is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry. The diphenylpropane-1,3-dionate system acts as a chelating ligand and coordinates through both of its ketonate O atoms, wh...
Bis(diphenylphosphino)methane dioxide compounds of uranyl nitrate and uranyl bis(β-diketonates) have been synthesized and characterized by spectroscopic and X-ray diffraction methods. Monodentate, bidentate chelate and bridging bidentate modes of coordination for this ligand have been established from the single-crystal X-ray diffraction studies of...
The X-ray structure of the compound [{UO2(DBM)2}2C6H5SOCH2SOC6H5 ] confirms the bridging bidentate mode of coordination for the β-disulfoxide ligand C6H5SOCH2SOC6H5.
The X-ray structure of the compound [{UO2(DBM)2}2C6H5SOCH2SOC6H5 ] confirms the bridging bidentate mode of coordination for the β-disulfoxide ligand C6H5SOCH2SOC6H5.
The first structurally characterised uranyl bis (β-diketonate)-amide adduct compound [ UO2(DBM)2. C4H9CON (3-C5H11) (sec-C4H9) ] (DBM = dibenzoylmethanate) shows that the amide ligand bonded through its amido oxygen atom to the uranyl group. The average bond distances for U-O(uranyl) , U-O(DBM) and U-O(amide) are 1.778(5), 2.346(5) and 2.411(5)Å re...
In the title compound, [UO2(C15H11O2)2(C18H15OP)] or [UO2(DBM)2(Ph3PO)], where DBM is dibenzoyl methanate, the UVI atom is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry. The diphenylpropane-1,3-dionate system acts as a chelating ligand and coordinates through both of its ketonate O atoms and the triphenyl phosphine...
In the title compound, [UO2(C15H11O2)2(C18H15OP)] or [UO2(DBM)2(Ph3PO)], where DBM is dibenzoyl methanate, the UVI atom is coordinated by seven O atoms in a distorted pentagonal–bipyramidal geometry. The diphenylpropane-1,3-dionate system acts as a chelating ligand and coordinates through both of its ketonate O atoms and the triphenyl phosphine...
N-oxide compounds of the type [UO2(OO)2·L] (OO=TTA, DBM, BA or BTA; L=C6H5CHN(O)C6H5 (L1), C6H5CHN(O)C6H4·CH3-p) (L2) or p-NO2C5H4NO) have been prepared and characterized by IR, 1H and 19F NMR spectroscopic and elemental analyses methods. Spectral studies show that the N-oxide ligands coordinate through its nitroxyl oxygen atom to the uranyl gro...
The U atom in the title compound, [UO2(PhCOCHCOPh)2(H2O)]·C14H20O5, is surrounded by seven O atoms at the vertices of a distorted pentagonal bipyramid. The crown ether molecule is not coordinated directly to the U atom, but is linked to the aquabis(dibenzoylmethanato)dioxouranium complex via hydrogen bonds involving the water molecule. The U...
Reaction of [UO2(TTA)22H2O] with benzo-15,crown-5 in chloroform yielded the compound [UO2(TTA)2H2O]2(benzo-15,crown-5) (1) in which the benzo-15,crown-5 ether acts as a second sphere ligand. However, similar reaction with dibenzo-18,crown-6 yielded the compound [UO2(TTA)2(μ-H2O)]2(H2O)2(dibenzo-18,crown-6) (2) in which the dibenzo-18,crown-6 ether...