(Solid + liquid) phase equilibria of (Ca(H2PO2)2 + CaCl2 + H2O) and (Ca(H2PO2)2 + NaH2PO2 + H2O) ternary systems at T = 323.15 K

International Nuclear Information System (INIS)

Cao, Hong-yu; Zhou, Huan; Bai, Xiao-qin; Ma, Ruo-xin; Tan, Li-na; Wang, Jun-min

2016-01-01

Graphical abstract: Solubility diagram of the (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) system at T = (323.15 and 298.15) K. - Highlights: • Phase diagrams of Ca 2+ -H 2 PO 2 − -Cl − -H 2 O, Ca 2+ -Na + -H 2 PO 2 − -H 2 O at 323.15 K were obtained. • Incompatible double salt of NaCa(H 2 PO 2 ) 3 in Ca 2+ -Na + -H 2 PO 2 − -H 2 O system was determined. • Density diagram of the corresponding liquid were simultaneously measured. - Abstract: Calcium hypophosphite has been widely used as an anti-corrosive agent, flame retardant, fertilizer, assistant for Ni electroless plating, and animal nutritional supplement. High purity calcium hypophosphite can be synthesized via the replacement reaction of sodium hypophosphite and calcium chloride. In this work, the (solid + liquid) phase equilibria of (Ca(H 2 PO 2 ) 2 + CaCl 2 + H 2 O) and (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) ternary systems at T = 323.15 K were studied experimentally via the classical isothermal solubility equilibrium method, and the phase diagrams for these two systems were obtained. It was found that two solid salts of CaCl 2 ·2H 2 O and Ca(H 2 PO 2 ) 2 exist in the (Ca(H 2 PO 2 ) 2 + CaCl 2 + H 2 O) system, and three salts of Ca(H 2 PO 2 ) 2 , NaH 2 PO 2 ·H 2 O and one incompatible double salt, NaCa(H 2 PO 2 ) 3 occur in the (Ca(H 2 PO 2 ) 2 + NaH 2 PO 2 + H 2 O) system.

Structure of LaH(PO3H)2.3H2O

International Nuclear Information System (INIS)

Loukili, M.; Durand, J.; Larbot, A.; Cot, L.; Rafiq, M.

1991-01-01

Lanthanum hydrogen bis(hydrogenphosphite) trihydrate, LaH(Po 3 H) 2 .3H 2 O, M r =353.8, monoclinic, P2 1 /c, a=9.687 (3), b=7.138 (2), c=13.518 A, β=104.48 (3) deg, V=905.0 (5) A 3 , Z=4, D m =2.56 (2), D x =2.598 Mg m -3 , λ(MoKα)=0.71073 A, μ(MoKα)=5.103 mm -1 , F(000)=672, T=300 K, R=0.032 for 1018 independent observed reflections. The structure contains two phosphite anions connected by a hydrogen bond. The La 3+ cation is eight coordinated by seven O atoms from phosphite anions and one O atom of a water molecule. (orig.)

Synthesis and crystal structure of acid indium phosphite In(H3PO3)3

International Nuclear Information System (INIS)

Zakharova, B.S.; Chudinova, N.N.; Ilyhkhin, A.B.

1996-01-01

A group of isostructural acid phosphites of trivalent metals M(H 2 PO 3 ) 3 , where M 3 =V, Fe, Ga, In, was synthesized. Crystal structure of In(H 2 PO 3 ) 3 was determined. The compound crystallizes in hexagonal syngony, a = 8.414(2), c = 7.069(2) A, V = 433.3(2) A 3 , Z = 2, sp.gr. P6 3 . In (H 2 PO 3 ) 3 structure is of frame type. 9 refs.; 3 tabs

Synthesis, crystal structures, and luminescent properties of two series' of new lanthanide (III) amino-carboxylate-phosphonates.

Science.gov (United States)

Zhou, Tian-Hua; Yi, Fei-Yan; Li, Pei-Xin; Mao, Jiang-Gao

2010-02-01

Hydrothermal reactions of lanthanide(III) chlorides with 4-HOOC-C(6)H(4)-CH(2)NHCH(2)PO(3)H(2) (H(3)L) at different ligand-to-metal (L/M) ratios afforded nine new lanthanide(III) carboxylate-phosphonates with two types of 3D network structures, namely, LnCl(HL)(H(2)O)(2) (Ln = Sm, 1; Eu, 2; Gd, 3; Tb, 4; Dy, 5; Er, 6) and [Ln(2)(HL)(H(2)L)(L)(H(2)O)(2)].4H(2)O (Ln = Nd, 7; Sm, 8; Eu, 9). Compounds 1-6 are isostructural and feature a 3D network in which the LnO(7)Cl polyhedra are interconnected by bridging CPO(3) tetrahedra into 2D inorganic layers parallel to the bc plane. These layers are further cross-linked by organic groups of the carboxylate-phosphonate ligands via the coordination of the carboxylate groups into a pillared-layered architecture. Compounds 7-9 are also isostructural and feature a 3D open-framework composed of 1D lanthanide(III) phosphonate inorganic slabs which are further bridged by organic groups of the carboxylate-phosphonate liagnds via the coordination of the carboxylate groups, forming large 1D tunnels along the b-axis which are filled by lattice water molecules. Luminescent measurements indicate that compounds 2, 4, and 5 show strong emission bands in red, green, and yellow light region, respectively. Magnetic properties of 2, 3, 5, and 7 have also been studied.

[H3N(CH2)4NH3]2[Al4(C2O4)(H2PO4)2(PO4)4].4[H2O]: A new layered aluminum phosphate-oxalate

International Nuclear Information System (INIS)

Peng Li; Li Jiyang; Yu Jihong; Li Guanghua; Fang Qianrong; Xu Ruren

2005-01-01

A new layered inorganic-organic hybrid aluminum phosphate-oxalate [H 3 N(CH 2 ) 4 NH 3 ] 2 [Al 4 (C 2 O 4 )(H 2 PO 4 ) 2 (PO 4 ) 4 ].4[H 2 O](AlPO-CJ25) has been synthesized hydrothermally, by using 1,4-diaminobutane (DAB) as structure-directing agent. The structure has been solved by single-crystal X-ray diffraction analysis and further characterized by IR, 31 P MAS NMR, TG-DTA as well as compositional analyses. Crystal data: the triclinic space group P-1, a=8.0484(7) A, b=8.8608(8) A, c=13.2224(11) A, α=80.830(6) deg. , β=74.965(5) deg. , γ=78.782(6) deg. , Z=2, R 1[ I >2 σ ( I )] =0.0511 and wR 2(alldata) =0.1423. The alternation of AlO 4 tetrahedra and PO 4 tetrahedra gives rise to the four-membered corner-sharing chains, which are interconnected through AlO 6 octahedra to form the layered structure with 4,6-net sheet. Interestingly, oxalate ions are bis-bidentately bonded by participating in the coordination of AlO 6 , and bridging the adjacent AlO 6 octahedra. The layers are held with each other through strong H-bondings between the terminal oxygens. The organic ammonium cations and water molecules are located in the large cavities between the interlayer regions. -- Graphical abstract: The alternation of AlO 4 tetrahedra and PO 4 tetrahedra gives rise to the four-membered corner-sharing chains, which are interconnected through AlO 6 octahedra to form the layered structure with 4,6-net sheet. Oxalate ions are bis-bidentately boned by participating in the coordination of AlO 6 , and bridging the adjacent AlO 6 octahedra

Obtention of Samarium and Gadolinium concentrates by solvent extraction using mono-2-ethylhexyl ester of 2-ethylhexyl phosphonic acid

International Nuclear Information System (INIS)

Miranda Junior, Pedro

1996-01-01

The rare earth chlorides solution employed in this study, which is constituted by medium and heavy fractions, is derived from monazite processing accomplished by NUCLEMON-Mineroquimica (SP). This solution shows an acidity about 1.18 M and 189 g/L of rare earth oxides, containing as main constituents: Sm(34.55%), Gd(23.85%), Dy (6.82%), and Y (24.45%). It was used, as organic phase, 2-ethylhexyl phosphonic acid, mono-2-ethylhexylester diluted to 1 M in isododecane. (author)

Three new d10 transition metal selenites containing PO4 tetrahedron: Cd7(HPO4)2(PO4)2(SeO3)2, Cd6(PO4)1.34(SeO3)4.66 and Zn3(HPO4)(SeO3)2(H2O)

Science.gov (United States)

Ma, Yun-Xiang; Gong, Ya-Ping; Hu, Chun-li; Mao, Jiang-Gao; Kong, Fang

2018-06-01

Three new d10 transition metal selenites containing PO4 tetrahedron, namely, Cd7(HPO4)2(PO4)2(SeO3)2 (1), Cd6(PO4)1.34(SeO3)4.66 (2) and Zn3(HPO4)(SeO3)2(H2O) (3), have been synthesized by hydrothermal reaction. They feature three different structural types. Compound 1 exhibits a novel 3D network composed of 3D cadmium selenite open framework with phosphate groups filled in the 1D helical tunnels. The structure of compound 2 displays a new 3D framework consisted of 2D cadmium oxide layers bridged by SeO3 and PO4 groups. Compound 3 is isostructural with the reported solids of Co3(SeO3)3-x(PO3OH)x(H2O) when x is equal to 1.0. Its structure could be viewed as a 3D zinc oxide open skeleton with SeO3 and HPO4 polyhedra attached on the wall of the tunnels. They represent the only examples in metal selenite phosphates in addition to the above cobalt compounds. Optical diffuse reflectance spectra revealed that these solids are insulators, which are consistent with the results of band structure computations based on DFT algorithm.

Removal of phosphonates from industrial wastewater with UV/FeII, Fenton and UV/Fenton treatment.

Science.gov (United States)

Rott, Eduard; Minke, Ralf; Bali, Ulusoy; Steinmetz, Heidrun

2017-10-01

Phosphonates are an important group of phosphorus-containing compounds due to their increasing industrial use and possible eutrophication potential. This study involves investigations into the methods UV/Fe II , Fenton and UV/Fenton for their removal from a pure water matrix and industrial wastewaters. It could be shown that the degradability of phosphonates by UV/Fe II (6 kWh/m 3 ) in pure water crucially depended on the pH and was higher the less phosphonate groups a phosphonate contains. The UV/Fe II method is recommended in particular for the treatment of concentrates with nitrogen-free phosphonates, only little turbidity and a low content of organic compounds. Using Fenton reagent, the degradation of polyphosphonates was relatively weak in a pure water matrix (Fenton method (6 kWh/m 3 ), those phosphonates with the smallest numbers of phosphonate groups were easier degraded as well at pH 3.5 in a pure water matrix (o-PO 4 3- formation rates of up to 80%). Despite an incomplete transformation of organically bound phosphorus to o-PO 4 3- with Fenton reagent in an organically highly polluted wastewater (max. 15%), an almost total removal of the total P occurred. The most efficient total P elimination rates were achieved in accordance with the following Fenton implementation: reaction → sludge separation (acidic) → neutralization of the supernatant → sludge separation (neutral). Accordingly, a neutralization directly after the reaction phase led to a lower total P removal extent. Copyright © 2017 Elsevier Ltd. All rights reserved.

Self-ordered Porous Alumina Fabricated via Phosphonic Acid Anodizing

OpenAIRE

Akiya, Shunta; Kikuchi, Tatsuya; Natsui, Shungo; Sakaguchi, Norihito; Suzuki, Ryosuke O.

2016-01-01

Self-ordered periodic porous alumina with an undiscovered cell diameter was fabricated via electrochemical anodizing in a new electrolyte, phosphonic acid (H3PO3). High-purity aluminum plates were anodized in phosphonic acid solution under various operating conditions of voltage, temperature, concentration, and anodizing time. Phosphonic acid anodizing at 150-180 V caused the self-ordering behavior of porous alumina, and an ideal honeycomb nanostructure measuring 370-440 nm in cell diameter w...

Mechanism of intercalation in protonic conductors: case of HUP (H3OUO2PO4, 3H2O) and the corresponding xerogel [(UO2)sub(1.5-x) PO4Hsub(2x),2H2O

International Nuclear Information System (INIS)

Colomban, P.; Pham Thi, M.

1985-01-01

Intercalation of acetone alkylammonium, methylviologen and cobalticinium ions in HUP framework (H 3 OUO 2 PO 4 .3H 2 O) have been studied with different methods (IR and Raman spectroscopies, X-ray diffraction, DSC and scanning electron microscopy). Various reactions have been pointed out: i.e. proton transfer from H 3 O + to PO 4 3- , ionisation of cobaltocene into cobalticinium. Species orientation is discussed and its influence on conductivity and phase transitions [fr

Synthesis and bioactivity study of 30kda linear peg-interferon and its comparison with tri-branched peg-interferon

International Nuclear Information System (INIS)

Sabar, M.F.; Awan, F.I.

2013-01-01

Summary: Polyethylene glycol (PEG) is conjugated to the therapeutic proteins to enhance their circulating half life. PEGylation is a clinically proven strategy for increasing the therapeutic efficacy of protein-based medicines. PEG size and structure is very important in achieving specific properties in the conjugated protein. In this study we have compared the properties of newly synthesized linear PEG-IFN with a same sized (i.e., 30KDa) tri-branched PEG-IFN synthesized in the same lab earlier. For PEGylation reaction, interferon-alpha2 (IFNalpha2) concentration in sodium borate buffer pH 8.5 was optimized as 4.0mg/ml. The optimized molar ratio of PEG/IFN alpha2 was 3:1 instead of 5:1 in the case of tri-branched PEG published earlier. Other parameters of reaction were same as in our previous publication. Mono PEGylation degree reached to 21%. Cation exchange chromatography was used to separate and purify mono PEGylated IFN from the reaction mixture. The purity of mono PEGylated IFN was greater than 95%. It is noticed that PEGylation was more site specific in tribranched than the linear conjugate. The in vitro bioactivity of linear mPEG-IFN is 10-fold lesser than as reported of tri-branched mPEG3L2-IFN. Thermal stability of linear mPEG-IFN is also smaller than mPEG/sub 3/L/sub 2/-IFN at 4 degree C. (author)

Conductivity And Thermal Stability of Solid Acid Composites CsH2PO4 /NaH2PO4/ SiO2

International Nuclear Information System (INIS)

Norsyahida Mohammad; Abu Bakar Mohamad; Abu Bakar Mohamad; Abdul Amir Hassan Kadhum

2016-01-01

Solid acid composites CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 with different mole ratios of CsH 2 PO 4 and NaH 2 PO 4 to SiO 2 were synthesized and characterized. Preliminary infrared measurements of CsH 2 PO 4 and its composites indicated that hydrogen bonds breaking and formation were detected between 1710 to 2710 cm -1 , while the rotation of phosphate tetrahedral anions occurred between 900 and 1200 cm -1 . The superprotonic transition of CsH 2 PO 4 / NaH 2 PO 4 / SiO 2 composite was identified at superprotonic temperatures between 230 and 260 degree Celcius, under atmospheric pressure. This study reveals higher conductivity values for composites with higher CsH 2 PO 4 (CDP) content. Solid acid composite CDP 613 appeared as the composite with the highest conductivity that is 7.2x10 -3 S cm -1 at 230 degree Celcius. Thermal stability of the solid acid composites such as temperature of dehydration, melting and decomposition were investigated. The addition of NaH 2 PO 4 lowers the dehydration temperature of the solid acid composites. (author)

Facile synthesis technology of Li_3V_2(PO_4)_3/C adding H_2O_2 in ball mill process

International Nuclear Information System (INIS)

Min, Xiujuan; Mu, Deying; Li, Ruhong; Dai, Changsong

2016-01-01

Highlights: • Sintering time of Li_3V_2(PO_4)_3 reduced to 6 hours by adding hydrogen peroxide. • Electrochemical performance of Li_3V_2(PO_4)_3 was improved by reducing sintering time. • The Li_3V_2(PO_4)_3 production process was simplified during material synthesis stage. - Abstract: Li_3V_2(PO_4)_3/C has stable structure, high theory specific capacity and good safety performance, therefore it has become the research focus of lithium-ion batteries in recent years. The facile synthesis technology of Li_3V_2(PO_4)_3/C was characterized by adding different amounts of H_2O_2. Structure and morphology characteristics were examined by XRD, TG, Raman Spectroscopy, XPS and SEM. Electrochemical performance was investigated by constant current charging and discharging test. The results revealed that the Li_3V_2(PO_4)_3/C electrochemical performance of adding 15 mL H_2O_2 was better after sintering during 6 h. At the charge cut-off voltage of 4.3 V, the first discharge capacity at 0.2 C rate reached 127 mAh g"−"1. Because of adding H_2O_2 in the ball-mill dispersant, the vanadium pentoxide formed the wet sol. The molecular-leveled mixture increased the homogeneity of raw materials. Therefore, the addition of H_2O_2 shortened the sintering time and significantly improved the electrochemical performance of Li_3V_2(PO_4)_3/C.

Systems of Ba(PO3)2-Sr(Pu3)2, Cd(PO3)2-Ca(PO3)2

International Nuclear Information System (INIS)

Tokman, I.A.; Bukhalova, G.A.

1977-01-01

Phase diagrams of the Ba(PO 3 ) 2 -Sr(PO 3 ) 2 and Cd(PO 3 ) 2 -Ca(PO 3 ) 2 systems have been studied and plotted by the methods of differential-thermal analysis (DTA), visual-polythermal, X-ray phase and infrared spectroscopy. The Ba(PO 3 ) 2 -Sr(PO 3 ) 2 system is of the eutectic type. In the binary system Cd(PO 3 ) 2 -Ca(PO 3 ) 2 the existence of a continuous series of solid solutions with a minimum at 858 deg C and 27.5 mol.% Ca(PO 3 ) 2 has been established

Nanocomposites of phosphonic-acid-functionalized polyethylenes with inorganic quantum dots.

Science.gov (United States)

Rünzi, Thomas; Baier, Moritz C; Negele, Carla; Krumova, Marina; Mecking, Stefan

2015-01-01

Insertion of diethyl vinyl phosphonates and free vinyl phosphonic acid, respectively, into [(P^O)Pd(Me)(dmso)] ((P^O) = κ(2)-P,O-Ar2PC6H4SO2O with Ar = 2-MeOC6H4) (1-dmso) occurs in a 2,1- as well as 1,2-fashion, to form a four-and a five-membered chelate [(P^O)Pd{κ(2)-C,O-CH(P(O)(OR)2)CH2CH3}] and [(P^O)Pd{κ(2)-C,O-CH2CH(P(O)(OR)2)CH3}] (R = H, Et). No decomposition or other reactions of 1 by free phosphonic acid moieties occur. Copolymerization in a pressure reactor by 1-dmso yields linear random poly(ethylene-co-diethyl vinyl phosphonate) and poly(ethylene-co-vinyl phosphonic acid). In these copolymerizations, reversible coordination of the phosphonate moieties of free monomer as well as chelate formation by incorporated monomer retards chain growth as also evidenced by relative binding studies of diethyl phosphonate towards 1. Post-polymerization emulsification of poly(ethylene-co-vinyl phosphonic acid) together with CdSe/CdS quantum dots (QDs) yields submicron (ca. 50 nm from dynamic light scattering (DLS) and transmission electron microscopy (TEM)) polymer particles with the QDs embedded in the functionalized polyethylene in a nonaggregated fashion. This embedding benefits the fluorescence behavior in terms of continuous emission and life-time as revealed by wide-field fluorescence measurements. These composite particle dispersions are employed as a ″masterbatch" together with an aqueous high density polyethylene (HDPE) dispersion to generate thin films (by spin-coating) and bulk materials (from the melt), respectively, in which the inorganic nanoparticles remain highly disperse. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Investigation of the Na2(H2PO2)2 - Ba(H2PO2)2 - H2O Water-Salt Ternary System at Room Temperature

OpenAIRE

Erge, Hasan; Turan, Hakan; Kul, Ali Riza

2016-01-01

Objective: In this study, the solubility, density, conductivity and phase equilibria of the Na2(H2PO2)2-Ba(H2PO2)2-H2O ternary system located in the structure of the Na+, Ba2+, (H2PO2)-//H2O quaternary reciprocal water-salt system were investigated using physicochemical analysis methods. Material and Methods: Riedel-de Haen and Merck salts were used to investigate the solubility and phase equilibria of the Na2(H2PO2)2 -Ba(H2PO2)2-H2O ternary water–salt system at room temperature Res...

Study of the solubility, viscosity and density in Na+, Zn2+/Cl− − H2O, Na+ − Zn2+ − (H2PO2)− − H2O, Na+, Cl−/(H2PO2)− − H2O, and Zn2+, Cl−/(H2PO2)− − H2O ternary systems, and in Na+, Zn2+/Cl−, (H2PO2)−//H2O reciprocal quaternary system at 273.15 K

International Nuclear Information System (INIS)

Adiguzel, Vedat; Erge, Hasan; Alisoglu, Vahit; Necefoglu, Hacali

2014-01-01

Highlights: • The physicochemical properties of ternary and one quaternary have been studied. • Reciprocal quaternary systems’ solubility and phase equilibrium have been studied. • In all systems the solid phases have been found. • It was found that Zn(H 2 PO 2 ) 2 salt contains 70% of the general crystallization field. - Abstract: The solubility and the physicochemical properties (density, viscosity) in the Na-Zn- Cl-H 2 O), (Na + Zn + H 2 PO 2 + H 2 O), (Na + Cl + H 2 PO 2 + H 2 O), and (Zn + Cl + H 2 PO 2 + H 2 O) ternaries, and in Na + , Zn 2+ /Cl − , (H 2 PO 2 ) − //H 2 O reciprocal quaternary systems at T = 273.15 K were investigated by using the isothermal method. The diagrams of ternary salts systems, (NaCl + ZnCl 2 + H 2 O), (NaCl + NaH 2 PO 2 + H 2 O), (NaH 2 PO 2 + Zn(H 2 PO 2 ) 2 + H 2 O), (ZnCl 2 + Zn(H 2 PO 2 ) 2 + H 2 O), are plotted in figures 1–4. However, whole ions of reciprocal quaternary salt systems are plotted in figure 5. Additionally, the density and viscosity values of ternary systems vs. their corresponding composition values in weight per cent are plotted in figures 6–10. At the (i) (ZnCl 2 + Zn(H 2 PO 2 ) 2 + H 2 O), (ii) (NaCl + ZnCl 2 + H 2 O), (iii) (NaCl + NaH 2 PO 2 + H 2 O), (iv) (NaH 2 PO 2 + Zn(H 2 PO 2 ) 2 + H 2 O) ternary systems the solid phase compositions have been determined as: (i) Zn(H 2 PO 2 ) 2 ⋅ H 2 O, Zn(H 2 PO 2 ) 2 , ZnCl 2 ⋅ 2H 2 O, (ii) NaCl, 2NaCl ⋅ ZnCl 2 ⋅ 2H 2 O, and ZnCl 2 ⋅ 2H 2 O, (iii) NaCl and NaH 2 PO 2 ⋅ H 2 O, (iv) Zn(H 2 PO 2 ) 2 ⋅ H 2 O and NaH 2 PO 2 ⋅ H 2 O, respectively. On the other hand reciprocal quaternary system was observed as: ZnCl 2 ⋅ 2H 2 O, 2NaCl ⋅ ZnCl 2 ⋅ 2H 2 O, Zn(H 2 PO 2 ) 2 ⋅ H 2 O, NaH 2 PO 2 ⋅ H 2 O, NaCl. According to results, the least soluble salt was Zn(H 2 PO 2 ) 2 . The crystallization field of this salt, being the largest in comparison with those of other salts, occupied 70% of the general crystallization field

Ferroelectric phase transition in hydrogen-bonded 2-aminopyridine phosphate (NC sub 4 H sub 4 NH sub 2)centre dot H sub 3 PO sub 4

CERN Document Server

Czapla, Z; Waskowska, A

2003-01-01

A new crystal of 2-aminopyridine phosphate (NC sub 4 H sub 4 NH sub 2)centre dot H sub 3 PO sub 4 has been grown and its x-ray structure and physical properties were studied. At room temperature the crystals are monoclinic, space group C2/c. The flat 2-aminopyridine cations are hydrogen bonded to the anionic [PO sub 4 ] groups. The interesting feature of the crystal structure is the three-dimensional network of hydrogen bonds including, among others, two strong, symmetrical O centre dot centre dot centre dot H, H centre dot centre dot centre dot O interactions with disordered proton locations. Symmetrically related PO sub 4 anions linked through these protons form infinite (PO sub 4) subinfinity chains along the crystal a-axis. The anomalies in the temperature dependence of the electric permittivity showed that the crystal undergoes ferroelectric phase transition at T sub c = 103.5 K. The spontaneous polarization takes place along the crystal a-axis, being parallel to the chains of the hydrogen-bonded PO sub ...

Obtention of Samarium and Gadolinium concentrates by solvent extraction using mono-2-ethylhexyl ester of 2-ethylhexyl phosphonic acid; Obtencao de concentrados de samario e gadolinio via extracao por solventes com o ester mono-2-etilhexil do acido 2-etilhexilfosfonico

Energy Technology Data Exchange (ETDEWEB)

Miranda, Junior, Pedro

1996-07-01

The rare earth chlorides solution employed in this study, which is constituted by medium and heavy fractions, is derived from monazite processing accomplished by NUCLEMON-Mineroquimica (SP). This solution shows an acidity about 1.18 M and 189 g/L of rare earth oxides, containing as main constituents: Sm(34.55%), Gd(23.85%), Dy (6.82%), and Y (24.45%). It was used, as organic phase, 2-ethylhexyl phosphonic acid, mono-2-ethylhexylester diluted to 1 M in isododecane. (author)

Synthesis and regulation of α-LiZnPO4.H2O via a solid-state reaction at low-heating temperatures

International Nuclear Information System (INIS)

Liao Sen; Chen Zhipeng; Tian Xiaozhen; Wu Wenwei

2009-01-01

A simple and novel route for the synthesis of a lithium zinc phosphate hydrate, α-LiZnPO 4 .H 2 O, was studied, and the target product was obtained with LiH 2 PO 4 .H 2 O and ZnCO 3 as raw materials and polyethylene glycol-400 (PEG-400) as a surfactant via a one step solid-state reaction at room temperature (25 deg. C). The product was characterized with X-ray powder diffraction (XRD), thermogravimetric analysis and the 1st derivativative of thermogravimetric analysis (TG/DTG) and Fourier transform infrared spectroscopy (FTIR). The comparison experimental results suggested that aging temperature controlled the products of the synthesis, that is, the α-LiZnPO 4 .H 2 O was formed when the reaction mixture was aged at room temperature, and the α-LiZnPO 4 was obtained when the reaction mixture was aged at 80 deg. C.

Synthesis and crystal structure of 4-fluorobenzylammonium dihydrogen phosphate, [FC6H4CH2NH3]H2PO4

Directory of Open Access Journals (Sweden)

Ali Rayes

2016-12-01

Full Text Available The asymmetric unit of the title salt, [p-FC6H4CH2NH3]+·H2PO4−, contains one 4-fluorobenzylammonium cation and one dihydrogen phosphate anion. In the crystal, the H2PO4− anions are linked by O—H...O hydrogen bonds to build corrugated layers extending parallel to the ab plane. The FC6H4CH2NH3+ cations lie between these anionic layers to maximize the electrostatic interactions and are linked to the H2PO4− anions through N—H...O hydrogen bonds, forming a three-dimensional supramolecular network. Two hydrogen atoms belonging to the dihydrogen phosphate anion are statistically occupied due to disorder along the OH...HO direction.

Effect of Phosphate Salts (Na3PO4, Na2HPO4, and NaH2PO4) on Ag3PO4 Morphology for Photocatalytic Dye Degradation under Visible Light and Toxicity of the Degraded Dye Products

NARCIS (Netherlands)

Amornpitoksuk, P; Intarasuwan, K; Suwanboon, S; Baltrusaitis, Jonas

2013-01-01

Ag3PO4 was synthesized by the precipitation method using three different types of phosphate salts (Na3PO4, Na2HPO4, and NaH2PO4) as a precipitating agent. Hydrolysis of each phosphate salt gave a specific pH that affected the purity and morphology of the prepared Ag3PO4. The Ag3PO4 prepared from

Equilibrium Studies on the Extraction of Yttrium from Chloride Medium by Mono (2-Ethylhexyl) 2-Ethylhexyl Phosphonic Acid (Ion quest 801)

International Nuclear Information System (INIS)

Zaki, E.E.; Ismail, Z.H.; Aly, H.F.; Sabet, S.A.

2008-01-01

Since 90 Y is one of the useful radioisotopes in nuclear medicine, liquid-liquid extraction of yttrium from chloride medium has been studied under various conditions using neutralized and un-neutralized mono (2-ethylhexyl) 2-ethylhexyl phosphonic acid (EHEHPA) as an extractant. Effect of reagent concentration, ph of the aqueous medium, metal ion concentration and nature of the diluent on the extraction process has been carried out. Effect of temperature was studied and thermodynamic parameters were evaluated. Yttrium extracted in organic phase was stripped with various reagents. The stoichiometry of the extracted species of yttrium was determined on the basis of slope analysis of experimental results. Equilibrium equations of the extraction process have been estimated and verified

Hydrothermal synthesis, crystal structure and properties of a novel chain coordination polymer constructed by tetrafunctional phosphonate anions and cobalt ions

International Nuclear Information System (INIS)

Guan, Lei; Wang, Ying

2015-01-01

A novel cobalt phosphonate, [Co(HL)(H 2 O) 3 ] n (1) (L=N(CH 2 PO 3 H) 3 3− ) has been synthesized by hydrothermal reaction at 150 °C and structurally characterized by X-ray diffraction, infrared spectroscopy, elemental and thermogravimetric analysis. Complex 1 features a 1D chain structure with double-channel built from CoO 6 octahedra bridged together by the phosphonate groups. Each cobalt ion is octahedrally coordinated by three phosphonate oxygen atoms and three water molecules. The coordinated water molecules can form the hydrogen bonds with the phosphonate oxygen atoms to link the 1D chains, building a 2D layered structure, further resulting in a 3D network. The luminescence spectrum indicates an emission maximum at 435 nm. The magnetic susceptibility curve exhibits a dominant antiferromagnetic behavior with a weakly ferromagnetic component at low temperatures. - Graphical abstract: The connectivity between cobalt ions and the ligands results in a chain structure with a 1D double-channel structure, which is constructed by A-type subrings and B-type subrings. - Highlights: • The tetrafunctional phosphonate ligand was used as the ligand. • A novel chain structure can be formed by A-type rings and B-type rings. • Two types of rings can form a 1D double-channel structure, along the c-axis

Synthesis and some properties of hydrogen phosphites M3(H2PO3)3, where M = Ga, V, Fe, or In

International Nuclear Information System (INIS)

Zakharova, B.S.; Tarnopol'skij, V.A.; Chudinova, N.N.

2001-01-01

The conditions on production and the properties of the acid phosphites M 3 (H 2 PO 3 ) 3 (M = Ga, V, Fe, In) are demonstrated. The compounds were investigated by X-ray diffraction, thermal gravimetric analysis, IR spectroscopy and conductometry. Interaction of M 2 O 3 (M = Ga, V, Fe, In) with the melt of phosphorous acid was studied in the P : M = 1. 5 : 1 - 10 : 1 interval of compositions. The lattice parameters are given, the hypothesis on the available of superstructure in the M 3 (H 2 PO 3 ) 3 compounds is corroborated. From the measurements the proton conductivity in vanadium and indium phosphites is comprised of 2.5 x 10 -5 and 1.9 x 10 8- S/cm correspondingly. Acid vanadium and indium phosphites are behaved similarly during heating. The limit of thermal stability of the acid phosphites V(H 2 PO 3 ) 3 , V(H 2 PO 3 ) 3 grows [ru

Preparation, Characterization, and Structure of Two Layered Molybdenum(VI) Phosphates: KMo(H 2O)O 2PO 4 and NH 4Mo(H 2O)O 2PO 4

Science.gov (United States)

Millini, Roberto; Carati, Angela

1995-08-01

New layered Mo(VI) compounds, KMo(H 2O)O 2PO 4 (I) and NH 4Mo(H 2O)O 2PO 4 (II), were synthesized hydrothermally and their structures were determined from single-crystal X-ray analysis. Compounds (I) and (II) are isostructural and crystallize in the monoclinic P2 1/ n space group with a = 12.353(3), b = 8.623(2), c = 5.841(1) Å, β = 102.78(1)°, V = 606.8(2) Å 3, Z = 4, and R = 0.027 ( Rw = 0.030) for compound (I) and a = 12.435(3), b = 8.761(2), c = 6.015(1), β = 103.45(1)°, V = 637.3(2) Å 3, Z = 4, and R = 0.040 ( Rw = 0.041) for compound (II). The structure consists of layers built up of eight- and four-membered rings resulting from the alternation of corner-sharing [MoO 6] octahedra and [PO 4] tetrahedra. The layers stack along the (1¯01) direction by intercalating K and NH 4 ions.

Syntheses, crystal structures, NMR spectroscopy, and vibrational spectroscopy of Sr(PO{sub 3}F).H{sub 2}O and Sr(PO{sub 3}F)

Energy Technology Data Exchange (ETDEWEB)

Jantz, Stephan G.; Hoeppe, Henning A. [Lehrstuhl fuer Festkoerperchemie, Institut fuer Physik, Universitaet Augsburg (Germany); Wuellen, Leo van; Fischer, Andreas [Lehrstuhl fuer Chemische Physik und Materialwissenschaften, Institut fuer Physik, Universitaet Augsburg (Germany); Libowitzky, Eugen [Institute for Mineralogy and Crystallography, Faculty of Geosciences, Geography and Astronomy, University of Vienna (Austria); Baran, Enrique J. [Centro de Quimica Inorganica (CEQUINOR/CONICET, UNLP), Facultad de Ciencias Exactas, Universidad Nacional de La Plata (Argentina); Weil, Matthias [Institute for Chemical Technologies and Analytics, Division Structural Chemistry, Vienna University of Technology (Austria)

2016-03-15

Single crystals of Sr(PO{sub 3}F).H{sub 2}O {P2_1/c, Z = 4, a = 7.4844(2) Aa, b = 7.0793(2) Aa, c = 8.4265(2) Aa, β = 108.696(1) , V = 422.91(2) Aa"3, 2391 F_o"2, 70 parameters, R_1[F"2 > 2σ(F"2)] = 0.036; wR_2(F"2 all) = 0.049, S = 1.054} were grown from an aqueous solution by a metathesis reaction. The structure comprises [SrO{sub 8}] polyhedra and PO{sub 3}F tetrahedra that form a layered arrangement parallel to (100). The topotactic dehydration of this phase proceeds between 80 and 140 C to afford Sr(PO{sub 3}F). The monazite-type crystal structure of Sr(PO{sub 3}F) was elucidated from the X-ray powder data by simulated annealing [P2{sub 1}/c, Z = 4, a = 6.71689(9) Aa, b = 7.11774(11) Aa, c = 8.66997(13) Aa, β = 128.0063(7) , V = 326.605(8) Aa{sup 3}, R{sub p} = 0.010, R{sub wp} = 0.015, R{sub F} = 0.030]. During dehydration, the structure of Sr(PO{sub 3}F) .H{sub 2}O collapses along [100] from a layered arrangement into a framework structure, accompanied by a change of the coordination number of the Sr{sup 2+} ions from eight to nine. The magic-angle spinning (MAS) NMR and vibrational spectroscopy data of both phases are discussed. (Copyright copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Formation of phosphonates and pyrophosphates in the reactions of ...

Indian Academy of Sciences (India)

Bu-4-Me-C6H2O)2P(O)]2O (8) could be isolated, although the reaction mixture showed several other compounds in the phosphorus NMR. A possible pathway for the formation of phosphonate salts is proposed. The X-ray crystal structures of 4, ...

H2O2 rejuvenation-mediated synthesis of stable mixed-morphology Ag3PO4 photocatalysts

Directory of Open Access Journals (Sweden)

Henry Agbe

2018-04-01

Full Text Available Ag3PO4 photocatalyst has attracted interest of the scientific community in recent times due to its reported high efficiency for water oxidation and dye degradation. However, Ag3PO4 photo-corrodes if electron accepter such as AgNO3 is not used as scavenger. Synthesis of efficient Ag3PO4 followed by a simple protocol for regeneration of the photocatalyst is therefore a prerequisite for practical application. Herein, we present a facile method for the synthesis of a highly efficient Ag3PO4, whose photocatalytic efficiency was demonstrated using 3 different organic dyes: Methylene Blue (MB, Methyl orange (MO and Rhodamine B (RhB organic dyes for degradation tests. Approximately, 19 % of Ag3PO4 is converted to Ag0 after 4.30 hours of continuous UV-Vis irradiation in presence of MB organic dye. We have shown that the Ag/Ag3PO4 composite can be rejuvenated by a simple chemical oxidation step after several cycles of photocatalysis tests. At an optimal pH of 6.5, a mixture of cubic, rhombic dodecahedron, nanosphere and nanocrystals morphologies of the photocatalyst was formed. H2O2 served as the chemical oxidant to re-insert the surface metallic Ag into the Ag3PO4 photocatalyst but also as the agent that can control morphology of the regenerated as-prepared photocatalyst without the need for any other morphology controlling Agent (MCA. Surprisingly, the as- regenerated Ag3PO4 was found to have higher photocatalytic reactivity than the freshly made material and superior at least 17 times in comparison with the conventional Degussa TiO2, and some of TiO2 composites tested in this work. Keywords: Materials chemistry, Materials science, Engineering

Neutralization of Na2PO4: Reaction between Na3PO4 and CaCL2

International Nuclear Information System (INIS)

Xia Shenglan; Wang Luning

1990-01-01

The results of reaction Na 3 PO 4 with CaCl 2 in water at ambient and higher temperature are described. The reaction rate of Na 3 PO 4 with CaCl 2 is slow at ambient temperature and the reaction is complete at 260 deg C after 2 h. The products are Ca(OH) 2 and Ca 5 (PO 4 ) 3 (OH). The quantity of them is dependent upon the quanity of Na 3 PO 4 and CaCl 2 contained in water, all of them control pH of water

Structural and electrochemical studies of PPy/PEG-LiFePO4 cathode material for Li-ion batteries

International Nuclear Information System (INIS)

Fedorkova, Andrea; Nacher-Alejos, Ana; Gomez-Romero, Pedro; Orinakova, Renata; Kaniansky, Dusan

2010-01-01

A simple chemical oxidative polymerization of pyrrole (Py) directly onto the surface of LiFePO 4 particles was applied to the synthesis of polypyrrole-LiFePO 4 (PPy-LiFePO 4 ) powder. The LiFePO 4 sample without carbon coating was synthesized by a solvothermal method. The polyethylene glycol (PEG) was used as additive during Py polymerization for increasing the PPy-LiFePO 4 conductivity. Properties of resulting LiFePO 4 , PPy-LiFePO 4 and PPy/PEG-LiFePO 4 samples were characterized by XRD, SEM, TGA and galvanostatic charge-discharge measurements. These methods confirmed the presence of polypyrrole on LiFePO 4 particles and its homogeneous distribution in the resulting powder material. The PPy/PEG-LiFePO 4 composites show higher discharge capacity than pure LiFePO 4 , as PPy/PEG network improves the electron conductivity. It presents specific discharge capacity of 153 mAh/g at C/5 rate.

Catalytic phosphonation of high performance polymers and POSS. Novel components for polymer blend and nanocomposite fuel cell membranes

Energy Technology Data Exchange (ETDEWEB)

Bock, T.R.

2006-10-15

low as 1 mol-% per bromine. The developed approach's low catalyst demand, high yield, bromine-free products and wide range of applicable substrates greatly improves on existing polymer analogous methods. Good solubility of phosphonated polyelectrolytes was observed for phosphonated PSU, which was NMP-miscible up to a degree of phosphonation dsP=102 mol% (Reduct=alkyl) and 223 mol-% (Reduct=SiMe3). TGA of phosphonated derivatives showed backbone stability in air to 325-400 C, while SO3H-derivatives desulfonated at 180-330 C. Film casting of phosphonated PSU with dsP = 41-102 mol% gave flexible and stable membranes with H+-conductivities of {sigma}=1,2-8,7 mS/cm at 25 C. The polar interaction of PO3H2-groups led to a negligible mass swelling of swM=5,1-9,8 wt-% and a negative area swelling of swA=-4 A% in water at 80 C. Such unrivalled beneficial combination of properties suggest excellent applicability of phosphonated polyelectrolytes as membrane material in DMFC.

The Ca(PO3)2-Sr(PO3)2 system

International Nuclear Information System (INIS)

Bukhalova, G.A.; Tokman, I.A.

1977-01-01

Phase diagram of the system Ca(PO 3 ) 2 -Sr(PO 3 ) 2 has been studied and plotted with the aid of differential thermal, visual polythermal, X-ray analysis, and infrared spectroscopy. Continuous solid solutions are formed in the system with a minimum at 968 deg C and 25 mol.% of Sr(PO 3 ) 2 . Solid solutions decompose with the formation of about 30 mol.% of Sr(PO 3 ) 2

High temperature proton exchange membranes prepared from epoxycyclohexylethyltrimethoxysilane and amino trimethylene phosphonic acid as anhydrous proton conductors

International Nuclear Information System (INIS)

Chen, Cheng; Shen, Chunhui; Kong, Gengjin; Gao, Shanjun

2013-01-01

High temperature anhydrous proton exchange membranes based on phosphonic acid were prepared from epoxycyclohexylethyltrimethoxysilane (EHTMS) and amino trimethylene phosphonic acid (ATMP) by sol–gel process. The structures and properties of membranes with different phosphonic acid content were extensively characterized by FTIR, TG-DSC and XRD. Their proton conductivity under dry condition was also investigated under different temperature. The results show that the proton conductivity of the prepared membranes strongly depends on temperature, and the proton conductivity ranges from 8.81 × 10 −5 S cm −1 at 20 °C to 4.65 × 10 −2 S cm −1 at 140 °C under anhydrous condition. It indicates that the increasing temperature is favorable for congregating of the grafted–PO 3 H 2 and increasing of the proton mobility. In addition, from the results of AFM images, it was confirmed that the continuous distribution of phosphonic acid groups is favorable for the formation of the proton transport channel, which can significantly enhance the proton conductivity of the membranes. Highlights: ► Hybrid membranes of Epoxycyclohexylethyltrimethoxysilane and Amino trimethylene phosphonic acid. ► The proton conductivity is 4.65 × 10 −2 S cm −1 at 140 °C under anhydrous condition. ► Continuous uniform distributions of phosphonic acid groups can be observed by AFM. ► There could be hydrogen bond network within high temperature membranes

High temperature proton exchange membranes prepared from epoxycyclohexylethyltrimethoxysilane and amino trimethylene phosphonic acid as anhydrous proton conductors

Energy Technology Data Exchange (ETDEWEB)

Chen, Cheng [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China); Shen, Chunhui, E-mail: shenchunhui@whut.edu.cn [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China); Kong, Gengjin; Gao, Shanjun [Department of Polymer Materials and Engineering, School of Material Science and Engineering, Wuhan University of Technology, No. 122 Luoshi Road, Wuhan 430070 (China)

2013-06-15

High temperature anhydrous proton exchange membranes based on phosphonic acid were prepared from epoxycyclohexylethyltrimethoxysilane (EHTMS) and amino trimethylene phosphonic acid (ATMP) by sol–gel process. The structures and properties of membranes with different phosphonic acid content were extensively characterized by FTIR, TG-DSC and XRD. Their proton conductivity under dry condition was also investigated under different temperature. The results show that the proton conductivity of the prepared membranes strongly depends on temperature, and the proton conductivity ranges from 8.81 × 10{sup −5} S cm{sup −1} at 20 °C to 4.65 × 10{sup −2} S cm{sup −1} at 140 °C under anhydrous condition. It indicates that the increasing temperature is favorable for congregating of the grafted–PO{sub 3}H{sub 2} and increasing of the proton mobility. In addition, from the results of AFM images, it was confirmed that the continuous distribution of phosphonic acid groups is favorable for the formation of the proton transport channel, which can significantly enhance the proton conductivity of the membranes. Highlights: ► Hybrid membranes of Epoxycyclohexylethyltrimethoxysilane and Amino trimethylene phosphonic acid. ► The proton conductivity is 4.65 × 10{sup −2} S cm{sup −1} at 140 °C under anhydrous condition. ► Continuous uniform distributions of phosphonic acid groups can be observed by AFM. ► There could be hydrogen bond network within high temperature membranes.

Hydrogen bonds and van der Waals forces as tools for the construction of a herringbone pattern in the crystal structure of hexane-1,6-diaminium hexane-1,6-diyl bis(hydrogen phosphonate

Directory of Open Access Journals (Sweden)

Guido J. Reiss

2017-01-01

Full Text Available The asymmetric unit of the title salt, [H3N(CH26NH3][(HOO2P(CH26PO2(OH], consists of one half of a hexane-1,6-diaminium dication and one half of a hexane-1,6-diyl bis(hydrogen phosphonate dianion. Both are located around different centres of inversion (Wyckoff sites: 2a and 2d of the space group P21/c. The shape of the hexane-1,6-diaminium cation is best described as a double hook. Both aminium groups as well as the two attached CH2 groups are turned out from the plane of the central four C atoms. In contrast, all six C atoms of the dianion are almost in a plane. The hydrogen phosphonate (–PO3H groups of the anions and the aminium groups of the cations form two-dimensional O—H... and O—H...N hydrogen-bonded networks parallel to the ac plane, built up from ten-membered and twelve-membered ring motifs with graph-set descriptors R33(10 and R54(12, respectively. These networks are linked by the alkylene chains of the anions and cations. The resulting three-dimensional network shows a herringbone pattern, which resembles the parent structures 1,6-diaminohexane and hexane-1,6-diphosphonic acid.

Aqua(pentahydrogennitrilotris(methylenephosphonato))lithium hydrate [Li(H{sub 2}O)(N(CH{sub 2}PO{sub 3}){sub 3}H{sub 5})] • H{sub 2}O: Synthesis and structure

Energy Technology Data Exchange (ETDEWEB)

Somov, N. V., E-mail: somov@phys.unn.ru [Lobachevsky State University of Nizhny Novgorod (Russian Federation); Chausov, F. F., E-mail: xps@ftiudm.ru [Russian Academy of Sciences, Physicotechnical Institute, Ural Branch (Russian Federation); Zakirova, R. M., E-mail: ftt@udsu.ru [Udmurt State University (Russian Federation)

2016-05-15

Aqua(pentahydrogennitrilotris(methylenephosphonato))lithium hydrate is a linear coordination polymer. Its crystal structure is described in space group P{sup –}1, Z = 2; a = 5.5732(2), b = 7.0106(2), and c = 16.9010(5) Å; α = 97.515(2)°, β = 94.551(2)°, and γ = 95.123(2)°. The tetrahedral coordination of the Li atom includes two oxygen atoms of a phosphonate ligand, one oxygen atom of another phosphonate ligand, and a water molecule. Complex formation is accompanied by closing of the eight-membered Li–O–P–C–N–C–P–O chelate ring. Polymeric chains run along the [100] direction. The chains are connected by hydrogen bonds.

A second polymorph with composition Co3(PO4)2·H2O

Science.gov (United States)

Lee, Young Hoon; Clegg, Jack K.; Lindoy, Leonard F.; Lu, G. Q. Max; Park, Yu-Chul; Kim, Yang

2008-01-01

Single crystals of Co3(PO4)2·H2O, tricobalt(II) bis­[ortho­phosphate(V)] monohydrate, were obtained under hydro­thermal conditions. The compound is the second polymorph of this composition and is isotypic with its zinc analogue, Zn3(PO4)2·H2O. Three independent Co2+ cations are bridged by two independent orthophosphate anions. Two of the metal cations exhibit a distorted tetra­hedral coordination while the third exhibits a considerably distorted [5 + 1] octa­hedral coordination environment with one very long Co—O distance of 2.416 (3) Å. The former cations are bonded to four different phosphate anions, and the latter cation is bonded to four anions (one of which is bidentate) and one water mol­ecule, leading to a framework structure. Additional hydrogen bonds of the type O—H⋯O stabilize this arrangement. PMID:21200979

Betaine Phosphate (CH3)3N+CH2COO-.H3PO4 Modification Using D2O

International Nuclear Information System (INIS)

Saryati; Ridwan; Deswita; Sugiantoro, Sugik

2002-01-01

Betaine fosfate (CH 3 ) 3 N + CH 2 COO - .H 3 PO 4 modification by using D 2 O has been studied. This modification was carried out by slowly evaporation the saturated Betaine phosphat in the D 2 O solution in the dry box at 40 o C, until the dry crystal were formed. Based on the NMR data, can be concluded that the exchange process with D has been runed well and Betaine phosphate-D (CH 3 ) 3 N + CH 2 COO - .H 3 PO 4 has been resulted. From the X-ray diffraction pattern data can be concluded that there are a deference in the crystal structure between Betaine phosphate and Betaine phosphate modification result. From the Differential Scanning Colorimeter (DSC) diagram at the range temperature from 30 o C to 250 o C, can be shown that the Betaine phosphate-H has two endothermic transition phase, at 99 o C with a very little adsorbed calor and at 221.50 o C with -26.75 cal/g. Modified Betaine phosphate has also two endothermic transition phase, at 99.86 o C with -1.94 cal/g and at 171.01 o C with -3.48 cal/g. It can be conclosed that the D atom substitution on the H atoms in Betaine phosphate, to change the crystal and the endothermic fase temperature and energy

Corrosion characteristics of an aluminium alloy in the H3PO4 - CO2 mixture

International Nuclear Information System (INIS)

Aljinovic, Lj.; Smith, M.; Gotovac, V.

1998-01-01

The Al 6063 alloy examined in this work contains silicon and magnesium capable of forming Mg 2 Si and iron, which can form an intermetallic second phase (FeAl 3 ). In order to examine the influence of temperature on the corrosion behaviour of the Al 6063 alloy, examinations were carried out in aerated H 3 PO 4 and in H 3 PO 4 saturated with CO 2 at temperatures of 20, 30, 40, and 50 C. The following electrochemical methods were applied: determination of dependence of E OCP on time, recording of anodic and cathodic polarization curves, and cyclic voltammetry. It has been observed that corrosion parameters obtained are strongly temperature dependent. They also depend on CO 2 dissolved in H 3 PO 4 . CO 2 retards cathodic and anodic reactions at all temperatures, which can be attributed to formation of a kind of mechanical passivity as alloy components react with CO 2 . (orig.)

A second polymorph with composition Co3(PO42·H2O

Directory of Open Access Journals (Sweden)

Yang Kim

2008-10-01

Full Text Available Single crystals of Co3(PO42·H2O, tricobalt(II bis[orthophosphate(V] monohydrate, were obtained under hydrothermal conditions. The compound is the second polymorph of this composition and is isotypic with its zinc analogue, Zn3(PO42·H2O. Three independent Co2+ cations are bridged by two independent orthophosphate anions. Two of the metal cations exhibit a distorted tetrahedral coordination while the third exhibits a considerably distorted [5 + 1] octahedral coordination environment with one very long Co—O distance of 2.416 (3 Å. The former cations are bonded to four different phosphate anions, and the latter cation is bonded to four anions (one of which is bidentate and one water molecule, leading to a framework structure. Additional hydrogen bonds of the type O—H...O stabilize this arrangement.

Facile synthesis technology of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C adding H{sub 2}O{sub 2} in ball mill process

Energy Technology Data Exchange (ETDEWEB)

Min, Xiujuan [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Mu, Deying [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Department of Environmental Engineering, Harbin University of Commerce, Harbin 150076 (China); Li, Ruhong [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China); Dai, Changsong, E-mail: changsd@hit.edu.cn [MIIT Key Laboratory of Critical Materials Technology for New Energy Conversion and Storage, Harbin Institute of Technology, School of Chemistry and Chemical Engineering, Harbin 150001 (China)

2016-11-15

Highlights: • Sintering time of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} reduced to 6 hours by adding hydrogen peroxide. • Electrochemical performance of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} was improved by reducing sintering time. • The Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} production process was simplified during material synthesis stage. - Abstract: Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C has stable structure, high theory specific capacity and good safety performance, therefore it has become the research focus of lithium-ion batteries in recent years. The facile synthesis technology of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C was characterized by adding different amounts of H{sub 2}O{sub 2}. Structure and morphology characteristics were examined by XRD, TG, Raman Spectroscopy, XPS and SEM. Electrochemical performance was investigated by constant current charging and discharging test. The results revealed that the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C electrochemical performance of adding 15 mL H{sub 2}O{sub 2} was better after sintering during 6 h. At the charge cut-off voltage of 4.3 V, the first discharge capacity at 0.2 C rate reached 127 mAh g{sup −1}. Because of adding H{sub 2}O{sub 2} in the ball-mill dispersant, the vanadium pentoxide formed the wet sol. The molecular-leveled mixture increased the homogeneity of raw materials. Therefore, the addition of H{sub 2}O{sub 2} shortened the sintering time and significantly improved the electrochemical performance of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C.

Structural transitions, ion mobility, and conductivity in CsSbF3(H2PO4)

Science.gov (United States)

Kavun, V. Ya.; Uvarov, N. F.; Slobodyuk, A. B.; Ulihin, A. S.; Kovaleva, E. V.; Zemnukhova, L. A.

2018-02-01

Structural transitions, ion mobility, and conductivity in CsSbF3(H2PO4) (I) have been investigated by the methods of 1H, 19F, 31P NMR (including 1H, 19F, 31P MAS NMR), DSC, X-ray diffraction, and impedance spectroscopy. It was found that the fundamental changes in 1H, 19F, 31P NMR spectra (above 390 K) were associated with the formation of a crystalline disorder phase I with high ionic mobility in the proton and fluoride sublattices, as a result of a phase transition in the 400-420 K range. In the same temperature range, the transition of PO2(OH)2- anions from the "rigid lattice" to fast reorientations takes place. Above 430 K, there occurs a transition from the crystalline disordered phase to the amorphous one. The types of ion mobility in CsSbF3(H2PO4) and its amorphous phase have been established and temperature ranges of their realization have been determined (150-450 K). According to the NMR data, the diffusion in the proton sublattice of the disordered crystalline and amorphous phases is preserved even at room temperature. The ionic conductivity in CsSbF3(H2PO4) reaches the values of 2.6 × 10-4 S/cm in the temperature range 410-425 K and decreases down to 2.0 × 10-5 S/cm upon transition to the amorphous phase (435-445 K).

The system La(PO3)3-Ca(PO3)2-P2O5

International Nuclear Information System (INIS)

Jungowska, W.; Znamierowska, T.

1993-01-01

Ternary system La(PO 3 ) 3 -Ca(PO 3 ) 2 -P 2 O 5 has been studied by means of thermal and roentgenography analysis. The existence of single intermediate compound CaLa(PO 3 ) 5 has been observed. The phase diagrams for the ternary system as well as for two binary systems La(PO 3 ) 3 -Ca(PO 3 ) 2 and CaLa(PO 3 ) 5 -LaP 5 O 11 have been shown. 7 refs, 3 figs

Investigation on pseudosymmetry, twinning and disorder in crystal structure determinations: Ba(H2O)M2III[PO3(OH)]4 (M=Fe, V) as examples

International Nuclear Information System (INIS)

Sun Wei; Huang Yaxi; Pan Yuanming; Mi Jinxiao

2012-01-01

Twinning commonly occurs in monoclinic crystals with dimensionally similar a and c axes and results in pseudo-orthorhombic symmetries with overlapping diffractions. For example, twinning in the new synthetic compound Ba(H 2 O)Fe 2 [PO 3 (OH)] 4 , which varies in space group from P2 1 to P2 1 /c with approximately equal a and c axial lengths, gives rise to a pseudosymmetry of C222 1 . Similarly, the related compound Ba(H 2 O)V 2 [PO 3 (OH)] 4 is commonly twinned and varies in space groups as well, arising from ordered to disordered distributions of the barium cations and water molecules in the cavities. Moreover, analyses of these and other twinned structures show that the small average standard uncertainty of bond distances is a sensitive criterion for structure determinations, especially for those involving crystal twinning as well as order–disorder. A proper structure determination leads to small standard uncertainties of the atomic displacement parameters, which further result in the small standard uncertainties of bond distances. - Graphical abstract: Ba(H 2 O)M 2 III [PO 3 (OH)] 4 (M=Fe, V) varies in space group from P2 1 to P2 1 /c, arising from ordered to disordered distributions of Ba 2+ and H 2 O in the cavities. Highlights: ► Twinning commonly occurs in monoclinic crystals with a≈c. ► Overlapping diffractions from twin domains hamper with the determination of real space groups. ► Conventional criteria for evaluating the real space groups are not effective in this case. ► Small standard uncertainty of bond distances is proposed as a sensitive criterion. ► Using this criterion we determined the order–disorder structures of Ba(H 2 O)M 2 III [PO 3 (OH)] 4 (M=Fe, V) from twinned crystals.

Canted antiferromagnetism in KNi3[PO3(F,OH)]2[PO2(OH)2]F2 with a stair-case Kagomé lattice

Science.gov (United States)

Liu, Li-Chen; Ren, Wei-Jian; Huang, Ya-Xi; Pan, Yuanming; Mi, Jin-Xiao

2017-10-01

A new nickel phosphate KNi3[PO3(F,OH)]2[PO2(OH)2]F2 has been synthesized using a modified hydrothermal method. Structural characterizations show that it adopts a 3D framework structure with 2D layers of Ni octahedra in a stair-case Kagomé lattice. The Ni2 octahedron at the inversion center shares two trans-faces with Ni1 octahedra to form a linear trimer (Ni3O8F6) as the basic structural unit. The Ni-trimers are linked between themselves by sharing F-corners and to [PO3(F,OH)] tetrahedral groups by sharing O-corners to form 2D stair-case Kagomé layers, which are parallel to the (100) plane and are stacked along the a-axis. Successive Kagomé layers are combined together by [PO2(OH)2] tetrahedral groups and interstice cations K+. Magnetic measurements reveal that KNi3[PO3(F,OH)]2[PO2(OH)2]F2 exhibits a canted antiferromagnetic ordering with a ferromagnetic component at low temperatures.

Separation of the components of the TBP-H2 MBP-HDBP-H3PO4 mixture

International Nuclear Information System (INIS)

Pires, M.A.F.; Abrao, A.

1981-04-01

Several schemes for the separation of dibutylphosphoric acid (HDBP), monobutylphosphoric acid (H 2 MBP) and orthophosphoric acid (H 3 PO 4 ) as hydrolytic and radiolytic degradation products from tri-n-butylphosphate (TBP) were studied. For the resolution of a HDBP, H 2 MPB and H 3 PO 4 mixture in TBP-diluent, or in TBP-diluent-heavy metal nitrate (U-VI, Th-IV or Zr-IV), techniques such as ion exchange chromatography, ion chromatography and separation onto a chromatographic alumina column were investigated. For the identification, determination and analytical resolution following up for the several systems studied, techniques such as refraction index measurement, electrical conductivity measurement, molecular spectrophotometry and gas chromatography were applied. Special emphasys was given to the separation using alumina column where the HDBP acid was retained and eluted selectively for its separation from TBP-varsol-uranyl nitrate mixtures. This analytical procedure was applied to the samples coming from the Uranium Purification Pilot Plant in operation at the Centro de Engenharia Quimica (IPEN). (Author) [pt

Use of new phosphonylating and coupling agents in the synthesis of oligodeoxyribonucleotides via the H-phosphonate approach.

OpenAIRE

Sakatsume, O; Yamane, H; Takaku, H; Yamamoto, N

1990-01-01

New phosphonylating and coupling agents for the synthesis of oligodeoxyribonucleotides via H-phosphonate approach have been developed. Tris(1,1,1,3,3,3-hexafluoro-2-propyl) phosphite, prepared by the reaction of lithium salt of 1,1,1,3,3,3-hexafluoro-2-propoxide with PCl3, reacts with deoxyribonucleosides in the presence of a catalytic amount of triethylamine to produce in the high yield the corresponding deoxyribonucleoside 3'-H-phosphonate units. The use of a new coupling reagent, 1,3-dimet...

Hydrated aluminophosphate (AlPO/sub 4/. 1. 5H/sub 2/O) with PO/sub 4/, AlO/sub 4/ and AlO/sub 4/(H/sub 2/O)/sub 2/ groups and encapsulated water

Energy Technology Data Exchange (ETDEWEB)

Pluth, J.J.; Smith, J.V.

1986-09-15

Aluminium phosphate hydrate, AlPO/sub 4/ /sub ./ 1.5H/sub 2/O, M/sub r/=148.98, orthorhombic, Pbca, a=19.3525(13), b=9.7272(7), c=9.7621(8) A, V=1837.7(1) A/sup 3/, Z=16, D/sub x/=2.15 g cm/sup -3/, lambda(CuK..cap alpha..)=1.5418 A, ..mu..=68.2 cm/sup -1/, F(000)=1200, Tproportional to 295 K, R=0.033 for 1530 diffractions. A 4-connected framework contains PO/sub 4/ tetrahedra interposed between AlO/sub 4/ tetrahedra and AlO/sub 4/(H/sub 2/O)/sub 2/ octahedra at the nodes of cross-linked alternate 6/sup 3/ and 4.8/sup 2/ nets. A two-dimensional channel system, limited by 8-rings, lies between adjacent 6/sup 3/ nets. One H/sub 2/O of each octahedron lies in a 6-ring, and the other forms a continuous chain with a third H/sub 2/O which is held in place only by hydrogen bonds.

Calcioferrite with composition (Ca3.94Sr0.06Mg1.01(Fe2.93Al1.07(PO46(OH4·12H2O

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Barbara Lafuente

2014-03-01

Full Text Available Calcioferrite, ideally Ca4MgFe3+4(PO46(OH4·12H2O (tetracalcium magnesium tetrairon(III hexakis-phosphate tetrahydroxide dodecahydrate, is a member of the calcioferrite group of hydrated calcium phosphate minerals with the general formula Ca4AB4(PO46(OH4·12H2O, where A = Mg, Fe2+, Mn2+ and B = Al, Fe3+. Calcioferrite and the other three known members of the group, montgomeryite (A = Mg, B = Al, kingsmountite (A = Fe2+, B = Al, and zodacite (A = Mn2+, B = Fe3+, usually occur as very small crystals, making their structure refinements by conventional single-crystal X-ray diffraction challenging. This study presents the first structure determination of calcioferrite with composition (Ca3.94Sr0.06Mg1.01(Fe2.93Al1.07(PO46(OH4·12H2O based on single-crystal X-ray diffraction data collected from a natural sample from the Moculta quarry in Angaston, Australia. Calcioferrite is isostructural with montgomeryite, the only member of the group with a reported structure. The calcioferrite structure is characterized by (Fe/AlO6 octahedra (site symmetries 2 and -1 sharing corners (OH to form chains running parallel to [101]. These chains are linked together by PO4 tetrahedra (site symmetries 2 and 1, forming [(Fe/Al3(PO43(OH2] layers stacking along [010], which are connected by (Ca/Sr2+ cations (site symmetry 2 and Mg2+ cations (site symmetry 2; half-occupation. Hydrogen-bonding interactions involving the water molecules (one of which is equally disordered over two positions and OH function are also present between these layers. The relatively weaker bonds between the layers account for the cleavage of the mineral parallel to (010.

Infrared spectroscopic investigation of M(H2PO4)2x2H2O (M=Mg, Mn, Cd) dehydration products

International Nuclear Information System (INIS)

Pechkovskij, V.V.; Dzyuba, E.D.; Mel'nikova, R.Ya.; Salonets, G.I.; Kovalishina, V.I.; Malashonok, I.E.

1982-01-01

Using the method of IR spectroscopy the composition of products separated at different stages of M(H 2 PO 4 ) 2 x2H 2 O dehydration, where M=Mg, Mn, Cd, has been investigated. It is shown that cation influence is expressed in strengthening of bond of proton-containing groups in the structure of initial compounds from magnesium to cadmium. A supposition is made that the difference in bond character of the groups more evidently expressed for partially dehydrated products of the composition M(H 2 PO 4 ) 2 , conditions a possibility of dehydration in two directions- with the formation of intermediate phase MH 2 P 2 O 7 or with separation of three phosphoric acid

3D-QSAR studies and molecular docking on [5-(4-amino-1 H-benzoimidazol-2-yl)-furan-2-yl]-phosphonic acid derivatives as fructose-1,6-biphophatase inhibitors

Science.gov (United States)

Lan, Ping; Xie, Mei-Qi; Yao, Yue-Mei; Chen, Wan-Na; Chen, Wei-Min

2010-12-01

Fructose-1,6-biphophatase has been regarded as a novel therapeutic target for the treatment of type 2 diabetes mellitus (T2DM). 3D-QSAR and docking studies were performed on a series of [5-(4-amino-1 H-benzoimidazol-2-yl)-furan-2-yl]-phosphonic acid derivatives as fructose-1,6-biphophatase inhibitors. The CoMFA and CoMSIA models using thirty-seven molecules in the training set gave r cv 2 values of 0.614 and 0.598, r 2 values of 0.950 and 0.928, respectively. The external validation indicated that our CoMFA and CoMSIA models possessed high predictive powers with r 0 2 values of 0.994 and 0.994, r m 2 values of 0.751 and 0.690, respectively. Molecular docking studies revealed that a phosphonic group was essential for binding to the receptor, and some key features were also identified. A set of forty new analogues were designed by utilizing the results revealed in the present study, and were predicted with significantly improved potencies in the developed models. The findings can be quite useful to aid the designing of new fructose-1,6-biphophatase inhibitors with improved biological response.

Lanthanide(III) complexes of a mono(methylphosphonate) analogue of H4dota: the influence of protonation of the phosphonate moiety on the TSAP/SAP isomer ratio and the water exchange rate.

Science.gov (United States)

Rudovský, Jakub; Cígler, Petr; Kotek, Jan; Hermann, Petr; Vojtísek, Pavel; Lukes, Ivan; Peters, Joop A; Vander Elst, Luce; Muller, Robert N

2005-04-08

A monophosphonate analogue of H4dota, 1,4,7,10-tetraazacyclododecane-4,7,10-tris(carboxymethyl)-1-methylphosphonic acid (H5do3aP), and its complexes with lanthanides were synthesized. Multinuclear NMR studies reveal that, in aqueous solution, lanthanide(III) complexes of the ligand exhibit structures analogous to those of H4dota complexes. Thus, the central ion is nine-coordinate, surrounded by four nitrogen atoms, three acetate and one phosphonate oxygen atoms, and one water molecule in an apical position. For complexes of H5do3aP with Ln(III) ions in the middle of the series, the abundance of the desired twisted square-antiprismatic (TSAP) isomer is higher than for the corresponding H4dota complexes. The TSAP/square-antiprismatic (SAP) isomer ratio is highly sensitive to protonation of the phosphonate group: a higher abundance of the TSAP isomer was found in acidic solutions. The microscopic protonation constants of the TSAP isomers are higher than those of the SAP isomers. The presence of one water molecule in the first coordination sphere of the complexes in the pH region studied (pH 2.5-7.0) is confirmed by 17O NMR spectroscopy. The results of a simultaneous fit of variable-temperature 17O NMR relaxation data and 1H NMRD profiles show that the residence time of water (tauM) in the Gd(III) complex is much smaller than for [Gd(dota)(H2O)]-. The exchange rate appears to be dependent on the pH of the solution. The values of tauM are 37, 40, and 14 ns at pH 2.5, 4.7, and 7.0, respectively. These observations can be explained by an extensive second-sphere hydrogen-bonding network that varies with the state of protonation of the phosphonate moiety. Upon protonation of the complex, the second-sphere hydration probably becomes more ordered, which may result in a decrease in penetrability and an increase in tauM. The relaxivity of the Gd(III) complex is almost independent of the pH and is equal to 4.7 s(-1) mM(-1) (20 MHz, pH 7 and 37 degrees C). The solid

Formation and transformations of radicals in frozen aqueous solutions of components of nucleic acids and H3PO4

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Minkhadzhidinova, D.R.; Chefranova, O.A.; Sharpatyj, V.A.

1977-01-01

Radiolysis of frozen aqueous solutions of 6-16 M H 3 PO 4 and 5 M NaH 2 PO 4 was studied, as well as radiolysis of these systems in the presence of nitrous bases and glucose. In aqueous solutions of H 3 PO 4 and NaH 2 PO 4 irradiated at 77 K, two groups of radicals formed as a result of interaction of the oxidative component of radiolysis of water with phosphate ions were identified. Their photolytic properties were studied. Primary products of radiolysis of the nitrous bases in phosphoric- acid solutions are anion- and cation-radicals. The molal absorption coefficients of the particles were determined

Analytical resolution of the mixture TBP-HDBP-H2MBP-H3PO4

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Pires, M.A.F.

1983-01-01

Several schemes for the separation of dibutylphosphoric acid (HDBP), main degradation product of tributylphosphate (TBP), in TBP/diluent, TBP/diluent-uranyl nitrate and TBP/diluent-thorium nitrate mixture were studied. For the resolution of HDBP-TBP/diluent-heavy metal nitrates (U-VI,Th-IV) systems, techniques such as: in exchange chromatography, ion chromatography using common ion exchangers and chromatographic separation with alumina column were investigated. For the identification, determination and analytical resolution following up the several systems studied, techniques such as refraction index measurement, electrical conductivity measurement, molecular absorption spectrophotometry, gas chromatography and ion chromatography, were applied. The separation of HDBP component was achieved using an alumina column where it was adsorbed from the TBP/diluent-uranyl nitrate and selectively eluted. Several modifications of this procedure for samples from the Uranium Purification Pilot Plant at Instituto de Pesquisas Energeticas e Nucleares (Sao Paulo, Brazil) were made. Special emphasis was given to the determination of HDBP using the ion chromatography technique. HDBP along with any monobutylphosphate acid (H 2 MBP) and phosphoric acid (H 3 PO 4 ) were stripped from the organic phase into dilute sodium hydroxide. HDBP is separated from H 2 MBP and H 3 PO 4 by ion chromatography and determined by its peak height. The determination of degradation products from TBP in TBP/diluent-uranyl nitrate and TBP/diluent-thorium nitrate systems was then performed. The detection limit for dibutylphosphate is 1.0μg HDBP/ml of analyte solution. (Author) [pt

Singlet ground state in the spin-1/2 weakly coupled dimer compound NH4[ (V2O3)2(4,4'-b p y ) 2(H2PO4)(PO4)2] .0.5 H2O

Science.gov (United States)

Arjun, U.; Kumar, Vinod; Anjana, P. K.; Thirumurugan, A.; Sichelschmidt, J.; Mahajan, A. V.; Nath, R.

2017-05-01

We present the synthesis and a detailed investigation of structural and magnetic properties of polycrystalline NH4[(V2O3)2(4,4'-b p y ) 2(H2PO4) (PO4)2] .0.5 H2O by means of x-ray diffraction, magnetic susceptibility, electron spin resonance, and 31P nuclear magnetic resonance measurements. Temperature-dependent magnetic susceptibility could be described well using a weakly coupled spin-1/2 dimer model with an excitation gap Δ /kB≃26.1 K between the singlet ground state and triplet excited states and a weak interdimer exchange coupling J'/kB≃4.6 K. A gapped chain model also describes the data well with a gap of about 20 K. The electron spin resonance intensity as a function of temperature traces the bulk susceptibility nicely. The isotropic Landé g factor is estimated to be about g ≃1.97 , at room temperature. We are able to resolve the 31P NMR signal as coming from two inequivalent P sites in the crystal structure. The hyperfine coupling constant between 31P nucleus and V4 + spins is calculated to be Ahf(1 ) ≃2963 Oe/μB and Ahf(2 ) ≃1466 Oe/μB for the P(1) and P(2) sites, respectively. Our NMR shift and spin-lattice relaxation rate for both the 31P sites show an activated behavior at low temperatures, further confirming the singlet ground state. The estimated value of the spin gap from the NMR data measured in an applied field of H =9.394 T is consistent with the gap obtained from the magnetic susceptibility analysis using the dimer model. Because of a relatively small spin gap, NH4[(V2O3)2(4,4'-b p y ) 2(H2PO4) (PO4)2] .0.5 H2O is a promising compound for further experimental studies under high magnetic fields.

An analysis of pH, pO2 and pCO2 in the peritoneal fluid of dogs with ascites of various etiologies.

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Glińska-Suchocka, K; Sławuta, P; Jankowski, M; Kubiak, K; Spużak, J; Borusewicz, P

2016-01-01

The aim of the study was to assess pH, pO2 and pCO2 in peritoneal fluid. The study was conducted on a group of 22 dogs with symptoms of ascites. Group 1 consisted of 4 dogs with adenocarcinoma, group 2--of 6 dogs with glomerulonephritis, group 3 of 8 dogs with hepatic cirrhosis and group 4 of 4 dogs with bacterial peritonitis. An abdominal cavity puncture was performed in all dogs and the fluid was drawn into a heparinized syringe in order to assess pH, pO2 and pCO2 . The analysis of pH in the peritoneal fluid revealed statistically significant differences between group 4 and groups 1 (p=0.01), 2 (p=0.01), and 3 (p=0.01). The lowest pH value compared to the other studied groups was recorded in group 4. In group 4, the pO2 was the lowest compared to the other groups (group 1 p=0.01, group 2 p=0.01, group 3 p=0.01). The value of pCO2 was the highest in group 4 compared to groups 1, 2, and 3. The study found statistically significant differences in pH, pCO2 and pCO2 between group 4 (the group of dogs with bacterial peritonitis) and the other groups of dogs. This was probably linked to the pathogenesis of peritonitis. As a result of an inflammatory reaction within the peritoneal cavity, there is an increase in fibrin accumulations leading to a decreased oxygen supply causing the oxidative glucose metabolism to change into a non-oxidative glucose metabolism. This, in turn, causes a decrease in pH, acidosis, and a low oxidoreduction potential. It also impairs phagocytosis and activates proteolytic enzymes which create ideal conditions for the growth of anaerobic bacteria. The obtained results indicate that the pH, pO2 and pCO2 may be used to differentiate bacterial peritonitis from ascites of other etiologies.

On thermal expansion of RbD2PO4, CsH2PO4 and CsDrPO4 crystals

International Nuclear Information System (INIS)

Vlokh, O.G.; Shchur, Ya.I.; Klymiv, I.M.

1994-01-01

Thermal expansion of RbD 2 PO 4 , CsH 2 PO 4 , CsD 2 PO 4 crystals in a wide range of temperatures embracing points of phase transitions was studied. An explanation of anomalous behaviour of thermal expansion factor along directions b and c in the course of RbD 2 PO 4 transfer into intermediate phase was suggested. 10 refs., 4 figs

Effect of H3PO4 Concentration and Particle Size of the Eggshell Used in Laying Hens Fed on Bone and Blood

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S. Kismiati

2013-06-01

Full Text Available Normal 0 false false false IN X-NONE X-NONE MicrosoftInternetExplorer4 The objective of this research was to evaluate the effect of H3 PO4 concentrations and particle size of eggshell used in the feed of laying hens on bone and blood profiles. Ninety-six laying hens (Isa Brown strain age 25 weeks were kept in individual battery cage and divided into 8 groups randomly. Group 1 was fed using eggshell with out H3PO4 and particle size of <1 mm (feed 1 , group 2 was fed using eggshell that has been soaked in H3PO4 3% and particle size of <1 mm (feed 2, group 3 were fed using eggshell that has been soaked in H3PO4 4% and particle size of <1 mm (feed 3, group 4 was fed using eggshell that has been soaked in H3PO4 5% and particle size of <1 mm (feed 4, group 5 was fed using eggshell that has been soaked in H3PO4 and particle size of <3 mm (feed 5 , group of 6 was fed using eggshell that has been soaked in H3PO4 3% and particle size of <3 mm (feed 6, group 7 was fed using eggshell that has been soaked in H3PO4 4 % and particle size of <3 mm (feed 7 and a group of 8 was fed using eggshell that has been soaked in H3PO4 5% and particle size of <3 mm (feed 8. A Completely Randomized Design patterns factorial 4 x 2 x 3 was used in this research. Result of this research showed that had no interaction effect (P>0.05 between the H3PO4 concentration and particle size of eggshell on weight, volume, diameter of tibia bone and calcium and phosphorus content of the blood. The concentration of H3PO4 or particles size also had no effect (P>0.05 on all variables. Normal 0 false false false IN X-NONE X-NONE MicrosoftInternetExplorer4 /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-qformat:yes; mso-style-parent:""; mso-padding-alt:0cm 5.4pt 0cm 5.4pt; mso-para-margin:0cm; mso-para-margin-bottom:.0001pt; mso-pagination:widow-orphan; font

Core/shell-type nanorods of Tb{sup 3+}-doped LaPO{sub 4}, modified with amine groups, revealing reduced cytotoxicity

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Runowski, Marcin [Adam Mickiewicz University, Department of Rare Earths, Faculty of Chemistry (Poland); Dąbrowska, Krystyna [Polish Academy of Sciences, Bacteriophage Laboratory, Institute of Immunology and Experimental Therapy (Poland); Grzyb, Tomasz [Adam Mickiewicz University, Department of Rare Earths, Faculty of Chemistry (Poland); Miernikiewicz, Paulina [Polish Academy of Sciences, Bacteriophage Laboratory, Institute of Immunology and Experimental Therapy (Poland); Lis, Stefan, E-mail: blis@amu.edu.pl [Adam Mickiewicz University, Department of Rare Earths, Faculty of Chemistry (Poland)

2013-11-15

A simple co-precipitation reaction between Ln{sup 3+} cations (Ln = lanthanide) and phosphate ions in the presence of polyethylene glycol (PEG), including post-treatment under hydrothermal conditions, leads to the formation of Tb{sup 3+}-doped LaPO{sub 4} crystalline nanorods. The nanoparticles obtained can be successfully coated with amorphous and porous silica, forming core/shell-type nanorods. Both products reveal intensive green luminescence under UV lamp irradiation. The surface of the core/shell-type product can also be modified with –NH{sub 2} groups via silylation procedure, using 3-aminopropyltriethoxysilane as a modifier. Powder X-ray diffraction, transmission electron microscopy, and scanning electron microscopy confirm the desired structure and needle-like shape of the products synthesized. Fourier transform infrared spectroscopy and specific surface area measurements by Brunauer–Emmett–Teller method reveal a successful surface modification with amine groups of the core/shell-type nanoparticles prepared. The nanomaterials synthesized exhibit green luminescence characteristic of Tb{sup 3+} ions, as solid powders and aqueous colloids, examined by spectrofluorometry. The in vitro cytotoxicity studies reveal different degree toxicity of the products. LaPO{sub 4}:Tb{sup 3+}@SiO{sub 2}@NH{sub 2} exhibits the smallest toxicity against B16F0 mouse melanoma cancer cells and human skin microvascular endothelial cell lines, in contrast to the most toxic LaPO{sub 4}:Tb{sup 3+}@SiO{sub 2}.Graphical Abstract.

Synthesis and X-ray Powder Structure of a New Pillared Layered Cadmium Phosphonate, Giving Evidence that the Intercalation of Alkylamines into Cd(O(3)PR).H(2)O Is Topotactic.

Science.gov (United States)

Fredoueil, Florence; Massiot, Dominique; Janvier, Pascal; Gingl, Franz; Bujoli-Doeuff, Martine; Evain, Michel; Clearfield, Abraham; Bujoli, Bruno

1999-04-19

A new pillared layered phosphonate, cadmium 2-aminoethylphosphonate, Cd(O(3)PC(2)H(4)NH(2)) (1), has been synthesized, and its structure was solved ab initio from X-ray powder diffraction data and refined by Rietveld methods. Compound 1 is orthorhombic: space group Pna2(1), a = 15.4643(2) Å, b = 5.16512(7) Å, c = 6.27650(8) Å, and Z = 4. Its layer arrangement is similar to that in Cd(O(3)PR).H(2)O, except that the water molecule coordinated to cadmium in Cd(O(3)PR).H(2)O is replaced by the nitrogen atom from the amino ends of the ethyl chains borne by phosphorus of the upper and lower layers. The strong similarity of the IR, (31)P, and (113)Cd NMR data for Cd(O(3)PC(2)H(4)NH(2)) and Cd(O(3)PCH(3)).n-NH(2)C(4)H(9) clearly shows the topotactic character of the intercalation of n-alkylamines in the dehydrated form of Cd(O(3)PR).H(2)O to yield Cd(O(3)PR).n-NH(2)R'.

Development and in vivo evaluation of an oral insulin-PEG delivery system.

Science.gov (United States)

Calceti, P; Salmaso, S; Walker, G; Bernkop-Schnürch, A

2004-07-01

Insulin-monomethoxypoly(ethylene glycol) derivatives were obtained by preparation of mono- and di-terbutyl carbonate insulin derivatives, reaction of available protein amino groups with activated 750 Da PEG and, finally, amino group de-protection. This procedure allowed for obtaining high yield of insulin-1PEG and insulin-2PEG. In vivo studies carried out by subcutaneous injection into diabetic mice demonstrated that the two bioconjugates maintained the native biological activity. In vitro, PEGylation was found to enhance the hormone stability towards proteases. After 1 h incubation with elastase, native insulin, insulin-1PEG and insulin-2PEG undergo about 70, 30 and 10% degradation, respectively, while in the presence of pepsin protein degradation was 100, 70 and 50%, respectively. The attachment of low molecular weight PEG did not significantly (P >0.05) alter insulin permeation behavior across the intestinal mucosa. Insulin-1PEG was formulated into mucoadhesive tablets constituted by the thiolated polymer poly(acrylic acid)-cysteine. The therapeutic agent was sustained released from these tablets within 5 h. In vivo, by oral administration to diabetic mice, the glucose levels were found to decrease of about 40% since the third hour from administration and the biological activity was maintained up to 30 h. According to these results, the combination of PEGylated insulin with a thiolated polymer used as drug carrier matrix might be a promising strategy for oral insulin administration.

Symmetry and topology code of the cluster self-assembly of framework MT structures of alumophosphates AlPO4(H2O)2 (metavariscite and variscite) and Al2(PO4)2(H2O)3 (APC)

Science.gov (United States)

Ilyushin, G. D.; Blatov, V. A.

2017-03-01

The supramolecular chemistry of alumophosphates, which form framework 3D MT structures from polyhedral AlO4(H2O)2 clusters with octahedral O coordination (of M polyhedra) and PO4 and AlO4 with tetrahedral O coordination (of T polyhedra), is considered. A combinatorial-topological modeling of the formation of possible types of linear (six types) and ring (two types) tetrapolyhedral cluster precursors M2T2 from MT monomers is carried out. Different versions of chain formation from linked (MT)2 rings (six types) are considered. The model, which has a universal character, has been used to simulate the cluster selfassembly of the crystal structure of AlPO4(H2O)2 minerals (metavariscite, m-VAR, and variscite, VAR) and zeolite [Al2(PO4)2(H2O)2] · H2O (APC). A tetrapolyhedral linear precursor is established for m-VAR and a ring precursor (MT)2 is established for VAR and APC. The symmetry and topology code of the processes of crystal structure self-assembly from cluster precursors is completely reconstructed. The functional role of the O-H···O hydrogen bonds is considered for the first time. The cluster self-assembly model explains the specific features of the morphogenesis of single crystals: m-VAR prisms, flattened VAR octahedra, and needleshaped APC square-base prisms.

PNA-PEG modified silicon platforms as functional bio-interfaces for applications in DNA microarrays and biosensors.

Science.gov (United States)

Cattani-Scholz, Anna; Pedone, Daniel; Blobner, Florian; Abstreiter, Gerhard; Schwartz, Jeffrey; Tornow, Marc; Andruzzi, Luisa

2009-03-09

The synthesis and characterization of two types of silicon-based biofunctional interfaces are reported; each interface bonds a dense layer of poly(ethylene glycol) (PEG(n)) and peptide nucleic acid (PNA) probes. Phosphonate self-assembled monolayers were derivatized with PNA using a maleimido-terminated PEG(45). Similarly, siloxane monolayers were functionalized with PNA using a maleimido-terminated PEG(45) spacer and were subsequently modified with a shorter methoxy-terminated PEG(12) ("back-filling"). The long PEG(45) spacer was used to distance the PNA probe from the surface and to minimize undesirable nonspecific adsorption of DNA analyte. The short PEG(12) "back-filler" was used to provide additional passivation of the surface against nonspecific DNA adsorption. X-ray photoelectron spectroscopic (XPS) analysis near the C 1s and N 1s ionization edges was done to characterize chemical groups formed in the near-surface region, which confirmed binding of PEG and PNA to the phosphonate and silane films. XPS also indicated that additional PEG chains were tethered to the surface during the back-filling process. Fluorescence hybridization experiments were carried out with complementary and noncDNA strands; both phosphonate and siloxane biofunctional surfaces were effective for hybridization of cDNA strands and significantly reduced nonspecific adsorption of the analyte. Spatial patterns were prepared by polydimethylsiloxane (PDMS) micromolding on the PNA-functionalized surfaces; selective hybridization of fluorescently labeled DNA was shown at the PNA functionalized regions, and physisorption at the probe-less PEG-functionalized regions was dramatically reduced. These results show that PNA-PEG derivatized phosphonate monolayers hold promise for the smooth integration of device surface chemistry with semiconductor technology for the fabrication of DNA biosensors. In addition, our results confirm that PNA-PEG derivatized self-assembled carboxyalkylsiloxane films are

Synthesis of phosphonic acid derivatized bipyridine ligands and their ruthenium complexes.

Science.gov (United States)

Norris, Michael R; Concepcion, Javier J; Glasson, Christopher R K; Fang, Zhen; Lapides, Alexander M; Ashford, Dennis L; Templeton, Joseph L; Meyer, Thomas J

2013-11-04

Water-stable, surface-bound chromophores, catalysts, and assemblies are an essential element in dye-sensitized photoelectrosynthesis cells for the generation of solar fuels by water splitting and CO2 reduction to CO, other oxygenates, or hydrocarbons. Phosphonic acid derivatives provide a basis for stable chemical binding on metal oxide surfaces. We report here the efficient synthesis of 4,4'-bis(diethylphosphonomethyl)-2,2'-bipyridine and 4,4'-bis(diethylphosphonate)-2,2'-bipyridine, as well as the mono-, bis-, and tris-substituted ruthenium complexes, [Ru(bpy)2(Pbpy)](2+), [Ru(bpy)(Pbpy)2](2+), [Ru(Pbpy)3](2+), [Ru(bpy)2(CPbpy)](2+), [Ru(bpy)(CPbpy)2](2+), and [Ru(CPbpy)3](2+) [bpy = 2,2'-bipyridine; Pbpy = 4,4'-bis(phosphonic acid)-2,2'-bipyridine; CPbpy = 4,4'-bis(methylphosphonic acid)-2,2'-bipyridine].

A new set of K3Fe3(PO4)4·yH2O (0 ≤ y ≤ 1) layered phases obtained by topotactic reactions

Science.gov (United States)

Trad, Khiem; Wattiaux, Alain; Ben Amara, Mongi; Delmas, Claude; Carlier, Dany

2018-06-01

K3Fe3(PO4)4·H2O powder was synthesized by Na+/K+ exchange reaction from Na3Fe3(PO4)4 in aqueous medium. The replacement of the sodium cations by the potassium larger ones and water molecules causes a structural distortion leading to P2/n monoclinic K3Fe3(PO4)4·H2O. This new layered phase was characterized by XRD, Mössbauer spectroscopy and magnetic measurements. The study of its thermal stability reveals that other new layered K3Fe3(PO4)4·yH2O with (0 ≤ y ≤ 1) phases can be stabilized up to 600 °C and finally at higher temperature a new K3Fe3(PO4)4 polymorph with a different structural type is irreversibility formed.

NMR investigation on isotope effect of glycinium phosphite H sub 3 NCH sub 2 COOH centre dot H sub 2 PO sub 3

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Ishibashi, T

2003-01-01

The motions of the phosphite anions and glycinium cations in H sub 3 NCH sub 2 COOH centre dot H sub 2 PO sub 3 (GPI) and its deuterated analogue (DGPI) were investigated by sup 1 H, sup 1 sup 3 C and sup 3 sup 1 P spin-lattice relaxation times T sub 1. For both GPI and DGPI, T sub 1 's of the sup 1 H, sup 1 sup 3 C and sup 3 sup 1 P nuclei reflect the amino rotation, methylene libration and motion of the phosphite anions, respectively. Activation energies obtained from T sub 1 's of sup 1 H, sup 1 sup 3 C and sup 3 sup 1 P nuclei are 28.6(2), 26.0(4) and 26.2(4) kJ/mol for GPI and are 34.9(6), 27(1), 47(2) kJ/mol for DGPI, respectively. The deuterium substitution increases E sub a for the motion influenced by the hydrogen bonding. In all the observed motions, correlation times of DGPI are larger than those of GPI. (author)

Selective detection of Fe2+ by combination of CePO4:Tb3+ nanocrystal-H2O2 hybrid system with synchronous fluorescence scan technique.

Science.gov (United States)

Chen, Hongqi; Ren, Jicun

2012-04-21

A new method for quenching kinetic discrimination of Fe(2+) and Fe(3+), and sensitive detection of trace amount of Fe(2+) was developed by using synchronous fluorescence scan technique. The principle of this assay is based on the quenching kinetic discrimination of Fe(2+) and Fe(3+) in CePO(4):Tb(3+) nanocrytals-H(2)O(2) hybrid system and the Fenton reaction between Fe(2+) and H(2)O(2). Stable, water-soluble and well-dispersible CePO(4):Tb(3+) nanocrystals were synthesized in aqueous solutions, and characterized by transmission electron microscopy (TEM) and electron diffraction spectroscopy (EDS). We found that both Fe(2+) and Fe(3+) could quench the synchronous fluorescence of CePO(4):Tb(3+) nanocrytals-H(2)O(2) system, but their quenching kinetics velocities were quite different. In the presence of Fe(3+), the synchronous fluorescent intensity was unchanged after only one minute, but in the presence of Fe(2+), the synchronous fluorescent intensity decreased slowly until 28 min later. The Fenton reaction between Fe(2+) and H(2)O(2) resulted in hydroxyl radicals which effectively quenched the synchronous fluorescence of the CePO(4):Tb(3+) nanocrystals due to the oxidation of Ce(3+) into Ce(4+) by hydroxyl radicals. Under optimum conditions, the linear range for Fe(2+) is 3 nM-2 μM, and the limit of detection is 2.0 nM. The method was used to analyze water samples.

Synthesis, structure and magnetic properties of a new iron phosphonate-oxalate with 3D framework: [Fe(O3PCH3)(C2O4)0.5(H2O)

International Nuclear Information System (INIS)

Zhang Yangyang; Qi Yue; Zhang Ying; Liu Ziyu; Zhao Yinfeng; Liu Zhongmin

2007-01-01

A new iron phosphonate-oxalate [Fe(O 3 PCH 3 )(C 2 O 4 ) 0.5 (H 2 O)] (1), has been synthesized under hydrothermal condition. The single-crystal X-ray diffraction studies reveal that 1 consists of layers of vertex-linked FeO 6 octahedra and O 3 PC tetrahedra, which are further connected by bis-chelate oxalate bridges, giving to a 3D structure with 10-membered channels. Crystal data: monoclinic, P2 1 /n (no. 14), a=4.851(2)A, b=16.803(7)A, c=7.941(4)A, β=107.516(6) o , V=617.2(5)A 3 , Z=4, R 1 =0.0337 and wR 2 =0.0874 for 1251 reflections [I>2σ(I)]. Mossbauer spectroscopy measurement confirms the existence of high-spin Fe(III) in 1. Magnetic studies show that 1 exhibits weak ferromagnetism with T N =30K due to a weak spin canting

Formation of condensed phosphates when heating CdO with NH4H2PO4

International Nuclear Information System (INIS)

Atstinya, L.Zh.; Dindune, A.P.; Konstant, Z.A.

1987-01-01

A study was made on process of CdO thermal condensation with NH 4 H 2 PO 4 depending on the ratio of basic substances and temperature synthesis conditions. It was established that reaction between CdO and NH 4 H 2 PO 4 of pure for analysis grade was initiated when basic mixtures were pounded with a pestle. Heating of cadmium-ammonium triphosphate with products of ammonium dihydrophosphate polycondensation in 330-350 deg C range resulted to CdNH 4 (PO 3 ) 3 formation. Exoeffect on DTA curves corresponded at 540 deg C to formation of α-Cd(PO 3 ) 2 . α-Cd(PO 3 ) 2 → β-Cd(PO 3 ) 2 transition took place at 810 deg C with successive melting of β-Cd(PO 3 ) 2 at 850 deg C, which was supported by the DTA curve and sharp change of the relative electric conductivity

In pursuit of the rhabdophane crystal structure: from the hydrated monoclinic LnPO{sub 4}.0.667H{sub 2}O to the hexagonal LnPO{sub 4} (Ln = Nd, Sm, Gd, Eu and Dy)

Energy Technology Data Exchange (ETDEWEB)

Mesbah, Adel, E-mail: adel.mesbah@cea.fr [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France); Clavier, Nicolas [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France); Elkaim, Erik [Synchrotron SOLEIL, L' Orme des Merisiers, Saint-Aubin, BP 48, 91192 Gif-sur-Yvette Cedex (France); Szenknect, Stéphanie; Dacheux, Nicolas [ICSM, UMR 5257 CNRS – CEA – ENSCM – Université de Montpellier, Site de Marcoule - Bât 426, BP 17171, 30207 Bagnols/Cèze (France)

2017-05-15

The dehydration process of the hydrated rhabdophane LnPO{sub 4}.0.667H{sub 2}O (Ln = La to Dy) was thoroughly studied over the combination of in situ high resolution synchrotron powder diffraction and TGA experiments. In the case of SmPO{sub 4}.0.667H{sub 2}O (monoclinic, C2), a first dehydration step was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2) with Z =12 and a =17.6264(1) Å, b =6.9704(1) Å, c =12.1141(1) Å, β=133.74(1) °, V =1075.33(1) Å{sup 3}. In agreement with the TGA and dilatometry experiments, all the water molecules were evacuated above 220 °C yielding to the anhydrous form, which crystallizes in the hexagonal P3{sub 1}21 space group with a =7.0389(1) Å, c =6.3702(1) Å and V =273.34(1) Å{sup 3}. This study was extended to selected LnPO{sub 4}.0.667H{sub 2}O samples (Ln= Nd, Gd, Eu, Dy) and the obtained results confirmed the existence of two dehydration steps before the stabilization of the anhydrous form, with the transitory formation of LnPO{sub 4}.0.5H{sub 2}O. - Graphical abstract: The dehydration process of the rhabdophane SmPO{sub 4}.0.667H{sub 2}O was studied over combination of in situ high resolution synchrotron powder diffraction and TGA techniques, a first dehydration was identified around 80 °C leading to the formation of SmPO{sub 4}.0.5H{sub 2}O (Monoclinic, C2). Then above 220 °C, the anhydrous form of the rhabdophane SmPO{sub 4} was stabilized and crystallizes in the hexagonal P3{sub 1}21 space group. - Highlights: • In situ synchrotron powder diffraction was carried out during the dehydration of the rhabdopahe LnPO{sub 4}.0.667H{sub 2}O. • The heat of the rhabdophane LnPO{sub 4}.0.667H{sub 2}O leads to LnPO{sub 4}.0.5H{sub 2}O then to anhydrous rhabdophane LnPO{sub 4}. • LnPO{sub 4}.0.5H{sub 2}O (monoclinic, C2) and LnPO{sub 4} (Hexagonal, P3{sub 1}21) were solved over the use of direct methods.

Conductivity of Composite Material Based on System NdPO4·nH2OCsH2PO4

DEFF Research Database (Denmark)

Anfimova, Tatiana; Bjerrum, Niels J.; Li, Qingfeng

2013-01-01

The goal of the present study was to obtain a comprehensive knowledge about synthesis conditions, structure, thermal behavior and conductivity properties of neodymiumorthophosphates in order to analyze of use this material in intermediate temperature fuel cells due to their thermal and chemical...... stability properties.The impedance spectroscopy technique (IS) was used to measure the conductivity. The conductivity of composites observed to be lower than conductivity of pure CsH2PO4 but had improved sufficiently conductivity of pure NdPO4·nH2O...

Nucleoside-O-Methyl-(H)-Phosphinates: Novel Monomers for the Synthesis of Methylphosphonate Oligonucleotides Using H-Phosphonate Chemistry.

Science.gov (United States)

Kostov, Ondřej; Páv, Ondřej; Rosenberg, Ivan

2017-09-18

This unit comprises the straightforward synthesis of protected 2'-deoxyribonucleoside-O-methyl-(H)-phosphinates in both 3'- and 5'-series. These compounds represent a new class of monomers compatible with the solid-phase synthesis of oligonucleotides using H-phosphonate chemistry and are suitable for the preparation of both 3'- and 5'-O-methylphosphonate oligonucleotides. The synthesis of 4-toluenesulfonyloxymethyl-(H)-phosphinic acid as a new reagent for the preparation of O-methyl-(H)-phosphinic acid derivatives is described. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

Structure and properties of polyaniline interacting with H-phosphonates

Czech Academy of Sciences Publication Activity Database

Bláha, Michal; Trchová, Miroslava; Bober, Patrycja; Morávková, Zuzana; Zujovic, Z. D.; Filippov, Sergey K.; Prokeš, J.; Pilař, Jan; Stejskal, Jaroslav

2017-01-01

Roč. 232, October (2017), s. 79-86 ISSN 0379-6779 R&D Projects: GA ČR(CZ) GA17-04109S Institutional support: RVO:61389013 Keywords : conducting polymers * polyaniline * H-phosphonate Subject RIV: CD - Macromolecular Chemistry OBOR OECD: Polymer science Impact factor: 2.435, year: 2016

Additional of polyethylene glycol on the preparation of LaPO4:Eu3+ phosphor

Science.gov (United States)

Panatarani, Camellia; Joni, I. Made

2013-09-01

Solution phase method was used to synthesis nanocrystal LaPO4:Eu3+. Polyethylene glycol with vary molecular weight (MW) was added to allow an exothermic reaction to get a high crystalinity of LaPO4:Eu3+. The x-ray pattern of as prepared LaPO4 was obtained by using an X'pert PANalytical diffractometer with CuKα radiation (λ = 1.5406 Å) and the photoluminescent measurement spectra is obtained by using Fluorescence Spectrometer LS55, Perkin Elmer. The additional of various MW of polyethylene glycol into the precursor solution of LaPO4:Eu3+ affected the crystal structure and luminescent properties. Higher MW of PEG depressing the luminescent spectra. The emission origin from 5D0-7F4 transition vanished by additional 500,000 and 2,000,000 MW of PEG.

Neutron diffraction studies of the Na-ion battery electrode materials NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3}

Energy Technology Data Exchange (ETDEWEB)

Yahia, H. Ben [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar); Essehli, R., E-mail: ressehli@qf.org.qa [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar); Avdeev, M. [Australian Nuclear Science and Technology Organisation, New Illawarra Road, Lucas Heights NSW 2234 (Australia); Park, J-B.; Sun, Y-K. [Department of Energy Engineering Hanyang University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Al-Maadeed, M.A. [Center for Advanced Materials (CAM), Qatar University, 2713 Doha (Qatar); Belharouak, I., E-mail: ibelharouak@qf.org.qa [Qatar Environment and Energy Research Institute, Hamad Bin Khalifa University, Qatar Foundation, P.O. Box 5825 Doha (Qatar)

2016-06-15

The new compounds NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} were synthesized by sol-gel method and their crystal structures were determined by using neutron powder diffraction data. These compounds were characterized by galvanometric cycling and cyclic voltammetry. NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} crystallize with a stuffed α-CrPO{sub 4}-type structure. The structure consists of a 3D-framework made of octahedra and tetrahedra that are sharing corners and/or edges generating channels along [100] and [010], in which the sodium atoms are located. Of significance, in the structures of NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} a statistical disorder Ni{sup 2+}/Cr{sup 3+} was observed on both the 8g and 4a atomic positions, whereas in NaCoCr{sub 2}(PO{sub 4}){sub 3} the statistical disorder Co{sup 2+}/Cr{sup 3+} was only observed on the 8g atomic position. When tested as negative electrode materials, NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} delivered specific capacities of 352, 385, and 368 mA h g{sup −1}, respectively, which attests to the electrochemical activity of sodium in these compounds. - Highlights: • NaCoCr{sub 2}(PO{sub 4}){sub 3}, NaNiCr{sub 2}(PO{sub 4}){sub 3}, and Na{sub 2}Ni{sub 2}Cr(PO{sub 4}){sub 3} were synthesized by sol-gel method. • The crystal structures were determined by using neutron powder diffraction data. • The three compounds crystallize with a stuffed α-CrPO{sub 4}-type structure. • The three compounds were tested as anodes in sodium-ion batteries. • Relatively high specific capacities were obtained for these compounds.

Magnesium doped gallium phosphonates Ga{sub 1-x}Mg{sub x}[H{sub 3+x}(O{sub 3}PCH{sub 2}){sub 3}N] (x = 0, 0.20) and the influence on proton conductivity

Energy Technology Data Exchange (ETDEWEB)

Homburg, Thomas; Reinsch, Helge; Stock, Norbert [Institut fuer Anorganische Chemie, Christian-Albrechts-Universitaet, Kiel (Germany); Tschense, Carsten B.L.; Senker, Juergen [Dept. of Inorganic Chemistry III, University of Bayreuth (Germany); Wolkersdoerfer, Konrad; Wark, Michael [Institut fuer Chemie, Carl von Ossietzky Universitaet Oldenburg (Germany); Toebbens, Daniel; Zander, Stefan [Helmholtz-Zentrum Berlin fuer Materialien und Energie GmbH, Berlin (Germany)

2018-02-01

In our contribution to the development of new proton conductive coordination polymers (CPs) we focus on the impact of a partial replacement of Ga{sup 3+} by Mg{sup 2+}. This approach should come along with the introduction of additional protons due to charge balances. In a first step we have synthesized an isostructural compound to the literature known compound AlH{sub 3}P3N [H{sub 6}P3N = nitrilotris(methylene)triphosphonic acid], where Al{sup 3+} is replaced by Ga{sup 3+}, since all attempts to incorporate Mg{sup 2+} ions directly into AlH{sub 3}P3N were not successful. The relative amount of Mg{sup 2+} and Ga{sup 3+} was established by EDX analysis. Rietveld refinement of the synchrotron data located the Ga{sup 3+} and Mg{sup 2+} ions on a split position, proving the disordered incorporation of the Mg{sup 2+} ions. Solid-state NMR spectroscopy confirms a disordered protonation of the phosphonate groups as well and shows that all amine groups are protonated. In order to investigate the effect on the proton conductivity the compounds Ga[H{sub 3}(O{sub 3}PCH{sub 2}){sub 3}N], denoted GaH{sub 3}P3N as well as Ga{sub 0.80}Mg{sub 0.20}[H{sub 3.20}(O{sub 3}PCH{sub 2}){sub 3}N], denoted GaMgH{sub 3.20}P3N, were characterized by electrochemical impedance spectroscopy (EIS). Arrhenius behavior in the investigated temperature range (70-130 C) was found for both compounds (activation energies of E{sub a} = 0.15 eV for GaH{sub 3}P3N and 0.17 eV for GaMgH{sub 3.20}P3N). The GaMgH{sub 3.20}P3N sample shows a reduced proton mobility (σ = 1.2 x 10{sup -4} S.cm{sup -1}) of about one order of magnitude in comparison to GaH{sub 3}P3N (σ = 1.0 x 10{sup -3} S.cm{sup -1}). (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

3.0 V High Energy Density Symmetric Sodium-Ion Battery: Na4V2(PO4)3∥Na3V2(PO4)3.

Science.gov (United States)

Yao, Xuhui; Zhu, Zixuan; Li, Qi; Wang, Xuanpeng; Xu, Xiaoming; Meng, Jiashen; Ren, Wenhao; Zhang, Xinhe; Huang, Yunhui; Mai, Liqiang

2018-03-28

Symmetric sodium-ion batteries (SIBs) are considered as promising candidates for large-scale energy storage owing to the simplified manufacture and wide abundance of sodium resources. However, most symmetric SIBs suffer from suppressed energy density. Here, a superior congeneric Na 4 V 2 (PO 4 ) 3 anode is synthesized via electrochemical preintercalation, and a high energy density symmetric SIB (Na 3 V 2 (PO 4 ) 3 as a cathode and Na 4 V 2 (PO 4 ) 3 as an anode) based on the deepened redox couple of V 4+ /V 2+ is built for the first time. When measured in half cell, both electrodes show stabilized electrochemical performance (over 3000 cycles). The symmetric SIBs exhibit an output voltage of 3.0 V and a cell-level energy density of 138 W h kg -1 . Furthermore, the sodium storage mechanism under the expanded measurement range of 0.01-3.9 V is disclosed through an in situ X-ray diffraction technique.

Brain parenchyma PO2, PCO2, and pH during and after hypoxic, ischemic brain insult in dogs.

Science.gov (United States)

McKinley, B A; Morris, W P; Parmley, C L; Butler, B D

1996-11-01

1) The investigation of fiberoptic PO2, PCO2, and pH sensor technology as a monitor of brain parenchyma during and after brain injury, and 2) the comparison of brain parenchyma PO2, PCO2, and pH with intracranial pressure during and after hypoxic, ischemic brain insult. Prospective, controlled, animal study in an acute experimental preparation. Physiology laboratory in a university medical school. Fourteen mongrel dogs (20 to 35 kg), anesthetized, room-air ventilated. Anesthesia was induced with thiopental and maintained after intubation using 1% to 1.5% halothane in room air (FiO2 0.21). Mechanical ventilation was established to maintain end-tidal PCO2 approximately 35 torr (-4.7 kPa). Intravenous, femoral artery, and pulmonary artery catheters were placed. The common carotid arteries were surgically exposed, and ultrasonic blood flow probes were applied. A calibrated intracranial pressure probe was placed through a right-side transcranial bolt, and a calibrated intracranial chemistry probe with optical sensors for PO2, PCO2, and pH was placed through a left-side bolt into brain parenchyma. Brain insult was induced in the experimental group (n = 6) by hypoxia (FiO2 0.1), ischemia (bilateral carotid artery occlusion), and hypotension (mean arterial pressure [MAP] approximately 40 mm Hg produced with isoflurane approximately 4%). After 45 mins, carotid artery occlusion was released, FiO2 was reset to 0.21, and anesthetic was returned to halothane (approximately 1.25%). The control group (n = 5) had the same surgical preparation and sequence of anesthetic agent exposure but no brain insult. Monitored variables included brain parenchyma PO2, PCO2, and pH, which were monitored at 1-min intervals, and intracranial pressure, MAP, arterial hemoglobin oxygen saturation (by pulse oximetry), end-tidal PCO2, and carotid artery blood flow rate, for which data were collected at 15-min intervals for 7 hrs. Arterial and mixed venous blood gas analyses were done at approximately 1

Measuring interstitial pH and pO2 in mouse tumors.

Science.gov (United States)

Jain, Rakesh K; Munn, Lance L; Fukumura, Dai

2013-07-01

This protocol outlines methods to measure two extravascular parameters, interstitial pH and partial pressure of oxygen (pO2), in mouse tumors. The method for measuring interstitial pH uses fluorescence ratio imaging microscopy (FRIM) of the pH-sensitive fluorescent dye 2',7'-bis-(2-carboxyethyl)-5,6-carboxyfluorescein (BCECF). The method for measuring interstitial pO2 is based on the oxygen-dependent quenching of the phosphorescence of albumin-bound palladium meso-tetra(4-carboxyphenyl)porphyrin, and can be used to measure microvascular as well as interstitial pO2. In addition, the two methods can be used sequentially to measure both pH and pO2 in the same tissues.

Hydrothermal synthesis and photoluminescent properties of hierarchical GdPO4·H2O:Ln3+ (Ln3+ = Eu3+, Ce3+, Tb3+) flower-like clusters

Science.gov (United States)

Amurisana, Bao.; Zhiqiang, Song.; Haschaolu, O.; Yi, Chen; Tegus, O.

2018-02-01

3D hierarchical GdPO4·H2O:Ln3+ (Ln3+ = Eu3+, Ce3+, Tb3+) flower clusters were successfully prepared on glass slide substrate by a simple, economical hydrothermal process with the assistance of disodium ethylenediaminetetraacetic acid (Na2H2L, where L4- = (CH2COO)2N(CH2)2N(CH2COO)24-). In this process, Na2H2L was used as both a chelating agent and a structure-director. The hierarchical flower clusters have an average diameter of 7-12 μm and are composed of well-aligned microrods. The influence of the molar ratio of Na2H2L/Gd3+ and reaction time on the morphology was systematically studied. A possible crystal growth and formation mechanism of hierarchical flower clusters is proposed based on the evolution of morphology as a function of reaction time. The self-assembled GdPO4·H2O:Ln3+ superstructures exhibit strong orange-red (Eu3+, 5D0 → 7F1), green (Tb3+, 5D4 → 7F5) and near ultraviolet emissions (Ce3+, 5d → 7F5/2) under ultraviolet excitation, respectively. This study may provide a new channel for building hierarchically superstructued oxide micro/nanomaterials with optical and new properties.

Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst

International Nuclear Information System (INIS)

Adamiak, Joanna; Kalinowska-Alichnewicz, Dorota; Szadkowski, Michal; Skupinski, Wincenty

2011-01-01

Highlights: → A novel catalyst H 3 PO 4 /MoO 3 /SiO 2 was characterized and used in nitration. → On the surface domains of phosphomolybdic acid (HPM) are obtained. → Dinitrotoluene is obtained with very high yield i.e. 96 wt.% in mild conditions. → Dinitrochlorobenzene is obtained with only twelve-fold excess of nitric acid. → It is sulfuric acid free and solvent free nitration of aromatic compounds. - Abstract: A new catalyst, H 3 PO 4 /MoO 3 /SiO 2 , was prepared by modification of MoO 3 /SiO 2 using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds.

Batagayite, CaZn2(Zn,Cu)6(PO4)4(PO3OH)3·12H2O, a new phosphate mineral from Këster tin deposit (Yakutia, Russia): occurrence and crystal structure

Science.gov (United States)

Yakovenchuk, Victor N.; Pakhomovsky, Yakov A.; Konopleva, Nataliya G.; Panikorovskii, Taras L.; Bazai, Ayya; Mikhailova, Julia A.; Bocharov, Vladimir N.; Ivanyuk, Gregory Yu.; Krivovichev, Sergey V.

2017-12-01

Batagayite, CaZn2(Zn,Cu)6(PO4)4(PO3OH)3·12H2O, is a new secondary phosphate mineral from the Këster deposit, Arga-Ynnykh-Khai massif, NE Yakutia, Russia. It is monoclinic, P21, a = 8.4264(4), b = 12.8309(6), c = 14.6928(9) Å, β = 98.514(6)o, V = 1571.05(15) Å3 and Z = 2 (from single-crystal X-ray diffraction data). Batagayite crystals are blades up to 2 mm long, flattened on {001} and elongated on [100]; blades often grow in radial aggregates. Associated minerals are arsenolite, native copper, epifanovite, fluorapatite, libethenite, Na-analogue of batagayite, pseudomalachite, quartz, sampleite, tobermorite, and Mg-analogue of hopeite. The streak is white and the luster is vitreous. The mineral is brittle and has a perfect cleavage on {001}, no parting was observed. The Mohs hardness is 3. Density, determined by the float-sink method in Clerici solution, is 2.90(3) g/cm3, and the calculated density is 3.02 g/cm3 (using the empirical formula and single-crystal unit-cell parameters). Batagayite is biaxial, optically negative, α = 1.566 ± 0.002, β = 1.572 ± 0.002, γ = 1.573 ± 0.002 at 589 nm. 2V meas. = 40(5)°, 2V calc = 44.3°. Optical orientation: Z is perpendicular to (001), further details unclear. No dispersion or pleochroism were observed. The mean chemical composition determined by electron microprobe is: Na2O 0.31, MgO 1.39, Al2O3 0.55, SiO2 0.48, P2O5 34.37, K2O 0.17, CaO 2.76, MnO 1.03, CuO 5.80, ZnO 35.62, CdO 0.24 wt%. The H2O content estimated from the crystal-structure refinement is 16.83 wt%, giving a total of 99.55 wt%. The empirical formula calculated on the basis of P + Si = 7 is (Zn6.22Cu1.04Ca0.70Mg0.49Mn0.21Al0.15Na0.14K0.05Cd0.03)Σ9.03(P6.89Si0.11)Σ7.00O24.91(OH)3.09·12.10H2O. The mineral easily dissolves in 10% room-temperature HCl. The eight diagnostic lines in the X-ray powder-diffraction pattern are (I-d[Å]-hkl): 100-14.59-001, 25-6.34-012, 11-6.02-111, 37-4.864-003, 13-4.766-112, 20-3.102-1 \\overline {2} \\overline {4} , 11-2.678-2

Superprotonic KH(PO3H)-SiO2 composite electrolyte for intermediate temperature fuel cells

NARCIS (Netherlands)

Bandarenka, A.; Bondarenko, Alexander S.; Zhou, W.; Bouwmeester, Henricus J.M.

2009-01-01

Novel thin film composite electrolyte membranes, prepared by dispersion of nano-sized SiO2 particles in the solid acid compound KH(PO3H), can be operated under both oxidizing and reducing conditions. Long-term stable proton conductivity is observed at not, vert, similar140 °C, i.e., slightly above

New crystals of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O system

Energy Technology Data Exchange (ETDEWEB)

Makarova, I. P., E-mail: makarova@crys.ras.ru; Grebenev, V. V.; Komornikov, V. A.; Selezneva, E. V. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation)

2016-11-15

Cs{sub 6}H(HSO{sub 4}){sub 3}(H{sub 2}PO{sub 4}){sub 4} crystals, grown for the first time based on an analysis of the phase diagram of the CsHSO{sub 4}–CsH{sub 2}PO{sub 4}–H{sub 2}O ternary system, have been investigated by structural analysis using synchrotron radiation. The atomic structure of the crystals is determined and its specific features are analyzed.

Preparation and characterization of activated carbon from reedy grass leaves by chemical activation with H{sub 3}PO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Xu, Jianzhong, E-mail: xjz8112@sina.com [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Chen, Lingzhi [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Department of Applied Chemistry, Hengshui University, Hengshui 053000, Hebei (China); Qu, Hongqiang; Jiao, Yunhong; Xie, Jixing [College of Chemistry and Environmental Science, Hebei University, Baoding 071002, Hebei (China); Xing, Guangen [Department of Applied Chemistry, Hengshui University, Hengshui 053000, Hebei (China)

2014-11-30

Highlights: • Activated carbons were produced from reedy grass leaves by activation with phosphoric acid. • The activated carbons have a large number of oxygen- and phosphorus-containing surface groups. • The structure of activated carbons was bight fibers features on the surface and the external surface of the activated carbons was slightly corrugated and abundant pores. - Abstract: Activated carbons were produced from reedy grass leaves by chemical activation with H{sub 3}PO{sub 4} in N{sub 2} atmosphere and their characteristics were investigated. The effects of activation temperature and time were examined. Adsorption capacity was demonstrated with BET and iodine number. Micropore volume and pore size distribution of activated carbons were characterized by N{sub 2} adsorption isotherms. The surface area and iodine number of the activated carbons produced at 500 °C for 2 h were 1474 m{sup 2}/g and 1128 mg/g, respectively. Thermal decomposition of pure reedy grass leaves and H{sub 3}PO{sub 4}-impregnated reedy grass leaves have been investigated with thermogravimetric/mass spectroscopy (TG–MS) technique. It was found that the temperature and intensity of maximum evolution of H{sub 2}O and CO{sub 2} of H{sub 3}PO{sub 4}-impregnated reedy grass leaves were lower than that of pure reedy grass leaves. This implies that H{sub 3}PO{sub 4} as an activating reagent changed the thermal degradation of the reedy grass leaves, stabilized the cellulose structure, leading to a subsequent change in the evolution of porosity. The results of X-ray photoelectron spectroscopy and Fourier-infrared spectroscopy analysis indicate that the produced activated carbons have rich functional groups on surface.

Crystal structure of Na3Sc2(PO4)3 at 60 deg C

International Nuclear Information System (INIS)

Lazoryak, B.I.; Kalinin, V.B.; Stefanovich, S.Yu.; Efremov, V.A.

1980-01-01

The structure of the ferroelectric phase of Na 3 Sc 2 (PO 4 ) 3 compound was studied. Na 3 Sc 2 (PO 4 ) 3 monocrystal heated by a jet of warm N 2 was investigated at 60 deg C. The rhombohedron modification was determined: a=8.927(3), c=22.34(4) A, Z=6, space group R anti 3c. Interatomic distances and inner angles of polyhedrons in Na 3 Sc 2 (PO 4 ) 3 structure were determined

Hydrothermal synthesis and crystal structure of CsFe23(HPO4)2(PO4)(H2O)

International Nuclear Information System (INIS)

Anisimova, N.Yu.; Ilyukhin, A.B.; Chudinova, N.N.; Serafin, M.

2001-01-01

The double acid iron-cesium orthophosphate CsFe 2 3 (HPO 4 ) 2 (PO 4 )(H 2 O) was prepared by hydrothermal synthesis (from the Fe 2 O 3 , Cs 2 CO 3 and H 3 PO 4 mixture at 290 Deg C during 1 h following by cooling to 25 Deg C). Its crystal structure (a = 5.021(3), b = 15.80(1), c = 13.646(8), β 94.49(4) Deg, sp. gr. P2 1 /n, Z = 4) was analyzed by X-ray diffraction. The structure is formed by the orthophosphate tetrahedrons and the FeO 6 octahedrons, the water molecule is coordinated by the iron atom [ru

H3PO4 imbibed polyacrylamide-graft-chitosan frameworks for high-temperature proton exchange membranes

Science.gov (United States)

Yuan, Shuangshuang; Tang, Qunwei; He, Benlin; Chen, Haiyan; Li, Qinghua; Ma, Chunqing; Jin, Suyue; Liu, Zhichao

2014-03-01

Proton exchange membrane (PEM), transferring protons from anode to cathode, is a key component in a PEM fuel cell. In the current work, a new class of PEMs are synthesized benefiting from the imbibition behavior of three-dimensional (3D) polyacrylamide-graft-chitosan (PAAm-graft-chitosan) frameworks to H3PO4 aqueous solution. Interconnected 3D framework of PAAm-graft-chitosan provides tremendous space for holding proton-conducting H3PO4. The highest anhydrous proton conductivity of 0.13 S cm-1 at 165 °C is obtained. A fuel cell using a thick membrane as a PEM showed a peak power density of 405 mW cm-2 with O2 and H2 as the oxidant and fuel, respectively. Results indicate that the interconnected 3D framework provides superhighway for proton conduction. The valued merits on anhydrous proton conductivity, huge H3PO4 loading, and easy synthesis promise the new membranes to be good alternatives as high-temperature PEMs.

Synthesis and crystal structure of the solid solution Co3(SeO3)3-x(PO3OH)x(H2O) involving crystallographic split positions of Se4+ and P5+.

Science.gov (United States)

Zimmermann, Iwan; Johnsson, Mats

2013-10-21

Three new cobalt selenite hydroxo-phosphates laying in the solid solution Co3(SeO3)3-x(PO3OH)x(H2O), with x = 0.8, x = 1.0, and x = 1.2 are reported. Single crystals were obtained by hydrothermal synthesis and the crystal structure was determined by single crystal X-ray diffraction. The structure can be described as a 3D framework having selenite and hydroxo-phosphate groups protruding into channels in the crystal structure. Se(4+) and P(5+) share a split position in the structure so that either SeO3 groups having a stereochemically active lone pair or tetrahedrally coordinated PO3OH groups are present. The OH-group is thus only present when the split position is occupied by P(5+). The crystal water is coordinated to a cobalt atom and TG and IR measurements show that the water and hydroxyl groups leave the structure at unusually high temperatures (>450 °C). Magnetic susceptibility measurements show antiferromagnetic coupling below 16 K and a magnetic moment of 4.02(3) μB per Co atom was observed.

Study on the Visible-Light Photocatalytic Performance and Degradation Mechanism of Diclofenac Sodium under the System of Hetero-Structural CuBi2O4/Ag3PO4 with H2O2

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Xiaojuan Chen

2018-03-01

Full Text Available Two kinds of CuBi2O4/Ag3PO4 with different heterojunction structures were prepared based on the combination of hydrothermal and in-situ precipitation methods with surfactant additives (sodium citrate and sodium stearate, and their characteristics were systematically resolved by X-ray Diffraction (XRD, Brunauer–Emmett–Teller (BET, X-ray Photoelectron Spectroscopy (XPS, Scanning Electron Microscope (SEM/ High-resolution Transmission Electron Microscopy (HRTEM, UV-vis Diffuse Reflectance Spectra (DRS and Photoluminescence (PL. Meanwhile, the photocatalytic properties of the catalysts were determined for diclofenac sodium (DS degradation and the photocatalytic mechanism was also explored. The results indicate that both of the two kinds of CuBi2O4/Ag3PO4 exhibit higher photocatalytic efficiency, mineralization rate, and stability than that of pure CuBi2O4 or Ag3PO4. Moreover, the catalytic activity of CuBi2O4/Ag3PO4 can be further enhanced by adding H2O2. The free radical capture experiments show that in the pure CuBi2O4/Ag3PO4 photocatalytic system, the OH• and O2•− are the main species participating in DS degradation; however, in the CuBi2O4/Ag3PO4 photocatalytic system with H2O2, all OH•, h+, and O2•− take part in the DS degradation, and the contribution order is OH• > h+ > O2•−. Accordingly, the photocatalytic mechanism of CuBi2O4/Ag3PO4 could be explained by the Z-Scheme theory, while the catalysis of CuBi2O4/Ag3PO4 with H2O2 follows the heterojunction energy band theory.

H3PO4/Al2O3 catalysts: characterization and catalytic evaluation of oleic acid conversion to biofuels and biolubricant

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Lucia Regina Raddi de Araujo

2006-06-01

Full Text Available Al2O3 and H3PO4/Al2O3 catalysts were investigated in the conversion of oleic acid to biofuels and biolubricant at 1 atm and at 623 K. The catalytic tests were performed in a fixed bed and continuous flow reactor, using an oleic acid-catalyst ratio of 4 and N2 as the carrier gas. The reaction products were analyzed by gas chromatography and acidity measurements. N2 adsorption-desorption, X ray diffraction, 31P nuclear magnetic resonance and FT-IR spectroscopy were also employed to evaluate the textural, structural and acidic properties of the catalysts. The results showed that phosphoric acid impregnation improved the alumina decarboxylation activities, generating hydrocarbons in the range of gasoline, diesel oil and lubricant oil. The best catalytic performance was achieved with the highest surface area alumina impregnated with H3PO4, which was the solid that allied high total acidity with a large quantity of mesopores.

Room temperature metathetic synthesis and characterization of α-hopeite, Zn3(PO4)2.4H2O

International Nuclear Information System (INIS)

Parhi, Purnendu; Manivannan, V.; Kohli, Sandeep; McCurdy, Patrick

2008-01-01

The synthesis of crystalline zinc phosphates (α-hopeite phase) through the metathetic pathway has been investigated. The reaction has been carried out by room-temperature grinding. High lattice energy of the by-product NaCl has driven the reaction in the forward direction, and as a result, stable phosphate phases have been synthesized. Reaction of a different phosphorus source (like Na 3 PO 4 , Na 2 HPO 4 , NaH 2 PO 4 , and K 2 HPO 4 ) with ZnCl 2 has been attempted. The structural, vibrational, thermal, optical, and chemical properties of synthesized powders are determined by powder X-ray diffraction (XRD), scanning electron microscope (SEM), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and diffused reflectance spectra (DR) in the UV-vis range. The direct band gap of the title compound was determined to be 3.6 ± 0.2 eV

Topotactic insertion of lithium in the layered structure Li4VO(PO4)2: The tunnel structure Li5VO(PO4)2

International Nuclear Information System (INIS)

Satya Kishore, M.; Pralong, V.; Caignaert, V.; Malo, S.; Hebert, S.; Varadaraju, U.V.; Raveau, B.

2008-01-01

A new V(III) lithium phosphate Li 5 VO(PO 4 ) 2 has been synthesized by electrochemical insertion of lithium into Li 4 VO(PO 4 ) 2 . This phase, which crystallizes in the space group I4/mcm, exhibits a tunnel structure closely related to the layered structure of Li 4 VO(PO 4 ) 2 and to the tunnel structure of VO(H 2 PO 4 ) 2 . The topotactic reactions that take place during lithium exchange and intercalation, starting from VO(H 2 PO 4 ) 2 and going to the final phase Li 5 VO(PO 4 ) 2 are explained on the basis of the flexible coordinations of V 4+ and V 3+ species. The electrochemical and magnetic properties of this new phase are also presented and explained on the basis of the structure dimensionality. - Graphical abstract: Electrochemical synthesis of a new 3D V(III) lithium phosphate, Li 5 VO(PO 4 ) 2 . Starting from the 2D Li 4 VO(PO 4 ) 2 , the topotactic reaction that take place during lithium intercalation is explained on the basis of the flexible coordinations of V 4+ and V 3+ species

PEG1000-Based Dicationic Acidic Ionic Liquid Catalyzed One-Pot Synthesis of 4-Aryl-3-Methyl-1-Phenyl-1H-Benzo[h]pyrazolo [3,4-b]quinoline-5,10-Diones via Multicomponent Reactions

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Yi-Ming Ren

2015-09-01

Full Text Available A novel and green approach for efficient and rapid synthesis of 4-aryl-3-methyl-1-phenyl-1H-benzo[h]pyrazolo[3,4-b]quinoline-5,10-diones has been accomplished by the one-pot condensation reaction of aromatic aldehydes, 3-methyl-1-phenyl-1H-pyrazol-5-amine and 2-hydroxynaphthalene-1,4-dione using PEG1000-based dicationic acidic ionic liquid (PEG1000-DAIL as a catalyst was reported. Recycling studies have shown that the PEG1000-DAIL can be readily recovered and reused several times without significant loss of activity. The key advantages are the short reaction time, high yields, simple workup, and recovered catalyst.

CINETIQUE DES IONS PHOSPHORIQUES H2PO4- ET HPO4-2 EN MILIEU GYPSEUX

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Hacène BOUZIANE

2011-06-01

Full Text Available L’étude de la fixation des ions H2PO4- et HPO4-2 par les divers types de gypse (tassé ; feuilleté ; fibreux. Donne une réaction positive quelle que soit la solution phosphaté et le type de gypse utilisé. Il convient de noter que l’adsorption est beaucoup plus forte pour les ions H2PO4- que celle des ions HPO4-2 et qu’elle varie d’un type de gypse à l’autre.                 L’étude de l’influence du temps, de la granulométrie et de la concentration des solutions montrent en effet que : plus le diamètre du grain est petit, plus l’adsorption est forte. La fixation se produit même pour une solution phosphatée à très faible concentration ; il se produit toujours une réaction avec précipitation et non un équilibre d’adsorption. La réaction des ions phosphatés augment rapidement dans les premières minutes quel que soit le type de gypse et la concentration utilisée. Nous avons abouti à la formation d’un gel phosphaté, visqueux et non soluble. L’analyse chimique de ce gel donne les résultats suivants : PO4=54,20% ,Ca=11,30% , K=32,94%; si l’on compare ces résultats avec les résultats calculés pour K3CaH,(PO42=PO4=54,59%, Ca=11,19%, K=33,62%, nos valeurs sont très voisines de celles-ci. Il s’agit donc du même sel sur lequel aucun travail sur la formation de K3CaH(PO42 à partir de CaSO42H2O ne semble avoir été publié.

Ternary phosphates in Ca3(PO4)2-Na3Ln(PO4)2 (Ln-Nd, Eu, Er) systems

International Nuclear Information System (INIS)

Lazoryak, B.I.; Ivanov, L.N.; Strunenkova, T.V.; Golubev, V.N.; Viting, B.N.

1990-01-01

Ternary phosphates, formed in Ca 3 (PO 4 ) 2 -Na 3 Ln(PO 4 ) 2 (Ln-Nd, Eu, Er) systems were investigated by the methods of X-ray phase, luminescent analyses and IR spectroscopy. 5 regions of homogeneity were found. Two of them (I and II) were distinguished for all systems. Samples in the region of up to 14.285 mol.% Na 3 Ln(PO 4 ) 2 crystallize on the basis of β-Ca 3 (PO 4 ) 2 structure, and in other homogeneity regions - on the basis of β-K 2 SO 4 structure

Bacterial biofilm formation versus mammalian cell growth on titanium-based mono- and bi-functional coating

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G Subbiahdoss

2010-05-01

Full Text Available Biomaterials-associated-infections (BAI are serious complications in modern medicine. Although non-adhesive coatings, like polymer-brush coatings, have been shown to prevent bacterial adhesion, they do not support cell growth. Bi-functional coatings are supposed to prevent biofilm formation while supporting tissue integration. Here, bacterial and cellular responses to poly(ethylene glycol (PEG brush-coatings on titanium oxide presenting the integrin-active peptide RGD (arginine-glycine-aspartic acid (bioactive “PEG-RGD” were compared to mono-functional PEG brush-coatings (biopassive “PEG” and bare titanium oxide (TiO2 surfaces under flow. Staphylococcus epidermidis ATCC 35983 was deposited on the surfaces under a shear rate of 11 s-1 for 2 h followed by seeding of U2OS osteoblasts. Subsequently, both S. epidermidis and U2OS cells were grown simultaneously on the surfaces for 48 h under low shear (0.14 s-1. After 2 h, staphylococcal adhesion was reduced to 3.6±1.8 × 103 and 6.0±3.9 × 103 cm-2 on PEG and PEG-RGD coatings respectively, compared to 1.3±0.4 × 105 cm-2 for the TiO2 surface. When allowed to grow for 48 h, biofilms formed on all surfaces. However, biofilms detached from the PEG and PEG-RGD coatings when exposed to an elevated shear (5.6 s-1 U2OS cells neither adhered nor spread on PEG brush-coatings, regardless of the presence of biofilm. In contrast, in the presence of biofilm, U2OS cells adhered and spread on PEG-RGD coatings with a significantly higher surface coverage than on bare TiO2. The detachment of biofilm and the high cell surface coverage revealed the potential significance of PEG-RGD coatings in the context of the “race for the surface” between bacteria and mammalian cells.

Co-hydrothermal synthesis of LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C nano-hybrid cathode material with enhanced electrochemical performance for lithium-ion batteries

International Nuclear Information System (INIS)

Zhang, Jun; Luo, Shaohua; Chang, Longjiao; Hao, Aimin; Wang, Zhiyuan; Liu, Yanguo; Xu, Qian; Wang, Qing; Zhang, Yahui

2017-01-01

Highlights: • A co-hydrothermal approach to synthesize LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C composite material in water/PEG system is present. • The Mn_1_-_xMg_xPO_4 precursor is prepared by precipitation reaction. • Co-modified with Mg"2"+ doping and LiAlO_2 compositing strategies play an important role in improving the electronic conductivity and facilitating the diffusion of lithium ion. • LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C composite material exhibits a high specific discharge capacity of 151.8 mAh/g at 0.05C. - Abstract: LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C is synthesized by a co-hydrothermal method in water/PEG system using Li_2CO_3, AAO and Mn_1_-_xMg_xPO_4 as raw material. The electronic structure and micromorphology of multi-component compound LiMn_1_-_xMg_xPO_4/C (x = 0, 1/24, 1/12, 1/6) and nano-hybrid LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C cathode materials are studied by first-principles calculation and experimental research including XRD, SEM, TEM. The calculated band gap of LiMn_2_3_/_2_4Mg_1_/_2_4PO_4/C is 2.296 eV, which is lower than other percentages Mg"2"+ doping samples. Electrochemical tests exhibit LiMn_2_3_/_2_4Mg_1_/_2_4PO_4/C has better cycling performance and rate capability than other contents Mg"2"+ doping samples with the discharge capacity of 143.5 mAh/g, 141.5 mAh/g, 139.2 mAh/g and 136.3 mAh/g at 0.05C, 0.1C, 0.5C and 1C in order. After compositing and preparation of LiMn_2_3_/_2_4Mg_1_/_2_4PO_4·LiAlO_2/C composite material by co-hydrothermal route, the initial discharge capacity reaches up to 151.8 mAh/g, which suggests that co-modified with Mg"2"+ doping and LiAlO_2 compositing material can improve the electronic conductivity of LiMnPO_4/C by facilitating the lithium ion diffusion rate in the interior of the materials.

21 CFR 862.1120 - Blood gases (PCO2, PO2) and blood pH test system.

Science.gov (United States)

2010-04-01

... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Blood gases (PCO2, PO2) and blood pH test system... Test Systems § 862.1120 Blood gases (PCO2, PO2) and blood pH test system. (a) Identification. A blood gases (PCO2, PO2) and blood pH test system is a device intended to measure certain gases in blood, serum...

Resolution of the mixture TBP-H2 MPB-HDB-PH3PO4

International Nuclear Information System (INIS)

Pires, M.A.F.; Abrao, A.

1980-01-01

Tributylphosphate (TBP) is presently the most used extractant for uranium, thorium and zirconium technologies, both for the purification of these elements from their concentrates and for the recovery of heavy metals in the reprocessing of irradiated fuels. Nevertheless, in the presence of phosphoric acid, some degradation products are formed, such as: di-n-butylphosphoric acid (HDBP), monobutylphosphoric ancd (H 2 MBP) and ortophosphoric acid. The accumulation of these degradation products in the organic phase of the liquid-liquid extraction processes is highly undesirable. In order to avoid this problem, the separation of the mixture HDBP, H 2 MBP and H 3 PO 4 in TBP-dilutent or TBP-diluent-uranyl, thorium of zirconyl nitrate was then studied. Several separation techniques were investigated: adsorption using a cationic resin saturated with U(VI), chromatogtraphy in macroporous polymers, chromatography in alumina columns. Refractive index and condutimetric measurements were carried out to follow up the separation processes. The best results were obtained in an alumina column. (C.L.B.) [pt

A functionalized phosphonate-rich organosilica layered hybrid material (PSLM) fabricated through a mild process for heavy metal uptake

Energy Technology Data Exchange (ETDEWEB)

Daikopoulos, Chris [Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110 (Greece); Bourlinos, Athanasios B. [Institute of Materials Science, NCSR “Demokritos”, Ag. Paraskevi Attikis, Athens 15310 (Greece); Georgiou, Yiannis [Laboratory of Physical Chemistry, Department of Environmental and Natural Resources Management, University of Patras, Seferi 2, Agrinio 30100 (Greece); Deligiannakis, Yiannis, E-mail: ideligia@cc.uoi.gr [Laboratory of Physical Chemistry, Department of Environmental and Natural Resources Management, University of Patras, Seferi 2, Agrinio 30100 (Greece); Zboril, Radek [Regional Centre of Advanced Technologies and Materials, Faculty of Science, Department of Physical Chemistry and Experimental Physics, Palacky University, Olomouc 77146 (Czech Republic); Karakassides, Michael A. [Department of Materials Science and Engineering, University of Ioannina, Ioannina 45110 (Greece)

2014-04-01

Highlights: • Novel phosphonate-rich organosilica layered hybrid material (PSLM) fabricated through a mild xerogel process. • Surface Complexation Modeling reveals that PSLM bears 2 types of functional groups able to bind heavy metal. • Maximum metal uptake capacities were found 2.72 mmol g{sup −1} for Cu{sup 2+}, 1.67 mmol g{sup −1} for Pb{sup 2+} and 1.00 mmol g{sup −1} for Cd{sup 2+} at pH 7. • EPR spectroscopy reveals local coordination environment for Cu{sup 2+} ions. - Abstract: A phosphonate-rich organosilica layered hybrid material (PSLM) made of 3-(trihydroxysilyl)propyl methylphosphonate, monosodium salt, as the single silica source, has been obtained from its aqueous solution through a xerogel process and mild thermal aging. The method is simple, affording bulk quantities of powdered PSLM in a single-step. The hybrid is stable in water and possesses a high content of phosphonate groups fixed on the solid matrix. In addition, PSLM shows good thermal stability, which exceeds 300 °C in air. The material was characterized using SEM, TEM, XRD, FT-IR and TGA techniques. Potentiometric titrations show that PSLM bears high-surface density of phosphonate groups (3 mmol g{sup −1}). As a result, the material displays high metal uptake capacity for heavy metal ions such as Cu{sup 2+} (2.72 mmol g{sup −1}), Pb{sup 2+} (1.67 mmol g{sup −1}) and Cd{sup 2+} (1.00 mmol g{sup −1}) at neutral pH values e.g. the pH of natural waters. Detailed theoretical modeling using a Surface Complexation Model combined with Electron Paramagnetic Resonance (EPR) spectroscopy shows that the surface distribution of surface bound Cu{sup 2+} ions is rather homogeneous e.g. copper-binding phosphonate sites are arranged in average distances 5–8 Å.

(Liquid + liquid) equilibrium of (NaNO{sub 3} + PEG 4000 + H{sub 2}O) ternary system at different temperatures

Energy Technology Data Exchange (ETDEWEB)

Jimenez, Yecid P. [Departamento de Ingenieria Quimica, Universidad de Antofagasta, CICITEM (Chile); Galleguillos, Hector R., E-mail: hgalleguillos@uantof.cl [Departamento de Ingenieria Quimica, Universidad de Antofagasta, CICITEM (Chile)

2011-11-15

Highlights: > LLE data for the ATPS NaNO{sub 3} + PEG 4000 were determined at T = (288.15 and 308.15) K. > The experimental data shown that the temperature increases as STL and biphasic area increase. > The Chen-NRTL, modified Wilson and UNIQUAC models were used to correlate the experimental tie-line data. > The results show that the quality of fitting is better with the UNIQUAC model. - Abstract: Phase diagram and (liquid + liquid) equilibrium (LLE) data for the (NaNO{sub 3} + polyethylene glycol 4000 (PEG 4000) + H{sub 2}O) system have been determined experimentally at T = (288.15 and 308.15) K. The effects of temperature on the binodal curves and tie-lines have been studied and it was found that an increasing in temperature caused the expansion of two-phase region. The Chen-NRTL, modified Wilson and UNIQUAC models were used to correlate the experimental tie-line data. The results show that the quality of fitting is better with the UNIQUAC model.

Separative recovery with lime of phosphate and fluoride from an acidic effluent containing H3PO4, HF and/or H2SiF6.

Science.gov (United States)

Gouider, Mbarka; Feki, Mongi; Sayadi, Sami

2009-10-30

Fluoride content and flow-rate of fertilizer plant wastewater from phosphoric acid and/or triple superphosphate (TSP) production lead to the discharge of several thousand tons of fluoride (F(-)) per year and even more for phosphate (PO4(3-)). Since sustainability is an important environmental concern, the removal methods should allow phosphorus and fluoride to be recycled as a sustainable products for use as raw materials either in agricultural or industrial applications. In the present work, separative recovery with lime of these two target species was investigated. A preliminary speciation study, carried out on the crude effluent, showed that two forms of fluoride: HF and H2SiF6 are present in a highly acidic medium (pH approximately 2). Evidence that fluoride is present under both free (HF) and combined (H2SiF6) forms, in the phosphate-containing effluent, was provided by comparing potentiometric titration curves of a crude wastewater sample and synthetic acid mixtures containing H3PO4, HF and H2SiF6. In a second step synthetic effluent containing mixtures of the following acids: HF, H2SiF6 and H3PO4, were treated with lime. The behaviour of these compounds under lime treatment was analysed. The data showed that fluoride has a beneficial effect on phosphate removal. Moreover, by acting on the precipitation pH, a "selective" recovery of fluoride and phosphate ions was possible either from phosphoric acid/hydrofluoric acid or phosphoric acid/hexafluorosilicic acid mixtures. Indeed, the first stage of the separative recovery, led to a fluoride removal efficiency of 97-98% from phosphoric acid/hydrofluoric acid mixture. It was of 93-95% from phosphoric acid/hexafluorosilicic acid mixture. During the second stage, the phosphate precipitation reached 99.8% from both acidic mixtures whereas it did not exceed 82% from a solution containing H3PO4 alone. The XRD and IR analyses showed that during lime treatment, a H2SiF6 hydrolysis occurred, instead of CaSiF6 solid

Electrochemical behaviours of Eu(III/E(II and Ce(IV/Ce(III in H3PO4-H2O media : solvation and complexation reactions

Directory of Open Access Journals (Sweden)

Belqat B.

2018-01-01

Full Text Available Many kinds of rare earth elements (REE such as europium and cerium have been make them essential elements in many high-tech components. The electrochemical studies can be presented as an interesting indication for europium and cerium extraction from phosphoric solutions, including solvation and complexation reactions. The normal redox potentials of Eu3+/Eu2+ and Ce4+/Ce3+ systems have been determined in H3PO4-H2O media with various phosphoric acid concentration. The solvation of these elements in phosphoric media is characterized by their transfer activity coefficients "f" calculated from the corresponding normal redox potentials. The corresponding solvation increases with increasing the H3PO4 concentration. For each REE, the electrochemical properties depend on its number of charges and on its basic properties. Results suggest that solvation and complexation of REE phosphates are important in controlling REE concentration.

Equilibrium diagram of KPO3-Y(PO3)3 system, chemical preparation and characterization of KY(PO3)4

International Nuclear Information System (INIS)

Jouini, Anis; Ferid, Mokhtar; Trabelsi-Ayadi, Malika

2003-01-01

Microdifferential thermal analysis (μ-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO 3 -Y(PO 3 ) 3 system. The only compound observed within the system was KY(PO 3 ) 4 melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO 3 ) 3 at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO 3 was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO 3 ) 4 polyphosphate has the P2 1 space group with lattice parameters: a=7.183(4) A, b=8.351(6) A, c=7.983(3) A, β=91.75(3) deg. and Z=2 is isostructural with KNd(PO 3 ) 4 . The second allotropic form of KY(PO 3 ) 4 belongs to the P2 1 /n space group with lattice parameters: a=10.835(3) A, b=9.003(2) A, c=10.314(1) A, β=106.09(7) deg. and Z=4 and is isostructural with TlNd(PO 3 ) 4 . The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP 4 O 12 crystallizes in the C2/c space group with lattice parameters: a=7.825(3) A, b=12.537(4) A, c=10.584(2) A, β=110.22(7) deg. and Z=4 is isostructural with RbNdP 4 O 12 and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported

Reactions of acetylenes with hypophosphorous and phosphonous acids

International Nuclear Information System (INIS)

Nifant'ev, E.E.; Solovetskaya, L.A.; Maslennikova, V.I.; Magdeeva, R.K.; Sergeev, N.M.

1986-01-01

Alkenylphosphonous, alkenylphosphinic, and alkylenebisphosphinic acids were prepared for the first time. The course of the hydrophosphorylation of 1-alkynes depends on the form of the reagent used. The homolytic hydrophosphorylation of acetylenes with hypophosphorous acid proceeds mainly with the participation of one molecule of the acid. The addition of phosphonous acids to acetylenic hydrocarbons leads to both mono- and di-phosphorylated adducts. The nature of the phosphonous acid taken has a substantial influence on the readiness with which the alkylenebisphosphinic acids are formed. Study of the stereoselectivity of the reactions showed that in the case of the monoaddition of hypophosphorous and phosphonous acids to acetylenes mixtures of cis and trans isomeric products are always formed. Phosphorous 31 and carbon 13 NMR spectra are analyzed

Synthesis, crystal structure, optical and thermal properties of lanthanide hydrogen-polyphosphates Ln[H(PO3)4] (Ln = Tb, Dy, Ho).

Science.gov (United States)

Förg, Katharina; Höppe, Henning A

2015-11-28

Lanthanide hydrogen-polyphosphates Ln[H(PO3)4] (Ln = Tb, Dy, Ho) were synthesised as colourless (Ln = Tb, Dy) and light pink (Ln = Ho) crystalline powders by reaction of Tb4O7/Dy2O3/Ho2O3 with H3PO3 at 380 °C. All compounds crystallise isotypically (P2(1)/c (no. 14), Z = 4, a(Tb) = 1368.24(4) pm, b(Tb) = 710.42(2) pm, c(Tb) = 965.79(3) pm, β(Tb) = 101.200(1)°, 3112 data, 160 parameters, wR2 = 0.062, a(Ho) = 1363.34(5) pm, b(Ho) = 709.24(3) pm, c(Ho) = 959.07(4) pm, β(Ho) = 101.055(1)°, 1607 data, 158 parameters, wR2 = 0.058). The crystal structure comprises two different infinite helical chains of corner-sharing phosphate tetrahedra. In-between these chains the lanthanide ions are located, coordinated by seven oxygen atoms belonging to four different polyphosphate chains. Vibrational, UV/Vis and fluorescence spectra of Ln[H(PO3)4] (Ln = Tb, Dy, Ho) as well as Dy[H(PO3)4]:Ln (Ln = Ce, Eu) and the magnetic and thermal behaviour of Tb[H(PO3)4] are reported.

Luminescence and energy transfer of Sm3+ and Eu3+ in Ca2PO4Cl

International Nuclear Information System (INIS)

Wang, Zhijun; Li, Panlai; Yang, Zhiping; Guo, Qinglin

2014-01-01

Sm 3+ , Eu 3+ , and Sm 3+ –Eu 3+ doped Ca 2 PO 4 Cl phosphors are synthesized by a solid-state method. Ca 2 PO 4 Cl:Sm 3+ can produce red emission under the 400 nm radiation excitation, and the emission peak is located at 601 nm, which is assigned to the 4 G 5/2 → 6 H 7/2 transition of Sm 3+ . Ca 2 PO 4 Cl:Eu 3+ can create red emission under the 392 nm radiation excitation, and the strongest peak is located at 620 nm, which is attributed to the 5 D 0 → 7 F 2 transition of Eu 3+ . The energy transfer from Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl has been validated and the critical distance (R c ) of Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl is calculated to be 1.14 nm. With increasing Eu 3+ doping concentration, the energy transfer efficiency (Sm 3+ →Eu 3+ ) gradually increases to 53.7%. The luminescence property of Ca 2 PO 4 Cl:Sm 3+ , Eu 3+ can be tuned by properly tuning the relative ratio of Sm 3+ –Eu 3+ , and the emission intensity of Ca 2 PO 4 Cl:Eu 3+ can be greatly enhanced by codoped Sm 3+ . - Highlights: • Ca 2 PO 4 Cl:Sm 3+ , Eu 3+ can produce red emission under the 400 nm radiation excitation. • The energy transfer from Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl has been validated. • The critical distance of Sm 3+ to Eu 3+ in Ca 2 PO 4 Cl is calculated to be 1.14 nm

In vitro antitumour activity, safety testing and subcellular distribution of two poly[oxyethylene(aminophosphonate-co-H-phosphonate]s in Ehrlich ascites carcinoma and BALB/c 3T3 cell culture systems

Directory of Open Access Journals (Sweden)

Ani Georgieva

2016-01-01

Full Text Available Two polyphosphoesters containing anthracene-derived aminophosphonate and hydrophilic H-phosphonate repeating units, poly[oxyethylene(aminophosphonate-co-H-phosphonate]s (1 and 2, were tested for the in vitro antitumour activity on cell cultures derived from ascitic form of Ehrlich mammary adenocarcinoma by 3-(4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide (MTT-dye reduction assay. The in vitro safety testing of the copolymers was performed by BALB/c 3T3 neutral red uptake assay. A study on their uptake and subcellular distribution in non-tumourigenic and tumour cells was performed by means of fluorescence microscopy. Both copolymers showed significant antitumour activity towards Ehrlich ascites carcinoma (EAC cells. However, the in vitro safety testing revealed significant toxicity of polymer 2 to BALB/c 3T3 mouse embryo cells. In contrast, polymer 1 showed complete absence of cytotoxicity to BALB/c 3T3 cells. The fluorescent studies showed that the substances were diffusely distributed in the cytoplasm in both cell culture systems. As opposed to BALB/c 3T3 cells, in EAC cells, intense fluorescent signal was observed in the nuclei and in the perinuclear region. The tested polyphosphoesters are expected to act under physiological conditions as prodrugs of aminophosphonates.

[3H]-labelling of hydroxyethyl groups - synthesis of S-(2-hydroxy [2-3H] ethyl) glutathione and of [3H]-melphalan

International Nuclear Information System (INIS)

Verny, M.; Nicolas, C.

1988-01-01

The easy preparation of 2-bromo [1- 3 H] ethanol allows the tritium labelling of molecules bearing S- or N-hydroxyethyl groups. Thus S-(2-hydroxy [2- 3 H] ethyl) glutathione and [ 3 H]-Melphalan were synthesised with specific radioactivities of around 10 mCi/mmol (370 MBq/mmol). These values could be theoretically raised to 10 Ci/mmol (370 GBq/mmol), according to the specific activity of the labelling precursor, sodium [ 3 H] borohydride. (author)

Electric Response and Conductivity Mechanism in H3PO4‑Doped Polybenzimidazole-4N−HfO2 Nanocomposite Membranes for High Temperature Fuel Cells

International Nuclear Information System (INIS)

Nawn, Graeme; Vezzù, Keti; Bertasi, Federico; Pagot, Gioele; Pace, Giuseppe; Conti, Fosca; Negro, Enrico

2017-01-01

Relaxation and polarization phenomena of phosphoric acid-doped [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y nanocomposite membranes for high-temperature proton-exchange membrane fuel cells are studied using Dynamic Mechanical Analysis (DMA) and Broadband Electrical Spectroscopy (BES). The membranes are obtained by casting combinations of a polybenzimidazole polymer (PBI4N) with increasing amounts of hafnium oxide nanofiller, resulting in [PBI4N(HfO 2 ) x ] hybrid systems with 0 ≤ x ≤ 0.32. Phosphoric acid at varying content levels (0 ÷ 18 wt%) is used as a doping agent, giving rise to [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y membranes. DMA and BES studies lead us to determine that the electric response of the membranes is modulated by polarization phenomena and by α and β dielectric relaxation events of the polymer matrix. Additionally, the experimental results suggest that in [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y membranes the conductivity occurs owing to three conductivity pathways: two mechanisms involving inter-domain proton migration phenomena by “hopping” events; and one mechanism in which proton exchange occurs between delocalization bodies. These results highlight the significant effect of the hafnium oxide nanofiller content on the conductivity of [PBI4N(HfO 2 ) x ](H 3 PO 4 ) y where, at x ≥ 0.04, demonstrates conductivity higher (9.0 × 10 −2 S/cm) than that of pristine H 3 PO 4 -doped PBI4N (4.8 × 10 −2 S/cm) at T ≥ 155 °C.

On the effect of the Fe(2+)/Fe(3+) redox couple on oxidation of carbon in hot H3PO4

Science.gov (United States)

Dhar, H. P.; Christner, L. G.; Kush, A. K.

1986-01-01

Oxidation studies of graphite:glassy carbon composites have been carried out at 1 and 4.7 atm. pressures in conc. H3PO4 in the presence and absence of iron ions. The concentration of the acid was varied over 85-100 wt pct, and of the iron ions over 30-300 ppm; the temperature varied over 190-210 C. Unlike the effect of Fe, which has been observed to increase the corrosion of carbon in sulphuric acid, the corrosion in phosphoric acid was observed to be slightly decreased or not at all affected. This result arises because of the catalytic reduction of the oxidized surface groups of carbon by Fe(2+) ions. The catalytic reduction is possible because under the experimental conditions the redox potential of the Fe(2+)/Fe(3+) couple is lower than the open-circuit voltage of carbon.

Sol–gel synthesis and electrochemical properties of 9LiFePO4·Li3V2(PO4)3/C composite cathode material for lithium ion batteries

International Nuclear Information System (INIS)

Zhong Shengkui; Wu Ling; Liu Jiequn

2012-01-01

Highlights: ► Nano-sized 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C powders are prepared by a sol–gel method. ► Mutual doping in 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C can improve its electronic conductivity. ► The addition of Li 3 V 2 (PO 4 ) 3 can improve the ionic diffusivity of LiFePO 4 . ► LiFePO 4 , Li 3 V 2 (PO 4 ) 3 and LiFePO 4 –Li 3 V 2 (PO 4 ) 3 unit cells coexist in the composite. - Abstract: 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C composite cathode material is prepared by a sol–gel method, using ferric citrate, V 2 O 5 , Li 2 CO 3 , NH 4 H 2 PO 4 and citric acid as raw materials. The composite material is composed of the olivine LiFePO 4 and monoclinic Li 3 V 2 (PO 4 ) 3 phases. XRD results indicate that most of the iron and vanadium in the raw materials tend to form the LiFePO 4 and Li 3 V 2 (PO 4 ) 3 phases, and only small amounts of Fe and V as the dopants enter into the lattice of Li 3 V 2 (PO 4 ) 3 and LiFePO 4 , respectively. The electronic conductivity and Li + diffusion coefficient of 9LiFePO 4 ·Li 3 V 2 (PO 4 ) 3 /C are 6.615 × 10 −3 S cm −1 and ∼10 −10 cm 2 s −1 , which are three orders of magnitude and one order of magnitude larger than those of the LiFePO 4 /C, respectively. The composite material shows a first discharge specific capacity of 131.3 mAh g −1 and capacity retention of 95.1% after 200 cycles at 10 C rate. Compared with the LiFePO 4 /C, its rate capability and cycle performance are both remarkably improved.

The Influence of Lactic Acid Concentration on the Separation of Light Rare Earth Elements by Continuous Liquid-Liquid Extraction with 2-Ethylhexyl Phosphonic Acid Mono-2-ethylhexyl Ester

Science.gov (United States)

de Carvalho Gomes, Rafael; Seruff, Luciana Amaral; Scal, Maira Labanca Waineraich; Vera, Ysrael Marrero

2018-02-01

The separation of rare earth elements (REEs) using solvent extraction adding complexing agents appears to be an alternative to saponification of the extractant. We evaluated the effect of lactic acid concentration on didymium (praseodymium and neodymium) and lanthanum extraction with 2-ethylhexyl phosphonic acid mono-2-ethyl hexyl ester [HEH(EHP)] as extractant. First, we investigated in batch experiments the separation of lanthanum (La) and didymium (Pr and Nd) using McCabe-Thiele diagrams to estimate the number of extraction stages when the feed solution was or was not conditioned with lactic acid. Additionally, we conducted continuous liquid-liquid extraction experiments and evaluated the influence of lactic acid concentration on the REE extraction and separation. The tests showed that the extraction percentage of REEs and the separation factor Pr/La increased when the lactic acid concentration increased, but the didymium purity decreased. Lanthanum, praseodymium, and neodymium extraction rate were 23.0, 89.7, and 99.2 pct, respectively, with 1:1 aqueous/organic volume flow rate and feed solution doped with 0.52 mol L-1 lactic acid. The highest didymium purity reached was 92.0 pct with 0.26 mol L-1 lactic acid concentration.

Ion conductivity and phase transitions in the Na3Sc2(PO4)3 - NaGe2(PO4)3 system

International Nuclear Information System (INIS)

Nogaj, A.S.

2002-01-01

Influence of heteropolyvalent substitution on dipole ordering of sodium-scandium phosphate, as well as on ion conductivity and phase transitions in the system Na 3 Sc 2 (PO 4 ) 3 - NaGe 2 (PO 4 ) 3 , was studied using the methods of solid phase synthesis, X-ray diffraction, laser spectroscopy and measurement of electric conductivity. Boundaries of the dipole-ordered and superionic phases existence ranges in the given system were identified. It is shown that expansion of the dipole-ordered phase existence range with increase in substituent cation concentration is characteristic of the phase on the basis of α-Na 3 Sc 2 (PO 4 ) 3 [ru

Synthesis, kinetic evaluation, and utilization of a biotinylated dipeptide proline diphenyl phosphonate for the disclosure of dipeptidyl peptidase IV-like serine proteases.

Science.gov (United States)

Gilmore, Brendan F; Carson, Louise; McShane, Laura L; Quinn, Derek; Coulter, Wilson A; Walker, Brian

2006-08-18

In this study, we report on the synthesis, kinetic characterisation, and application of a novel biotinylated and active site-directed inactivator of dipeptidyl peptidase IV (DPP-IV). Thus, the dipeptide-derived proline diphenyl phosphonate NH(2)-Glu(biotinyl-PEG)-Pro(P)(OPh)(2) has been prepared by a combination of classical solution- and solid-phase methodologies and has been shown to be an irreversible inhibitor of porcine DPP-IV, exhibiting an over all second-order rate constant (k(i)/K(i)) for inhibition of 1.57 x 10(3) M(-1) min(-1). This value compares favourably with previously reported rates of inactivation of DPP-IV by dipeptides containing a P(1) proline diphenyl phosphonate grouping [B. Boduszek, J. Oleksyszyn, C.M. Kam, J. Selzler, R.E. Smith, J.C. Powers, Dipeptide phophonates as inhibitors of dipeptidyl peptidase IV, J. Med. Chem. 37 (1994) 3969-3976; B.F. Gilmore, J.F. Lynas, C.J. Scott, C. McGoohan, L. Martin, B. Walker, Dipeptide proline diphenyl phosphonates are potent, irreversible inhibitors of seprase (FAPalpha), Biochem, Biophys. Res. Commun. 346 (2006) 436-446.], thus demonstrating that the incorporation of the side-chain modified (N-biotinyl-3-(2-(2-(3-aminopropyloxy)-ethoxy)-ethoxy)-propyl) glutamic acid residue at the P(2) position is compatible with inhibitor efficacy. The utilisation of this probe for the detection of both purified dipeptidyl peptidase IV and the disclosure of a dipeptidyl peptidase IV-like activity from a clinical isolate of Porphyromonas gingivalis, using established electrophoretic and Western blotting techniques previously developed by our group, is also demonstrated.

Crystal structures and magnetic properties of iron (III)-based phosphates: Na4NiFe(PO4)3 and Na2Ni2Fe(PO4)3

International Nuclear Information System (INIS)

Essehli, Rachid; Bali, Brahim El; Benmokhtar, Said; Bouziane, Khalid; Manoun, Bouchaib; Abdalslam, Mouner Ahmed; Ehrenberg, Helmut

2011-01-01

Graphical abstract: A perspective view of the Na 2 Ni 2 Fe(PO 4 ) 3 structure along the [0 0 1] direction. Both compounds seem to exibit antiferromagnetic interactions between magnetic entities at low temperature. Display Omitted Research highlights: → Nasicon and Alluaudite compounds, Iron(III)-based phosphates, Crystal structures of Na 4 NiFe(PO 4 ) 3 and Na 2 Ni 2 Fe(PO 4 ) 3 . → Magnetism behaviours of Na 4 NiFe(PO 4 ) 3 and Na 2 Ni 2 Fe(PO 4 ) 3 . → Antiferromagnetism interactions. → Mossbauer spectroscopy. - Abstract: Crystal structures from two new phosphates Na 4 NiFe(PO 4 ) 3 (I) and Na 2 Ni 2 Fe(PO 4 ) 3 (II) have been determined by single crystal X-ray diffraction analysis. Compound (I) crystallizes in a rhombohedral system (S. G: R-3c, Z = 6, a = 8.7350(9) A, c = 21.643(4) A, R 1 = 0.041, wR 2 =0.120). Compound (II) crystallizes in a monoclinic system (S. G: C2/c, Z = 4, a = 11.729(7) A, b = 12.433(5) A, c = 6.431(2) A, β = 113.66(4) o , R 1 = 0.043, wR 2 =0.111). The three-dimensional structure of (I) is closely related to the Nasicon structural type, consisting of corner sharing [(Ni/Fe)O 6 ] octahedra and [PO 4 ] tetrahedra forming [NiFe(PO 4 ) 3 ] 4+ units which align in chains along the c-axis. The Na + cations fill up trigonal antiprismatic sites within these chains. The crystal structure of (II) belongs to the alluaudite type. Its open framework results from [Ni 2 O 10 ] units of edge-sharing [NiO 6 ] octahedra, which alternate with [FeO 6 ] octahedra that form infinite chains. Coordination of these chains yields two distinct tunnels in which site Na + . The magnetization data of compound (I) reveal antiferromagnetic (AFM) interactions by the onset of deviations from a Curie-Weiss behaviour at low temperature as confirmed by Moessbauer measurements performed at 4.2 K. The corresponding temperature dependence of the reciprocal susceptibility χ -1 follows a typical Curie-Weiss behaviour for T > 105 K. A canted AFM state is proposed for

Biological reduction-deposition and luminescent properties of nanostructured CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Yu, Xiaoniu [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Research Institute of Green Construction Materials, Southeast University, Nanjing 211189 (China); Qian, Chunxiang, E-mail: cxqian@seu.edu.cn [School of Materials Science and Engineering, Southeast University, Nanjing 211189 (China); Research Institute of Green Construction Materials, Southeast University, Nanjing 211189 (China)

2016-03-01

Nano-sized CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} with hexagonal phase have been prepared by simply varying the reactant P/Ce molar ratio in bacterial liquid. The phase composition of two samples was checked via Fourier transform infrared spectroscopy (FTIR), energy dispersive analysis of X-rays (EDS) and X-ray diffraction (XRD) analyses, displaying the presence of CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} with average crystallite size are 32.34 and 15.61 nm, respectively. The scanning electron microscopy (SEM) images show that nano-clusters and sphere-like in shape with a narrow diameter distribution were observed in two samples. The transmission electron microscopy (TEM) photographs further indicate obtained CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} nanoparticles correspond to nanosheets and nanorods, respectively. The emission spectra of CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} display a broad band of 300–380 nm range with the strongest emission at 342 nm in the violet region. - Highlights: • A new method was found to synthesize CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) and CePO{sub 4} nanoparticles. • CePO{sub 4}@NaCe(SO{sub 4}){sub 2}(H{sub 2}O) nanoparticles have good luminescent properties. • Size and luminescent properties of two samples have been studied and compared.

Microwave synthesis of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C as positive-electrode materials for rechargeable lithium batteries

Energy Technology Data Exchange (ETDEWEB)

Xi, Yupeng; Zhang, Yanhui; Su, Zhi, E-mail: suzhixj@sina.com

2015-04-15

Highlights: • High performance LVP/C synthesized by self-assembly microwave oven. • TEM showed the carbon layer is consisted of two kinds of concrete components. • The fast and efficient method make the process feasible commercially. - Abstract: The paper reports a microwave irradiation method to rapidly synthesize Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C materials as cathode for lithium ion batteries by the self-assembly microwave reaction oven with carbon seal reactor, using LiH{sub 2}PO{sub 4}, V{sub 2}O{sub 5} and sucrose as raw materials. Sucrose was used to be reducer and carbon source. Thermogravimetric (TG) analysis, X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM) were used to characterize its structure and morphology. Electrochemical properties of the Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C materials were studied by cyclic voltammetry (CV) and charge–discharge cycling performance. The results showed that the diffraction peaks of the sample correspond to a single-phase, and can be indexed as monoclinic structure with a space group of P2{sub 1}/n. An electrochemical test showed that Li{sub 3}V{sub 2}(PO{sub 4}){sub 3}/C demonstrated an excellent electrochemical capacity of 138 mA h g{sup −1} at 0.2 C rate and 124.1 mA h g{sup −1} at 5 C rate with stable cycle ability.

[Pr2(pdc3(Hpdc(H2O4]n·n(H3hp·8n(H2O, a One-Dimensional Coordination Polymer Containing PrO6N3 Tri-Capped Trigonal Prisms and PrO8N Mono-Capped Square Anti-Prisms (H2pdc = Pyridine 2,6-Dicarboxylic Acid, C7H5NO4; 3hp = 3-Hydroxy Pyridine, C5H5NO

Directory of Open Access Journals (Sweden)

Shahzad Sharif

2012-08-01

Full Text Available The synthesis, structure and some properties of the one-dimensional coordination polymer, [Pr2(pdc3(Hpdc]n·n(H3hp·8n(H2O, (H2pdc = pyridine 2,6-dicarboxylic acid, C7H5NO4; 3hp = 3-hydroxypyridine, C5H5NO are described. One of the Pr3+ ions is coordinated by two O,N,O-tridentate pdc2− ligands and one tridentate Hpdc− anion to generate a fairly regular PrO6N3 tri-capped trigonal prism, with the N atoms acting as the caps. The second Pr3+ ion is coordinated by one tridentate pdc2− dianion, four water molecules and two monodentate bridging pdc2− ligands to result in a PrO8N coordination polyhedron that approximates to a mono-capped square-anti-prism. The ligands bridge the metal-atom nodes into a chain, which extends in the [100] direction. The H3hp+ cation and uncoordinated water molecules occupy the inter-chain regions and an N–HLO and numerous O–HLO hydrogen bonds consolidate the structure. The H3hp+ species appears to intercalate between pendant pdc rings to consolidate the polymeric structure. Crystal data: 1 (C33H43N5O29Pr2, Mr = 1255.54, triclinic,  (No. 2, Z = 2, a = 13.2567(1 Å, b = 13.6304(2 Å, c = 13.6409(2 Å, α = 89.695(1°, β = 63.049(1°, γ = 86.105(1°, V = 2191.16(5 Å3, R(F = 0.033, wR(F2 = 0.084.

Acid/Base and H2PO4(-) Controllable High-Contrast Optical Molecular Switches with a Novel BODIPY Functionalized [2]Rotaxane.

Science.gov (United States)

Arumugaperumal, Reguram; Srinivasadesikan, Venkatesan; Ramakrishnam Raju, Mandapati V; Lin, Ming-Chang; Shukla, Tarun; Singh, Ravinder; Lin, Hong-Cheu

2015-12-09

A novel multifunctional mechanically interlocked switchable [2]rotaxane R4 containing two molecular stations and rotaxane arms terminated with boron-dipyrromethene (BODIPY) fluorophores and its derivatives were synthesized for the first time by CuAAC click reaction. The shuttling motion of macrocycle between the dibenzylammonium and triazolium recognition sites and the distance dependent photoinduced electron transfer process of R4 is demonstrated by utilizing external chemical stimuli (acid/base). Interestingly, the reversible self-assembly process of R4 was recognized by the acid-base molecular switch strategy. Notably, two symmetrical triazolium groups acted as molecular stations, H2PO4(-) receptors, and H-bonded donors. Both [2]rotaxane R4 and thread R2 demonstrated excellent optical responses and high selectivity toward H2PO4(-) ion. The specific motion and guest-host interactions of mechanically interlocked machines (MIMs) were also further explored by quantum mechanical calculations. The thread R2 also demonstrated to enable the detection of H2PO4(-) in RAW 264.7 cells successfully.

Improvement of the mechanical properties and corrosion resistance of biodegradable β-Ca3(PO4)2/Mg-Zn composites prepared by powder metallurgy: the adding β-Ca3(PO4)2, hot extrusion and aging treatment.

Science.gov (United States)

Yan, Yang; Kang, Yijun; Li, Ding; Yu, Kun; Xiao, Tao; Deng, Youwen; Dai, Han; Dai, Yilong; Xiong, Hanqing; Fang, Hongjie

2017-05-01

In this study, 10%β-Ca 3 (PO 4 ) 2 /Mg-6%Zn (wt.%) composites with Mg-6%Zn alloy as control were prepared by powder metallurgy. After hot extrusion, the as-extruded composites were aged for 72h at 150°C. The effects of the adding β-Ca 3 (PO 4 ) 2 , hot extrusion and aging treatment on their microstructure, mechanical properties and corrosion resistance were investigated. The XRD results identified α-Mg, MgZn phase and β-Ca 3 (PO 4 ) 2 phase in these composites. After hot extrusion, grains were significantly refined, and the larger-sized β-Ca 3 (PO 4 ) 2 particles and coarse MgZn phases were broken into linear-distributed β-Ca 3 (PO 4 ) 2 and MgZn phases along the extrusion direction. After aging treatment, the elements of Zn, Ca, P and O presented a more homogeneous distribution. The compressive strengths of the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites were approximately double those of natural bone, and their densities and elastic moduli matched those of natural bone. The immersion tests and electrochemical tests revealed that the adding β-Ca 3 (PO 4 ) 2 , hot extrusion and aging treatment could promote the formation of protective corrosion product layer on the sample surface in Ringer's solution, which improved corrosion resistance of the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites. The XRD results indicated that the corrosion product layer contained Mg(OH) 2 , β-Ca 3 (PO 4 ) 2 and hydroxyapatite (HA). The cytotoxicity assessments showed the as-extruded β-Ca 3 (PO 4 ) 2 /Mg-Zn composite aged for 72h was harmless to L-929 cells. These results suggested that the β-Ca 3 (PO 4 ) 2 /Mg-Zn composites prepared by powder metallurgy were promising to be used for bone tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Ratiometric fluorescent receptors for both Zn2+ and H2PO4(-) ions based on a pyrenyl-linked triazole-modified homooxacalix[3]arene: a potential molecular traffic signal with an R-S latch logic circuit.

Science.gov (United States)

Ni, Xin-long; Zeng, Xi; Redshaw, Carl; Yamato, Takehiko

2011-07-15

A ratiometric fluorescent receptor with a C(3) symmetric structure based on a pyrene-linked triazole-modified homooxacalix[3]arene (L) was synthesized and characterized. This system exhibited an interesting ratiometric detection signal output for targeting cations and anions through switching the excimer emission of pyrene from the "on-off" to the "off-on" type in neutral solution. (1)H NMR titration results suggested that the Zn(2+) center of receptor L·Zn(2+) provided an excellent pathway of organizing anion binding groups for optimal host-guest interactions. It is thus believed that this receptor has potential application in sensing, detection, and recognition of both Zn(2+) and H(2)PO(4)(-) ions with different optical signals. In addition, the fluorescence emission changes by the inputs of Zn(2+) and H(2)PO(4)(-) ions can be viewed as a combinational R-S latch logic circuit at the molecular level.

LiFePO4 Nanostructures Fabricated from Iron(III) Phosphate (FePO4 x 2H2O) by Hydrothermal Method.

Science.gov (United States)

Saji, Viswanathan S; Song, Hyun-Kon

2015-01-01

Electrode materials having nanometer scale dimensions are expected to have property enhancements due to enhanced surface area and mass/charge transport kinetics. This is particularly relevant to intrinsically low electronically conductive materials such as lithium iron phosphate (LiFePO4), which is of recent research interest as a high performance intercalation electrode material for Li-ion batteries. Many of the reported works on LiFePO4 synthesis are unattractive either due to the high cost of raw materials or due to the complex synthesis technique. In this direction, synthesis of LiFePO4 directly from inexpensive FePO4 shows promise.The present study reports LiFePO4 nanostructures prepared from iron (III) phosphate (FePO4 x 2H2O) by precipitation-hydrothermal method. The sintered powder was characterized by X-ray diffractometry (XRD), X-ray photoelectron spectroscopy (XPS), Inductive coupled plasma-optical emission spectroscopy (ICP-OES), and Electron microscopy (SEM and TEM). Two synthesis methods, viz. bulk synthesis and anodized aluminum oxide (AAO) template-assisted synthesis are reported. By bulk synthesis, micro-sized particles having peculiar surface nanostructuring were formed at precipitation pH of 6.0 to 7.5 whereas typical nanosized LiFePO4 resulted at pH ≥ 8.0. An in-situ precipitation strategy inside the pores of AAO utilizing the spin coating was utilized for the AAO-template-assisted synthesis. The template with pores filled with the precipitate was subsequently subjected to hydrothermal process and high temperature sintering to fabricate compact rod-like structures.

Chirality- and pH-Controlled Supramolecular Isomerism in Cobalt Phosphonates and Its Impact on the Magnetic Behavior.

Science.gov (United States)

Feng, Jian-Shen; Bao, Song-Song; Ren, Min; Cai, Zhong-Sheng; Zheng, Li-Min

2015-11-23

Two pairs of enantiomeric compounds with formulas (S)- or (R)-Co3 (ppap)2 (4,4'-bpy)2 (H2 O)2 ⋅4 H2 O [(S)-1 or (R)-1], (S)- or (R)-Co3 (ppap)2 (4,4'-bpy)2 (H2 O)2 ⋅3 H2 O [(S)- or (R)-2), and related racemic compound Co3 (ppap)2 (4,4'-bpy)2 (H2 O)2 ⋅4 H2 O (rac-3; 4,4'-bpy=4,4'-bipyridine, H3 ppap=3-phenyl-2-[(phosphonomethyl)amino]propanoic acid) are reported. Compounds 1 and rac-3 show identical three-dimensional framework structures, whereas compounds 2 have two-dimensional layer structures. Compounds 1 and 2 are catenation isomers, formation of which is controlled solely by the pH of the reaction mixtures, whereas the formation of isomeric compounds 1 and rac-3 is controlled purely by the chirality of the phosphonate ligand. The magnetic properties of fully dehydrated (S)-1, (S)-2, and rac-3 are highly dependent on both structure and chirality. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A fast synthesis of Li 3V 2(PO 4) 3 crystals via glass-ceramic processing and their battery performance

Science.gov (United States)

Nagamine, Kenta; Honma, Tsuyoshi; Komatsu, Takayuki

A synthesis of Li 3V 2(PO 4) 3 being a potential cathode material for lithium ion batteries was attempted via a glass-ceramic processing. A glass with the composition of 37.5Li 2O-25V 2O 5-37.5P 2O 5 (mol%) was prepared by a melt-quenching method and precursor glass powders were crystallized with/without 10 wt% glucose in N 2 or 7%H 2/Ar atmosphere. It was found that heat treatments with glucose at 700 °C in 7%H 2/Ar can produce well-crystallized Li 3V 2(PO 4) 3 in the short time of 30 min. The battery performance measurements revealed that the precursor glass shows the discharge capacity of 14 mAh g -1 at the rate of 1 μA cm -2 and the glass-ceramics with Li 3V 2(PO 4) 3 prepared with glucose at 700 °C in 7%H 2/Ar show the capacities of 117-126 mAh g -1 (∼96% of the theoretical capacity) which are independent of heat treatment time. The present study proposes that the glass-ceramic processing is a fast synthesizing route for Li 3V 2(PO 4) 3 crystals.

[Synthesis and biological activity of 2,3-secotriterpene acid mono- and diamides].

Science.gov (United States)

Tolmacheva, I A; Igosheva, E V; Vikharev, Iu B; Grishko, V V; Savinova, O V; Boreko, E I; Eremin, V F

2013-01-01

Four types of amide (C3; C28; C3-C28) conjugates based on 2,3-seco-18alphaH-oleanane and 2,3-secolupane mono- and dicarboxylic acids were synthesized. The range of diamide derivatives was supplemented with C3-C3' and C28-C28' dicondensed amides with two A-secotriterpene backbones educed by reacting monocarboxylic A-secoacids with biogenic amino acid lysine. Compounds with inhibitory action against herpes virus reproduction (EC50 8.7 and 4.1 McM) were found among the synthesized mono- and diamide derivatives containing an ethyl-beta-alaninate fragment. It has been ascertained that diamide with ethyl-beta-alaninate fragment combines anti-herpes virus properties and anti-HIV activity (EC50 5.1 McM). For active compounds, the maximum non-toxic concentration (MNTC)/EC50 ratios ranges from 9.7 to 40.8. The synthesized amide conjugates do not exhibit any marked cytotoxic effects against human tumor cell lines rabdomiosarcoma RD TE32, A549 lung carcinoma and melanoma MS.

Toluene and chlorobenzene dinitration over solid H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2} catalyst

Energy Technology Data Exchange (ETDEWEB)

Adamiak, Joanna, E-mail: jadamiak@ch.pw.edu.pl [Warsaw University of Technology, Faculty of Chemistry, Division of High Energetic Materials, Noakowskiego 3, 00-664 Warsaw (Poland); Kalinowska-Alichnewicz, Dorota; Szadkowski, Michal; Skupinski, Wincenty [Warsaw University of Technology, Faculty of Chemistry, Division of High Energetic Materials, Noakowskiego 3, 00-664 Warsaw (Poland)

2011-11-15

Highlights: {yields} A novel catalyst H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2} was characterized and used in nitration. {yields} On the surface domains of phosphomolybdic acid (HPM) are obtained. {yields} Dinitrotoluene is obtained with very high yield i.e. 96 wt.% in mild conditions. {yields} Dinitrochlorobenzene is obtained with only twelve-fold excess of nitric acid. {yields} It is sulfuric acid free and solvent free nitration of aromatic compounds. - Abstract: A new catalyst, H{sub 3}PO{sub 4}/MoO{sub 3}/SiO{sub 2}, was prepared by modification of MoO{sub 3}/SiO{sub 2} using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds.

Resveratrol induces cellular senescence with attenuated mono-ubiquitination of histone H2B in glioma cells

International Nuclear Information System (INIS)

Gao, Zhen; Xu, Michael S.; Barnett, Tamara L.; Xu, C. Wilson

2011-01-01

Research highlights: → Resveratrol induces cellular senescence in glioma cell. → Resveratrol inhibits mono-ubiquitination of histone H2B at K120. → Depletion of RNF20, phenocopies the inhibitory effects of resveratrol. → Mono-ubiquitination of histone H2B at K120 is a novel target of resveratrol. → RNF20 inhibits cellular senescence in proliferating glioma cells. -- Abstract: Resveratrol (3,4',5-trihydroxy-trans-stilbene), a polyphenol naturally occurring in grapes and other plants, has cancer chemo-preventive effects and therapeutic potential. Although resveratrol modulates multiple pathways in tumor cells, how resveratrol or its affected pathways converge on chromatin to mediate its effects is not known. Using glioma cells as a model, we showed here that resveratrol inhibited cell proliferation and induced cellular hypertrophy by transforming spindle-shaped cells to enlarged, irregular and flatten-shaped ones. We further showed that resveratrol-induced hypertrophic cells expressed senescence-associated-β-galactosidase, suggesting that resveratrol-induced cellular senescence in glioma cells. Consistent with these observations, we demonstrated that resveratrol inhibited clonogenic efficiencies in vitro and tumor growth in a xenograft model. Furthermore, we found that acute treatment of resveratrol inhibited mono-ubiquitination of histone H2B at K120 (uH2B) in breast, prostate, pancreatic, lung, brain tumor cells as well as primary human cells. Chronic treatment with low doses of resveratrol also inhibited uH2B in the resveratrol-induced senescent glioma cells. Moreover, we showed that depletion of RNF20, a ubiquitin ligase of histone H2B, inhibited uH2B and induced cellular senescence in glioma cells in vitro, thereby recapitulated the effects of resveratrol. Taken together, our results suggest that uH2B is a novel direct or indirect chromatin target of resveratrol and RNF20 plays an important role in inhibiting cellular senescence programs that are

Resveratrol induces cellular senescence with attenuated mono-ubiquitination of histone H2B in glioma cells

Energy Technology Data Exchange (ETDEWEB)

Gao, Zhen; Xu, Michael S.; Barnett, Tamara L. [Nevada Cancer Institute, Las Vegas, NV 89135 (United States); Xu, C. Wilson, E-mail: wxu@nvcancer.org [Nevada Cancer Institute, Las Vegas, NV 89135 (United States)

2011-04-08

Research highlights: {yields} Resveratrol induces cellular senescence in glioma cell. {yields} Resveratrol inhibits mono-ubiquitination of histone H2B at K120. {yields} Depletion of RNF20, phenocopies the inhibitory effects of resveratrol. {yields} Mono-ubiquitination of histone H2B at K120 is a novel target of resveratrol. {yields} RNF20 inhibits cellular senescence in proliferating glioma cells. -- Abstract: Resveratrol (3,4',5-trihydroxy-trans-stilbene), a polyphenol naturally occurring in grapes and other plants, has cancer chemo-preventive effects and therapeutic potential. Although resveratrol modulates multiple pathways in tumor cells, how resveratrol or its affected pathways converge on chromatin to mediate its effects is not known. Using glioma cells as a model, we showed here that resveratrol inhibited cell proliferation and induced cellular hypertrophy by transforming spindle-shaped cells to enlarged, irregular and flatten-shaped ones. We further showed that resveratrol-induced hypertrophic cells expressed senescence-associated-{beta}-galactosidase, suggesting that resveratrol-induced cellular senescence in glioma cells. Consistent with these observations, we demonstrated that resveratrol inhibited clonogenic efficiencies in vitro and tumor growth in a xenograft model. Furthermore, we found that acute treatment of resveratrol inhibited mono-ubiquitination of histone H2B at K120 (uH2B) in breast, prostate, pancreatic, lung, brain tumor cells as well as primary human cells. Chronic treatment with low doses of resveratrol also inhibited uH2B in the resveratrol-induced senescent glioma cells. Moreover, we showed that depletion of RNF20, a ubiquitin ligase of histone H2B, inhibited uH2B and induced cellular senescence in glioma cells in vitro, thereby recapitulated the effects of resveratrol. Taken together, our results suggest that uH2B is a novel direct or indirect chromatin target of resveratrol and RNF20 plays an important role in inhibiting cellular

Paternally expressed Peg3 controls maternally expressed Zim1 as a trans factor.

Directory of Open Access Journals (Sweden)

An Ye

Full Text Available The expression of two adjacent imprinted genes, Peg3 and Zim1, is inversely correlated: down-regulation of Peg3 coinciding with up-regulation of Zim1. The current study characterized this inverse correlation using a mutant allele targeting Peg3. According to the results, the mutation on the paternal allele of Peg3 resulted in a dramatic increase in the transcription levels of the maternal allele of Zim1, suggesting the involvement of unknown trans factors in this trans-allelic event. Subsequent ChIP experiments revealed that the protein encoded by Peg3 itself binds to the zinc finger exon of Zim1, which is modified with the repression mark H3K9me3. Interestingly, the levels of H3K9me3 on Zim1 are also reduced in the mutant cells lacking the protein PEG3, suggesting potential roles for PEG3 in establishing H3K9me3 on Zim1. Reintroducing PEG3 into the mutant cell restored down-regulation of Zim1, confirming the predicted repressor role for Peg3 on Zim1. Overall, these results demonstrated that paternally expressed Peg3 controls maternally expressed Zim1 as a trans factor. The current study also provides the first case for the trans-allelic interaction of two oppositely imprinted genes through their gene products.

Synthesis, crystal structure, and ionic conductivity of a new layered metal phosphate, Li2Sr2Al(PO4)3

International Nuclear Information System (INIS)

Kim, Sung-Chul; Kwak, Hyun-Jung; Yoo, Chung-Yul; Yun, Hoseop; Kim, Seung-Joo

2016-01-01

A new layered metal phosphate, Li 2 Sr 2 Al(PO 4 ) 3 , was synthesized in the form of either a single-crystal or polycrystalline powder using the molten hydroxide flux method or a solid-state reaction, respectively. Li 2 Sr 2 Al(PO 4 ) 3 crystallizes to the P2 1 /n (Z=4) monoclinic space group with lattice parameters a≈4.95 Å, b≈22.06 Å, c≈8.63 Å, and β≈91.5°. The structure is composed of stacked [LiSrAl(PO 4 ) 2 ] layers alternating regularly with [LiSrPO 4 ] layers. In the [LiSrAl(PO 4 ) 2 ] sublattice, the AlO 6 octahedra and PO 4 tetrahedra are tilted cooperatively to form an anionic, corrugated, two-dimensional [Al(PO 4 ) 2 ] 3− framework that can be regarded as a “distorted-glaserite” structure. The [LiSrPO 4 ] sublattice is that of a layered block containing a six-membered ring formed from alternating linkages of LiO 4 and PO 4 tetrahedra. The six-membered rings show a boat-type arrangement with the up(U) or down(D) pointing sequence, UUDUUD. The interspace between the two sublattices generates a two-dimensional pathway for Li + ion conduction. The impedance measurement indicated that Li 2 Sr 2 Al(PO 4 ) 3 had a moderate ion conductivity (σ≈1.30×10 −4 S cm −1 at 667 K), with an activation energy E a ≈1.02 eV. - Graphical abstract: Polyhedral view of Li 2 Sr 2 Al(PO 4 ) 3 . Li + ions are represented by green spheres, Sr atoms by white spheres, AlO 6 groups by octahedra, and PO 4 groups by tetrahedra. - Highlights: • New compound Li 2 Sr 2 Al(PO 4 ) 3 is reported. • The crystal structure is investigated by single-crystal XRD analysis. • The structure is formed by the alternate stacking of two different sublattices. • Correlation between the crystal structure and ionic conductivity is discussed.

Equilibrium diagram of KPO{sub 3}-Y(PO{sub 3}){sub 3} system, chemical preparation and characterization of KY(PO{sub 3}){sub 4}

Energy Technology Data Exchange (ETDEWEB)

Jouini, Anis; Ferid, Mokhtar; Trabelsi-Ayadi, Malika

2003-04-17

Microdifferential thermal analysis ({mu}-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO{sub 3}-Y(PO{sub 3}){sub 3} system. The only compound observed within the system was KY(PO{sub 3}){sub 4} melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO{sub 3}){sub 3} at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO{sub 3} was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO{sub 3}){sub 4} polyphosphate has the P2{sub 1} space group with lattice parameters: a=7.183(4) A, b=8.351(6) A, c=7.983(3) A, {beta}=91.75(3) deg. and Z=2 is isostructural with KNd(PO{sub 3}){sub 4}. The second allotropic form of KY(PO{sub 3}){sub 4} belongs to the P2{sub 1}/n space group with lattice parameters: a=10.835(3) A, b=9.003(2) A, c=10.314(1) A, {beta}=106.09(7) deg. and Z=4 and is isostructural with TlNd(PO{sub 3}){sub 4}. The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP{sub 4}O{sub 12} crystallizes in the C2/c space group with lattice parameters: a=7.825(3) A, b=12.537(4) A, c=10.584(2) A, {beta}=110.22(7) deg. and Z=4 is isostructural with RbNdP{sub 4}O{sub 12} and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported.

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Agougui, H.; Aissa, A. [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia); Maggi, S. [CNR-IC Istituto di Cristallografia, via Amendola 122/O, 70126 Bari (Italy); Debbabi, M., E-mail: m.debbabi@yahoo.fr [Laboratoire de Physico-Chimie des Materiaux, Faculte des sciences de Monastir, 5019 Monastir (Tunisia)

2010-12-15

Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ({sup 1}H and {sup 31}P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH{sup -} groups of the apatitic structure.

Phosphonate-hydroxyapatite hybrid compounds prepared by hydrothermal method

International Nuclear Information System (INIS)

Agougui, H.; Aissa, A.; Maggi, S.; Debbabi, M.

2010-01-01

Calcium hydroxyapatite (CaHAp) was prepared in the presence of two alkylphosphonates, the tert-butyl phosphonic acid TBPOH and the 2-carboxyletylphosphonic acid 2-CEPA, by hydrothermal method at 120 deg. C for 15 h. The modification of hydroxyapatite by grafting organic moieties is confirmed by IR and NMR MAS ( 1 H and 31 P) spectroscopy and chemical analysis. X-ray powder diffraction patterns show that the incorporation of organic moieties induces a significant loss of the material crystallinity and a clear increase of the unit cell lattice parameter a as function of 2-CEPA grafting rate. The specific surface area (SSA) increases with increasing phosphonate amount especially for 2-CEPA. All techniques show the lower reactivity of TBPOH due to the steric effects of tert-butyl, whereas the 2-CEPA with a linear chain and double acidic functions is more reactive and can replace the OH - groups of the apatitic structure.

Extraction of uranium from aqueous solution by phosphonic acid-imbedded polyurethane foam

International Nuclear Information System (INIS)

Katragadda, S.; Gesser, H.D.; Chow, A.

1997-01-01

Phenylphosphonic acid was imbedded into the matrix of the polyurethane foam during the fabrication process of the polymer. The extraction of uranium by phosphonic acid-imbedded polyurethane foam and blank polyurethane (i.e., foam without phosphonic acid functional groups) was investigated. Phosphonic acid-imbedded foam showed superior extractability of uranium from solutions with pH = 7.0 ± 1.5 over a wide range of temperatures. (author)

Na3Tb(PO4)2: Synthesis, crystal structure and greenish emitting properties

Science.gov (United States)

Zhao, Dan; Ma, Zhao; Liu, Bao-Zhong; Zhang, Rui-Juan; Wu, Zhi-Qiang; Wang, Jian; Duan, Pei-Gao

2018-03-01

A anhydrous orthoborate Na3Tb(PO4)2 has been prepared and its crystal structure was determined by X-Ray diffraction of a non-merohedral twinned single crystal. The results show that the compound crystallizes in monoclinic space group C2/c and the structure features a 3D framework containing PO4, NaO6, NaO7, NaO8 and TbO8 polyhedra. Under near-UV excitation (370 nm), Na3Tb(PO4)2 shows intense characteristic emission bands of Tb3+ (490 nm, 543 nm, 585 nm and 620 nm) with the CIE coordinate of (0.3062, 0.5901), corresponding to greenish color. The excitation spectrum covers a wide range from 340 nm to 390 nm, which indicates that phosphor Na3Tb(PO4)2 can be efficiently activated by near-UV LED ship.

Proton-conducting solid acid electrolytes based upon MH(PO3H)

NARCIS (Netherlands)

Zhou, W.

2011-01-01

Solid acids, such as CsHSO4 and CsH2PO4, are a novel class of anhydrous proton-conducting compounds that can be used as electrolyte in H2/O2 and direct methanol fuel cells. The disordering of the hydrogen-bonded network above the so-called superprotonic phase transition results in an increase of the

Structures and Spectroscopy Studies of Two M(II-Phosphonate Coordination Polymers Based on Alkaline Earth Metals (M = Ba, Mg

Directory of Open Access Journals (Sweden)

Kui-Rong Ma

2013-01-01

Full Text Available The two examples of alkaline-earth M(II-phosphonate coordination polymers, [Ba2(L(H2O9]·3H2O (1 and [Mg1.5(H2O9]·(L-H21.5·6H2O (2 (H4L = H2O3PCH2N(C4H8NCH2PO3H2, N,N′-piperazinebis(methylenephosphonic acid, (L-H2 = O3PH2CHN(C4H8NHCH2PO3 have been hydrothermally synthesized and characterized by elemental analysis, FT-IR, PXRD, TG-DSC, and single-crystal X-ray diffraction. Compound 1 possesses a 2D inorganic-organic alternate arrangement layer structure built from 1D inorganic chains through the piperazine bridge, in which the ligand L−4 shows two types of coordination modes reported rarely at the same time. In 1, both crystallographic distinct Ba(1 and Ba(2 ions adopt 8-coordination two caps and 9-coordination three caps triangular prism geometry structures, respectively. Compound 2 possesses a zero-dimensional mononuclear structure with two crystallographic distinct Mg(II ions. Free metal cations   [MgO6]n2+ and uncoordinated anions (L-H2n2- are joined together by static electric force. Results of photoluminescent measurement indicate three main emission bands centered at 300 nm, 378.5 nm, and 433 nm for 1 and 302 nm, 378 nm, and 434.5 nm for 2 (λex=235 nm, respectively. The high energy emissions could be derived from the intraligand π∗-n transition stations of H4L (310 nm and 382 nm, λex=235 nm, while the low energy emission (>400 nm of 1-2 may be due to the coordination effect with metal(II ions.

Toluene and chlorobenzene dinitration over solid H3PO4/MoO3/SiO2 catalyst.

Science.gov (United States)

Adamiak, Joanna; Kalinowska-Alichnewicz, Dorota; Szadkowski, Michał; Skupiński, Wincenty

2011-11-15

A new catalyst, H(3)PO(4)/MoO(3)/SiO(2), was prepared by modification of MoO(3)/SiO(2) using phosphoric acid. The characterization of the catalyst was performed using Infrared and Raman Spectroscopy, potentiometric titration and nitrogen adsorption-desorption methods. Molybdenum oxides were identified along with phosphomolybdic acid and polymolybdates on the modified surface. The suitability of the catalysts for toluene and chlorobenzene nitration in continuous process was examined. Toluene is effectively nitrated to dinitrotoluene (DNT) in one-stage process (96 wt.% of DNT in the product) and in mild conditions i.e. at room temperature and only with ten-fold excess of nitric acid. In chlorobenzene nitration only twelve-fold excess of nitric acid is needed to obtain as high yield as 95 wt.%. Most importantly, the novel catalysts we have developed, provide the opportunity for sulfuric acid- free nitration of aromatic compounds. Copyright © 2011 Elsevier B.V. All rights reserved.

Synthesis, structure, and photoluminescence properties of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors for white-light-emitting diodes.

Science.gov (United States)

Jiao, Mengmeng; Lü, Wei; Shao, Baiqi; Zhao, Lingfei; You, Hongpeng

2015-08-24

A series of novel KBaSc2 (PO4 )3 :Ce(3+) /Eu(2+) /Tb(3+) phosphors are prepared using a solid-state reaction. X-ray diffraction analysis and Rietveld structure refinement are used to check the phase purity and crystal structure of the prepared samples. Ce(3+) - and Eu(2+) -doped phosphors both have broad excitation and emission bands, owing to the spin- and orbital-allowed electron transition between the 4f and 5d energy levels. By co-doping the KBaSc2 (PO4 )3 :Eu(2+) and KBaSc2 (PO4 )3 :Ce(3+) phosphors with Tb(3+) ions, tunable colors from blue to green can be obtained. The critical distance between the Eu(2+) and Tb(3+) ions is calculated by a concentration quenching method and the energy-transfer mechanism for Eu(2+) →Tb(3+) is studied by utilizing the Inokuti-Hirayama model. In addition, the quantum efficiencies of the prepared samples are measured. The results indicate that KBaSc2 (PO4 )3 :Eu(2+) ,Tb(3+) and KBaSc2 (PO4 )3 :Ce(3+) ,Tb(3+) phosphors might have potential applications in UV-excited white-light-emitting diodes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Room temperature H{sub 2}S gas sensing characteristics of platinum (Pt) coated porous alumina (PoAl) thick films

Energy Technology Data Exchange (ETDEWEB)

More, P.S., E-mail: p_smore@yahoo.co.in [Department of Physics, Institute of Science, Mumbai 400 032 (India); Raut, R.W. [Department of Botany, Institute of Science, Mumbai 400 032 (India); Ghuge, C.S. [Department of Physics, Institute of Science, Mumbai 400 032 (India)

2014-02-14

The study reports H{sub 2}S gas sensing characteristics of platinum (Pt) coated porous alumina (PoAl) films. The porous alumina (PoAl) thick layers were formed in the dark on aluminum substrates using an electrochemical anodization method. Thin semitransparent platinum (Pt) films were deposited on PoAl samples using chemical bath deposition (CBD) method. The films were characterized using energy dispersive X-ray analysis (EDAX) and scanning electron microscopy (SEM). The thicknesses of coated and bare films were measured using ellipsometry. The sensing properties such as sensitivity factor (S.F.), response time, recovery time and repeatability were measured using a static gas sensing system for H{sub 2}S gas. The EDAX studies confirmed the purity of Pt–PoAl film and indicated the formation of pure platinum (Pt) phase. The ellipsometry studies revealed the thickness of PoAl layer of about 15–17 μm on aluminum substrates. The SEM studies demonstrated uniform distribution of spherical pores with a size between 0.250 and 0.500 μm for PoAl film and nearly spherical platinum particles with average particle size ∼100 nm for Pt–PoAl film. The gas-sensing properties of these samples were studied in a home-built static gas characterization system. The H{sub 2}S gas sensing properties of Pt–PoAl at 1000 ppm of H{sub 2}S gave maximum sensitivity factor (S.F.) = 1200. The response time and recovery time were found to be 2–3 min and ∼1 min respectively. Further, the measurement of H{sub 2}S gas sensing properties clearly indicated the repeatability of gas sensing response of Pt–PoAl film. The present study indicated the significant potential of Pt coated PoAl films for H{sub 2}S gas sensing applications in diverse areas. - Highlights: • Electrochemical anodization, cheap and effective method for fabrication of PoAl. • Chemical bath deposition, a simple and effective method for deposition of Pt on PoAl. • A nano-composite film sensor with high sensitivity

Phosphonate removal from discharged circulating cooling water using iron-carbon micro-electrolysis.

Science.gov (United States)

Zhou, Zhen; Qiao, Weimin; Lin, Yangbo; Shen, Xuelian; Hu, Dalong; Zhang, Jianqiao; Jiang, Lu-Man; Wang, Luochun

2014-01-01

Phosphonate is a commonly used corrosion and scale inhibitor for a circulating cooling water (CCW) system. Its discharge could cause eutrophication of receiving waters. The iron-carbon (Fe/C) micro-electrolysis technology was used to degrade and remove phosphonate from discharged CCW. The influences of initial pH, Fe/C ratio (FCR) and temperature on phosphonate removal were investigated in a series of batch tests and optimized by response surface methodology. The quadratic model of phosphonate removal was obtained with satisfactory degrees of fitness. The optimum conditions with total phosphorus removal efficiency of 95% were obtained at pH 7.0, FCR of 1.25, and temperature of 45 °C. The phosphonate removal mechanisms were also studied. Phosphonate removal occurred predominantly via two consecutive reactive phases: the degradation of phosphonate complexes (Ca-phosphonate) and the precipitation of Fe/C micro-electrolysis products (PO₄(3-), Ca²⁺ and Fe³⁺).

H-PoP and H-PoPG: heuristic partitioning algorithms for single individual haplotyping of polyploids.

Science.gov (United States)

Xie, Minzhu; Wu, Qiong; Wang, Jianxin; Jiang, Tao

2016-12-15

Some economically important plants including wheat and cotton have more than two copies of each chromosome. With the decreasing cost and increasing read length of next-generation sequencing technologies, reconstructing the multiple haplotypes of a polyploid genome from its sequence reads becomes practical. However, the computational challenge in polyploid haplotyping is much greater than that in diploid haplotyping, and there are few related methods. This article models the polyploid haplotyping problem as an optimal poly-partition problem of the reads, called the Polyploid Balanced Optimal Partition model. For the reads sequenced from a k-ploid genome, the model tries to divide the reads into k groups such that the difference between the reads of the same group is minimized while the difference between the reads of different groups is maximized. When the genotype information is available, the model is extended to the Polyploid Balanced Optimal Partition with Genotype constraint problem. These models are all NP-hard. We propose two heuristic algorithms, H-PoP and H-PoPG, based on dynamic programming and a strategy of limiting the number of intermediate solutions at each iteration, to solve the two models, respectively. Extensive experimental results on simulated and real data show that our algorithms can solve the models effectively, and are much faster and more accurate than the recent state-of-the-art polyploid haplotyping algorithms. The experiments also show that our algorithms can deal with long reads and deep read coverage effectively and accurately. Furthermore, H-PoP might be applied to help determine the ploidy of an organism. https://github.com/MinzhuXie/H-PoPG CONTACT: xieminzhu@hotmail.comSupplementary information: Supplementary data are available at Bioinformatics online. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com.

Synthesis and performance of Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} cathode materials

Energy Technology Data Exchange (ETDEWEB)

Dai, Changsong; Chen, Zhenyu; Jin, Haizu; Hu, Xinguo [School of Chemical Engineering and Technology, Harbin Institute of Technology, Harbin 150001 (China)

2010-09-01

In order to search for cathode materials with better performance, Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} (0, 0.04, 0.07, 0.10 and 0.13) is prepared via a carbothermal reduction (CTR) process with LiOH.H{sub 2}O, V{sub 2}O{sub 5}, Mg(CH{sub 3}COO){sub 2}.4H{sub 2}O, NH{sub 4}H{sub 2}PO{sub 4}, and sucrose as raw materials and investigated by X-ray diffraction (XRD), scanning electron microscopic (SEM) and electrochemical impedance spectrum (EIS). XRD shows that Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} (x = 0.04, 0.07, 0.10 and 0.13) has the same monoclinic structure as undoped Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} while the particle size of Li{sub 3}(V{sub 1-x}Mg{sub x}){sub 2}(PO{sub 4}){sub 3} is smaller than that of Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} according to SEM images. EIS reveals that the charge transfer resistance of as-prepared materials is reduced and its reversibility is enhanced proved by the cyclic votammograms. The Mg{sup 2+}-doped Li{sub 3}V{sub 2}(PO{sub 4}){sub 3} has a better high rate discharge performance. At a discharge rate of 20 C, the discharge capacity of Li{sub 3}(V{sub 0.9}Mg{sub 0.1}){sub 2}(PO{sub 4}){sub 3} is 107 mAh g{sup -1} and the capacity retention is 98% after 80 cycles. Li{sub 3}(V{sub 0.9}Mg{sub 0.1}){sub 2}(PO{sub 4}){sub 3}//graphite full cells (085580-type) have good discharge performance and the modified cathode material has very good compatibility with graphite. (author)

The hydrogen dynamics of CsH5(PO4)2 studied by means of nuclear magnetic resonance

International Nuclear Information System (INIS)

Gradisek, A; Dimnik, B; Vrtnik, S; Dolinsek, J; Wencka, M; Zdanowska Fraczek, M; Lavrova, G V

2011-01-01

We have investigated the hydrogen dynamics of cesium pentahydrogen diphosphate, CsH 5 (PO 4 ) 2 , by means of nuclear magnetic resonance (NMR) spectroscopy, in order to address the question of why there is no superprotonic phase transition in this compound, in contrast to other structurally similar hydrogen-bonded ionic salts, where a superprotonic transition is frequently found to be present. The analysis of the NMR spectrum and the spin-lattice relaxation rate revealed that the temperature-dependent hydrogen dynamics of CsH 5 (PO 4 ) 2 involves motional processes (the intra-H-bond jumps and the inter-H-bond jumps at elevated temperatures, as a mechanism of the ionic conductivity) identical to those for the other H-bonded superprotonic salts. The considerably stronger H-bond network in CsH 5 (PO 4 ) 2 prompts the search for a higher superprotonic transition temperature. However, due to the relatively weak bonding between the {[H 2 PO 4 ]} ∞ planes in the [100] direction of the CsH 5 (PO 4 ) 2 structure by means of the ionic bonding via the cesium atoms and the small number of H bonds in that direction (where out of five H bonds in the unit cell, four are directed within the {[H 2 PO 4 ]} ∞ planes and only one is between the planes), the bonds between the planes become thermally broken and the crystal melts before the H-bond network rearranges via water release into an open structure typical of the superprotonic phase. Were the coupling between the {[H 2 PO 4 ]} ∞ planes in the CsH 5 (PO 4 ) 2 somewhat stronger, the superprotonic transition would occur in the same manner as it does in other structurally related hydrogen-bonded ionic salts.

Influence of preparation conditions on porous structures of olive stone activated by H3PO4

International Nuclear Information System (INIS)

Yavuz, Reha; Akyildiz, Hanife; Karatepe, Nilguen; Cetinkaya, Eda

2010-01-01

An olive factory residue was used as a precursor in the preparation of granular activated carbon by chemical activation with H 3 PO 4 . Effects of final activation temperature, time, and H 3 PO 4 concentration used in the impregnation stage on the porous development were investigated. SO 2 adsorption experiments were also performed for some of the activated carbon samples to represent their adsorption performance. Activation at low temperature represented that micropores were developed first at early stages of the temperatures. Mesoporosity developed at around 250 C, enhanced up to 400 C, and then started to decrease due to possibly shrinking of pores. The optimum temperature for olive stone was found to be around 400 C on the basis of total pore volume and BET surface area. It was clearly demonstrated that H 3 PO 4 concentration used in the impregnation stage was not only effective for development of surface area and pore volumes but also an effective tool for tailoring the pore structure and size distribution. (author)

Aberrant PO2 values in proficiency testing.

Science.gov (United States)

Fonzi, C E; Clausen, J L; Mahoney, J

1993-03-01

We prospectively determined the frequency of aberrant vials of fluorocarbon/buffer used for proficiency testing of measurements of pH, PCO2, and PO2, using 20 duplicate vials from 12 lots of fluorocarbon/buffer and two arterial blood gas analyzers in eight reference laboratories. We defined aberrant vials as vials for which both duplicate measurements differed from the mean value of repeated measurements for the specific instrument (for each lot of testing materials) by > 0.04 for pH, > 10% of the mean or 3.0 mm Hg, whichever was greater, for PCO2; or > 10% of the mean or 6 mm Hg, whichever was greater, for PO2. Four of 1620 vials (0.25%) were aberrant, all based on PO2 measurements (range of mean values: pH, 7.181-7.631; PCO2, 12.7-65.9; PO2, 32.5-150.1) were 0.0055 for pH, 0.67 mm Hg for PCO2, and 1.65 mm Hg for PO2. Deliberate contamination of the fluorocarbon emulsion with room air, as might occur during sampling from the vial, indicated that only minor increases in PO2 (e.g., 1.0 mm Hg at PO2 of 56 mm Hg) occur when samples are aspirated. Larger increases in PO2 (mean 7.1 mm Hg at a PO2 of 66 mm Hg) occurred when the syringe samples were contaminated with room air. We conclude that isolated aberrant measurements of PO2 in blood gas proficiency testing attributable to vial contents can occur, but the frequency is very low.

Facile sonochemical synthesis and morphology control of CePO4 nanostructures via an oriented attachment mechanism: Application as luminescent probe for selective sensing of Pb2+ ion in aqueous solution

International Nuclear Information System (INIS)

Shiralizadeh Dezfuli, Amin; Ganjali, Mohammad Reza; Norouzi, Parviz

2014-01-01

CePO 4 nanostructures with hexagonal phase were controllably synthesized using Ce(NO 3 ) 3 reaction with NH 4 H 2 PO 4 through a sonochemical method by simply varying the reaction conditions. By adding ethanol and polyethylene glycol (PEG), coral-reef nanostructures (CRNs) were synthesized and controlling over pH caused to nanorods/nanowires. Oriented attachment (OA) is proposed as dominant mechanism on the growth of nanostructures which is in competition with Ostwald ripening (OR). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM), respectively. The luminescent properties of CePO 4 with different morphologies have been studied. Among the nanostructures, nanoparticles with the highest intensity of fluorescent have been used as luminescent probe for selective sensing of Pb 2+ ion in aqueous solution. - Highlights: • Facile sonochemical method has been used for synthesis of CePO 4 nanostructures. • Coral-reef as a new morphology of nanostructures is introduced. • CePO 4 NPs have been used as luminescent probe for selective sensing of Pb 2+ ion

Photoluminescence and thermoluminescence characterization of Eu3+- and Dy3+ -activated Ca3(PO4)2 phosphor

International Nuclear Information System (INIS)

Nagpure, I.M.; Saha, Subhajit; Dhoble, S.J.

2009-01-01

Rare-earth-doped polycrystalline Ca 3 (PO 4 ) 2 :Eu, Ca 3 (PO 4 ) 2 :Dy and Ca 3 (PO 4 ) 2 :Eu,Dy phosphors prepared by a modified solid-state synthesis has been studied for its X-ray diffraction, thermoluminescence (TL) and photoluminescence (PL) characteristics. The PL emission spectra of the phosphor suggest the presence of Eu 3+ ion in Ca 3 (PO 4 ) 2 :Eu and Dy 3+ ion in Ca 3 (PO 4 ) 2 :Dy lattice sites. The TL glow curve of the Ca 3 (PO 4 ) 2 :Eu compounds has a simple structure with a prominent peak at 228 deg. C, while Ca 3 (PO 4 ) 2 :Dy peaking at 146 and 230 deg. C. TL sensitivity of phosphors are compared with CaSO 4 : Dy and found 1.52 and 1.20 times less in Ca 3 (PO 4 ) 2 :Eu and Ca 3 (PO 4 ) 2 :Dy phosphors, respectively. The Ca 3 (PO 4 ) 2 :Eu,Dy phosphors shows switching behavior under two different excitation wavelengths and enhancement in PL intensity of Dy 3+ ions were reported. The paper discusses the photoluminescence and thermoluminescence behavior of Eu 3+ and Dy 3+ ion in Ca 3 (PO 4 ) 2 hosts, it may be applicable to solid-state lighting as well as thermoluminescence dosimetry applications.

The supramolecular architecture of tris(naphthalene-1,5-diaminium) bis(5-aminonaphthalen-1-aminium) octakis[hydrogen (5-carboxypyridin-3-yl)phosphonate].

Science.gov (United States)

Wilk, Magdalena; Janczak, Jan; Videnova-Adrabinska, Veneta

2012-09-01

The asymmetric unit of the title compound, 3C(10)H(12)N(2)(2+)·2C(10)H(11)N(2)(+)·8C(6)H(5)NO(5)P(-), contains one and a half naphthalene-1,5-diaminium cations, in which the half-molecule has inversion symmetry, one 5-aminonaphthalen-1-aminium cation and four hydrogen (5-carboxypyridin-3-yl)phosphonate anions. The crystal structure is layered and consists of hydrogen-bonded anionic monolayers between which the cations are arranged. The acid monoanions are organized into one-dimensional chains along the [101] direction via hydrogen bonds established between the phosphonate sites. (C)O-H···N(py) hydrogen bonds (py is pyridine) crosslink the chains to form an undulating (010) monolayer. The cations serve both to balance the charge of the anionic network and to connect neighbouring layers via multiple hydrogen bonds to form a three-dimensional supramolecular architecture.

Thermodynamics, dielectric permittivity and phase diagrams of the Rb1-x(NH4xH2PO4 type proton glasses

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S.I. Sorokov

2010-01-01

Full Text Available The cluster pseudospin model of proton glasses, which takes into account the energy levels of protons around the PO4 group, the long-range interactions between the hydrogen bonds, and an internal random deformational field is used to investigate thermodynamical characteristics, longitudinal and transverse dielectric permittivities of Rb1-x(ND4xD2PO4 and Rb1-x(NH4xH2AsO4 compounds. A review of experimental and theoretical works on the Rb1-x(NH4xH2PO4 type crystals is presented.

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, a new very complex Ba-Sc phosphate mineral from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia)

Science.gov (United States)

Yakovenchuk, Victor N.; Ivanyuk, Gregory Yu.; Pakhomovsky, Yakov A.; Panikorovskii, Taras L.; Britvin, Sergei N.; Krivovichev, Sergey V.; Shilovskikh, Vladimir V.; Bocharov, Vladimir N.

2018-02-01

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, is a new Ba-Sc phosphate from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia). It is orthorhombic, Pnma, a = 11.256(1), b = 8.512(1), c = 27.707(4) Å, V = 2654.6(3) Å3 and Z = 4 (from powder diffraction data) or a = 11.2261(9), b = 8.5039(6), c = 27.699(2) Å, V = 2644.3(3) Å3 (from single-crystal diffraction data). The mineral was found in a void within the calcite-magnetite phoscorite (enriched in hydroxylapatite and Sc-rich baddeleyite) inside the axial zone of the Kovdor phoscorite-carbonatite pipe. Kampelite forms radiated aggregates (up to 1.5 mm in diameter) of platy crystals grown on the surfaces of crystals of quintinite-2 H in close association with pyrite, bobierrite and quintinite-3 R. Kampelite is colourless, with a pearly lustre and a white streak. The cleavage is perfect on {001}, the fracture is smooth. Mohs hardness is about 1. In transmitted light, the mineral is colourless without pleochroism or dispersion. Kampelite is biaxial + (pseudouniaxial), α ≈ β = 1.607(2), γ = 1.612(2) (589 nm), and 2 V calc = 0°. The calculated and measured densities are 3.28 and 3.07(3) g·cm-3, respectively. The mean chemical composition determined by electron microprobe is: MgO 4.79, Al2O3 0.45, P2O5 31.66, K2O 0.34, Sc2O3 16.17, Mn2O3 1.62, Fe2O3 1.38, SrO 3.44, and BaO 29.81 wt%. The H2O content estimated from the crystal-structure refinement is 7.12 wt%, giving a total of 96.51 wt%. The empirical formula calculated on the basis of P = 6 apfu (atoms per formula unit) is (Ba2.62Sr0.45K0.10Ca0.06)Σ3.23Mg1.60Mn0.28(Sc3.15Fe3+ 0.23Al0.12)Σ3.50(PO4)6(OH)2.61·4.01H2O. The simplified formula is Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O. The mineral easily dissolves in 10% cold HCl. The strongest X-ray powder-diffraction lines [listed as d in Å ( I) ( hkl)] are as follows: 15.80(100)(001), 13.86(45)(002), 3.184(18)(223), 3.129(19)(026), 2.756(16)(402), 2.688(24)(10 10). The crystal structure of kampelite was

Energy transfer mechanism from Gd3+ to Sm3+ in K3Gd(PO4)2:Sm3+ phosphor

International Nuclear Information System (INIS)

Gupta, Palvi; Bedyal, A K; Kumar, Vinay; Khajuria, Y; Sharma, Vishal; Ntwaeaborwa, O M; Swart, H C

2015-01-01

Undoped K 3 Gd(PO 4 ) 2 and trivalent samarium (0.5–2.5 mol%) doped K 3 Gd(PO 4 ) 2 phosphors were synthesized by the solid-state method. The phase formation, optical and luminescence properties were investigated by x-ray diffraction (XRD), diffuse reflectance (DR) spectroscopy, and photoluminescence (PL) spectroscopy. The fluorescence decay spectra of the obtained phosphors were also recorded to study the energy transfer from sensitizer (Gd 3+ ) to activator (Sm 3+ ). Energy transfer effects from sensitizer to activator caused by rare-earth ions were mainly observed in the obtained PL and lifetime spectra. The decay curves of K 3 Gd(PO 4 ) 2 phosphor with different Sm 3+ ions concentrations were found to be non-exponential and the data is well fitted with the Inokuti–Hirayama (I–H) model. The energy transfer parameters such as critical distance for the transfer processes were determined. The Commission Internationale de l’Eclairage (CIE) chromatic coordinates and color-correlated temperature were also determined for the prepared phosphor. (paper)

BaO-Nd2O3-CuOx subsolidus equilibria under carbonate-free conditions at pO2=100 Pa and at pO2=21 kPa

International Nuclear Information System (INIS)

Wong-Ng, W.; Cook, L.P.; Suh, J.; Coutts, R.; Stalick, J.K.; Levin, I.; Huang, Q.

2003-01-01

Subsolidus phase equilibria of the BaO-Nd 2 O 3 -CuO x system at pO 2 =100 Pa (0.1% O 2 volume fraction, 810 deg. C) and at pO 2 =21 kPa (21% O 2 volume fraction, 930 deg. C) have been investigated by applying controlled-atmosphere methods to minimize the presence of carbonate and CO 2 and H 2 O contamination. Under carbonate-free conditions, the BaO-Nd 2 O 3 -CuO x phase diagrams at pO 2 =100 Pa and at pO 2 =21 kPa are similar to one another except for differences in the extent of the solid solutions. Apart from the limiting binary phases, the ternary system consists of three solid solutions and one stoichiometric ternary compound. The first solid solution is the high T c series, Ba 2-x Nd 1+x Cu 3 O 6+z (0.3≥x≥0 at pO 2 =100 Pa; 0.95≥x≥ 0 at pO 2 =21 kPa). At pO 2 =21 kPa, a compositionally dependent phase change was detected, from tetragonal (0.7>x≥0) to orthorhombic (0.95≥x≥0.7). The second solid solution series, the 'brown-phase' Ba 1+x Nd 2-x CuO z , has a narrow homogeneity region (0.10>x≥0 at pO 2 =100 Pa; 0.15>x≥0 at pO 2 =21 kPa). In the high BaO part of the phase diagram, a third solid solution (Ba 2-x Nd x )CuO 3+z (x=0 to ∼ 0.3 at pO 2 =100 Pa; x=0-0.45 at pO 2 =21 kPa) was confirmed, as well as a nominally stoichiometric phase, Ba 4 Nd 2 Cu 2 O z . The latter phase is an insulator, with a structure comprised of unusual CuO 5 linear chains. A significant difference in tie line distribution involving the Ba 2-x Nd 1+x Cu 3 O 6+z superconductor was found under carbonate-free conditions relative to literature studies completed in air. Instead of the BaCuO 2+x -Ba 2+x Nd 4-x Cu 2 O z tie line normally encountered in air, a Ba 2-x Nd 1+x Cu 3 O 6+z -(Ba,Nd) 2 CuO 3+x tie line was established. This tie line substantially expands the field of stability of the Ba 2-x Nd 1+x Cu 3 O 6+z superconductor phase into the BaO-rich region of the phase diagram. Implications for the processing of materials based on the Ba 2-x Nd 1+x Cu 3 O 6+z

Both H4K20 mono-methylation and H3K56 acetylation mark transcription-dependent histone turnover in fission yeast

International Nuclear Information System (INIS)

Yang, Hanna; Kwon, Chang Seob; Choi, Yoonjung; Lee, Daeyoup

2016-01-01

Nucleosome dynamics facilitated by histone turnover is required for transcription as well as DNA replication and repair. Histone turnover is often associated with various histone modifications such as H3K56 acetylation (H3K56Ac), H3K36 methylation (H3K36me), and H4K20 methylation (H4K20me). In order to correlate histone modifications and transcription-dependent histone turnover, we performed genome wide analyses for euchromatic regions in G2/M-arrested fission yeast. The results show that transcription-dependent histone turnover at 5′ promoter and 3′ termination regions is directly correlated with the occurrence of H3K56Ac and H4K20 mono-methylation (H4K20me1) in actively transcribed genes. Furthermore, the increase of H3K56Ac and H4K20me1 and antisense RNA production was observed in the absence of the histone H3K36 methyltransferase Set2 and histone deacetylase complex (HDAC) that are involved in the suppression of histone turnover within the coding regions. These results together indicate that H4K20me1 as well as H3K56Ac are bona fide marks for transcription-dependent histone turnover in fission yeast.

Both H4K20 mono-methylation and H3K56 acetylation mark transcription-dependent histone turnover in fission yeast

Energy Technology Data Exchange (ETDEWEB)

Yang, Hanna [Department of Biological Sciences, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon 34141 (Korea, Republic of); Kwon, Chang Seob [Department of Chemistry and Biology, Korea Science Academy of KAIST, Busan, 614-822 (Korea, Republic of); Choi, Yoonjung, E-mail: jjungii@kaist.ac.kr [Department of Biological Sciences, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon 34141 (Korea, Republic of); Lee, Daeyoup, E-mail: daeyoup@kaist.ac.kr [Department of Biological Sciences, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon 34141 (Korea, Republic of)

2016-08-05

Nucleosome dynamics facilitated by histone turnover is required for transcription as well as DNA replication and repair. Histone turnover is often associated with various histone modifications such as H3K56 acetylation (H3K56Ac), H3K36 methylation (H3K36me), and H4K20 methylation (H4K20me). In order to correlate histone modifications and transcription-dependent histone turnover, we performed genome wide analyses for euchromatic regions in G2/M-arrested fission yeast. The results show that transcription-dependent histone turnover at 5′ promoter and 3′ termination regions is directly correlated with the occurrence of H3K56Ac and H4K20 mono-methylation (H4K20me1) in actively transcribed genes. Furthermore, the increase of H3K56Ac and H4K20me1 and antisense RNA production was observed in the absence of the histone H3K36 methyltransferase Set2 and histone deacetylase complex (HDAC) that are involved in the suppression of histone turnover within the coding regions. These results together indicate that H4K20me1 as well as H3K56Ac are bona fide marks for transcription-dependent histone turnover in fission yeast.

Hydrophosphorylation of substituted alkynes by phosphonic acids

International Nuclear Information System (INIS)

Nifant'ev, E.F.; Solovetskaya, L.A.; Maslennikova, V.I.; Sergeev, N.M.

1987-01-01

Hydrophosphorylation of functionally substituted alkynes by phosphonic acids can be a convenient method for synthesis of functionally substituted mono- and diphosphine oxides. The ease of hydrophosphorylation is determined by the strength of the negative inductive effect of the substituents on the triple bond and the steric factor. The structure of the bis-adducts was confirmed by elementary analysis and the 31 P and 13 C NMR spectra. The 31 P NMR spectrum is an AB two-spin system. The values of the chemical shifts and spin-spin interaction constants 3 J/sub PP/ are in agreement with the data in the literature for similar compounds

Crystal structure of polyphosphates NaCd(PO3)3 and NaMn(PO3)3

International Nuclear Information System (INIS)

Murashova, E.V.; Chudinova, N.N.

1997-01-01

Crystal structure of NaCd(PO 3 ) 3 (1) and NaMn(PO 3 ) 3 (2) isostructural polyphosphates was determined for twin samples. Rhombic lattice parameters of (1): a = 14.678, b = 14.669, c = 14.705 A, sp. gr. P2 1 2 1 2 1 , Z = 16. The structure of compounds is of frame type. Polyphosphate chain with repetition period of 24 PO 4 tetrahedrons contacts with NaO 6 and M 2 O 6 octahedrons by means of common oxygen vertices. Similarities and differences in structure of mentioned polyphosphates and earlier analyzed NaMg(PO 3 ) 3 polyphosphate are noted [ru

One-pot syntheses of Li3V2(PO4)3/C cathode material for lithium ion batteries via ascorbic acid reduction approach

International Nuclear Information System (INIS)

Huang, J.S.; Yang, L.; Liu, K.Y.

2011-01-01

Highlights: → Ascorbic acid (C 6 H 8 O 6 ) was used as reducing agent and organic carbon source. → The strategy shortened the period of material preparation and lowered energy cost. → Li 3 V 2 (PO 4 ) 3 /C was obtained with enhanced electrochemical performance. → Effects of reagents on electrochemical performance of Li 3 V 2 (PO 4 ) 3 were evaluated. - Abstract: Monoclinic Li 3 V 2 (PO 4 ) 3 /C composite synthesized by ascorbic acid reduction method is examined as a cathode material for Li-ion batteries. Transmission electron microscopy (TEM) images show that the nano-size particles are obtained. The reversible capacity of Li 3 V 2 (PO 4 ) 3 /C prepared with LiOH and H 3 PO 4 is 141.2 mAh g -1 after 100 cycles at 1C discharge rate between 3 V and 4.8 V, and the retention rates of discharge capacity is 93.4%. Ascorbic acid plays not only as reduction reagent, but also as carbon sources. This strategy shortens the time of solid state reaction and facilitates the procedure of synthesis. Effects of different precursors materials on the performance of the Li 3 V 2 (PO 4 ) 3 /C are investigated.

Anti-HIV therapy with AZT prodrugs: AZT phosphonate derivatives, current state and prospects.

Science.gov (United States)

Khandazhinskaya, Anastasiya; Matyugina, Elena; Shirokova, Elena

2010-06-01

AIDS, a disease caused by human immunodeficiency virus, was called 'plague of the twentieth century'. 3'-Azido-3'-deoxythymidine (AZT), the first compound approved for the treatment of HIV, is still a mandatory component of treatment schemes. However, its toxicity stimulated a search for new agents. This review presents the history and current state of the design of AZT prodrugs based on its phosphonate derivatives. Although every effort was made to include as many AZT structures bearing phosphonate residues and demonstrate the variety they offer, we also concentrated on the studies performed in our laboratory. Special attention was also paid to AZT 5'-H-phosphonate (phosphazide, Nikavir) approved in the Russian Federation as a drug for the prevention and treatment of HIV infection. The prodrug strategy applied to AZT phosphonate derivatives enriched chemistry, biology and medicine not only with new knowledge, methods and structures, but also with a new anti-HIV drug Nikavir. Currently, study of another phosphonate, AZT 5'-aminocarbonylphosphonate, is underway. Slow release of AZT following oral administration and penetration into cells, decreased toxicity and the lack of cumulative properties make the compounds of this group promising as extended-release forms of AZT.

Fabrication and characterization of mesoporous activated carbon from Lemna minor using one-step H3PO4 activation for Pb(II) removal

International Nuclear Information System (INIS)

Huang, Yang; Li, Shunxing; Lin, Haibin; Chen, Jianhua

2014-01-01

Graphical abstract: - Highlights: • Activated carbon was prepared from Lemna minor using H 3 PO 4 activation. • Materials have higher mesoporosity (92.2%) and more oxygen and nitrogen-containing functional groups. • Materials can remove Pb(II) rapidly with monolayer adsorption capacity (170.9 mg/g). • The adsorption process fitted to Langmuir isotherm and pseudo-first-order kinetic. • Materials could be used as an economical, efficient adsorbent to remove Pb(II) ions. - Abstract: A low cost and locally available material, Lemna minor, was used to fabricate activated carbon using H 3 PO 4 activation. After H 3 PO 4 activation, the L. minor activated carbons (LACs) possess high mesoporosity (92.2%) and a surface area of 531.9 m 2 /g according to Brunauer–Emmett–Teller (BET) analysis. Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectrometer (XPS) analyses reveal the presence of rich hydroxyl, carboxyl, amide and phosphate functional groups on the LACs surface, leading to facile Pb(II) binding to the surface through strong chemisorptive bonds or ion-exchange. The kinetic and equilibrium data were well described by pseudo-first-order model and Langmuir isotherm, with the maximum monolayer adsorption capacity (q m ) 170.9 mg/g at 25 °C. The intra-particle diffusion mechanism was partially responsible for the adsorption. The adsorption process was spontaneous and endothermic with negative ΔG and positive ΔH. The Pb(II)-loaded LACs could be easily regenerated using 0.1-M HCl and reused for seven cycles without significant adsorption capacity reduction. The maximum percentage removal rate for Pb(II) (20 mg/L) was found to be 91.8% within 30 min, at optimum conditions of pH 6.0 and 25 °C. These suggested that the low-cost LACs could be used as a potential adsorbent in the treatment of lead-contaminated water

New equations to calculate temperature correction factors for PO2 in human blood.

Science.gov (United States)

Inaba, H; Ohwada, T; Sato, J; Mizuguchi, T; Hirasawa, H

1986-01-01

Effects of hemoglobin concentration (Hb), pH, and body temperature (T) on the relationships between delta log PO2/delta T and PO2 were studied by means of a mathematical model using a Newton-Raphson iteration method. The functions between delta log PO2/delta T and PO2 were affected by the above three factors. New equations considering the effects of Hb, pH, and T were proposed by modifying the equation reported by Severinghaus: delta log PO2/delta T = (L +(U-L)/(A(vPO237)B + 1))(10(-2) where U = 3.15-0.45(7.4-pH37) L = 0.68-0.09(7.4-pH37) A = 5.86(exp10(0.074(T)-0.294(7.4-pH37)-11))((Hb)0.913) B = 6.33(exp10(-0.0051(T)))((Hb)-0.113) + 0.24(7.4-pH37) and vPO237 is virtual PO237 which may exist when PO237 is corrected to standard conditions (pH = 7.4, BE = 0) by the following equations: vPO237 = PO237(exp10(fB(7.4-pH37)-0.0013(BE))) fB = (PO237/26.6)0.08-1.52 where fB is the Bohr factor. The above equations provided values of delta log PO2/delta T which fit closely to those obtained by the complex iteration method with maximum differences of less than 1.3 X 10(-3) at T = 27, indicating that maximum % errors for PO2 at T (PO2T) are less than 3.0% at T = 27 and that our equations can be applied over a wide range of Hb, pH37 and T.

Synthesis and photoluminescence of Eu3+ and Mn2+ doped double phosphates KMLa(PO4)2 (M = Zn, Mg)

International Nuclear Information System (INIS)

Pan Yuexiao; Zhang Qinyuan; Jiang Zhonghong

2006-01-01

Two compounds, KMgLa(PO 4 ) 2 and KZnLa(PO 4 ) 2 doped with Eu 3+ and Mn 2+ ions, have been synthesized by a conventional solid-state method at 850 deg. C. Structures of KMgLa(PO 4 ) 2 and KZnLa(PO 4 ) 2 have been investigated and confirmed by X-ray diffraction and photoluminescence spectra. The results indicate that the compounds have remained the monoclinic structure of LaPO 4 with space group of C s when (K + , Mg 2+ ) or (K + , Zn 2+ ) could substitute half of the La 3+ ions. Under an ultraviolet source, KMgLa(PO 4 ) 2 :Mn 2+ has shown a bright red phosphorescent color, while KZnLa(PO 4 ) 2 :Mn 2+ has shown an orange-red emission which is assigned to the electronic transition of 4 T 1 ( 4 G)- 6 A 1 ( 6 S) of Mn 2+ in strong crystal field

A comparative structural and electrochemical study of monoclinic Li3V2(PO4)3/C and rhombohedral Li2.5Na0.5V(2−2x/3)Nix(PO4)3/C

International Nuclear Information System (INIS)

Wang, Wenhui; Chen, Zhenyu; Zhang, Jiaolong; Dai, Changsong; Li, Jiajie; Ji, Dalong

2013-01-01

In order to synthesize pure derivative of rhombohedral Li 3 V 2 (PO 4 ) 3 (LVP), lithium-ion batteries materials Li 2.5 Na 0.5 V (2−2x/3) Ni x (PO 4 ) 3 /C (x = 0.03, 0.06, 0.09) and its control, monoclinic Li 3 V 2 (PO 4 ) 3 /C (LVP/C), were prepared by sol–gel method. The samples were investigated by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) spectroscopy, scanning electron microscopy (SEM), Raman spectroscopy, and electrochemical methods. The XRD patterns of Li 2.5 Na 0.5 V (2−2x/3) Ni x (PO 4 ) 3 /C are in good agreement with that of rhombohedral LVP, which indicates that the Na + –Ni 2+ composite doping can change the structure of monoclinic LVP. All the composite doping samples displayed a single flat plateau at 3.7 V in the charge/discharge voltage profile, which is caused by transformation of multi-phase mechanism to single-phase mechanism. For Li 2.5 Na 0.5 V 1.98 Ni 0.03 (PO 4 ) 3 /C, a specific discharge capacity of 108 mAh g −1 was achieved at a 0.5 C charge rate and a 1 C discharge rate, and a 99.0% retention rate of the initial capacity was obtained after 50 cycles

Comparison of Interstitial Fluid pH, PCO2, PO2 with Venous Blood Values During Repetitive Handgrip Exercise

Science.gov (United States)

Hagan, Ronald Donald; Soller, Babs R.; Shear, Michael; Walz, Matthias; Landry, Michelle; Heard, Stephen

2006-01-01

We evaluated the use of a small, fiber optic sensor to measure pH, PCO2 and PO2 from forearm muscle interstitial fluid (IF) during handgrip dynamometry. PURPOSE: Compare pH, PCO2 and PO2 values obtained from venous blood with those from the IF of the flexor digitorum superficialis (FDS) during three levels of exercise intensity. METHODS: Six subjects (5M/1F), average age 29+/-5 yrs, participated in the study. A venous catheter was placed in the retrograde direction in the antecubital space and a fiber optic sensor (Paratrend, Diametrics Medical, Inc.) was placed through a 22 G catheter into the FDS muscle under ultrasound guidance. After a 45 min rest period, subjects performed three 5-min bouts of repetitive handgrip exercise (2s contraction/1 s relaxation) at attempted levels of 15%, 30% and 45% of maximal voluntary contraction. The order of the exercise bouts was random with the second and third bouts started after blood lactate had returned to baseline. Venous blood was sampled every minute during exercise and analyzed with an I-Stat CG-4+ cartridge, while IF fiber optic sensor measurements were obtained every 2 s. Change from pre-exercise baseline to end of exercise was computed for pH, PCO2 and PO2. Blood and IF values were compared with a paired t-test. RESULTS: Baseline values for pH, PCO2 and PO2 were 7.37+/-0.02, 46+/-4 mm Hg, and 36+/-6 mm Hg respectively in blood and 7.39+/-0.02, 44+/-6 mm Hg, and 35+/-14 mm Hg in IF. Average changes over all exercise levels are noted in the Table below. For each parameter the exercise-induced change was at least twice as great in IF as in blood. In blood and IF, pH and PCO2 increases were directly related to exercise intensity. Change in venous PO2 was unrelated to exercise intensity, while IF PO2 decreased with increases in exercise intensity. CONCLUSIONS: Measurement of IF pH, PCO2 and PO2 is more sensitive to exercise intensity than measurement of the same parameters in venous blood and provides continuous

Colorimetric and fluorescent chemosensor for highly selective and sensitive relay detection of Cu2 + and H2PO4- in aqueous media

Science.gov (United States)

Su, Jun-Xia; Wang, Xiao-Ting; Chang, Jing; Wu, Gui-Yuan; Wang, Hai-Ming; Yao, Hong; Lin, Qi; Zhang, You-Ming; Wei, Tai-Bao

2017-07-01

In this manuscript, a new colorimetric and fluorescent chemosensor (T) was designed and synthesized, it could successively detect Cu2 + and H2PO4- in DMSO/H2O (v/v = 9:1, pH = 7.2) buffer solution with high selectivity and sensitivity. When added Cu2 + ions into the solution of T, it showed a color changes from yellow to colorless, meanwhile, the green fluorescence of sensor T quenched. This recognition behavior was not affected in the presence of other cations, including Hg2 +, Ag+, Ca2 +, Co2 +, Ni2 +, Cd2 +, Pb2 +, Zn2 +, Cr3 +, and Mg2 + ions. More interestingly, the Cu2 + ions contain sensor T solution could recover the color and fluorescence upon the addition of H2PO4- anions in the same medium. And other surveyed anions (including F-, Cl-, Br-, I-, AcO-, HSO4-, ClO4-, CN- and SCN-) had nearly no influence on the recognition behavior. The detection limits of T to Cu2 + and T-Cu2 + to H2PO4- were evaluated to be 1.609 × 10- 8 M and 0.994 × 10- 7 M, respectively. In addition, the sensor T also could be served as a recyclable component and the logic gate output was also defined in sensing materials. The test strips based on sensor T were fabricated, which acted as a convenient and efficient Cu2 + and H2PO4- test kits.

Synthesis, crystal structure and optical properties of the catena-metaphosphates Ce(PO3)4 and U(PO3)4

International Nuclear Information System (INIS)

Hoeppe, Henning A.; Daub, Michi

2012-01-01

The catena-metaphosphates of tetravalent cerium and tetravalent uranium were obtained as phase pure crystalline powders by reaction of the respective dioxides with phosphoric acid at 500 C. Ce(PO 3 ) 4 and U(PO 3 ) 4 crystallise in space group C2/c (Z = 16, a Ce = 13.7696(3) Aa, b Ce = 29.7120(7) Aa, c Ce = 8.9269(2) Aa, β Ce = 90.00(1) Aa 3 and a U = 13.786(3) Aa, b U = 29.843(6) Aa, c U = 8.9720(18) Aa, β U = 90.01(3) Aa 3 ). The vibrational and optical spectra of pale yellow Ce(PO 3 ) 4 and emerald-greenish U(PO 3 ) 4 are also reported. (orig.)

Partial exchange of the Li+, Na+ and K+ alkaline cations in the HNi(PO4).H2O layered compound

International Nuclear Information System (INIS)

Escobal, Jaione; Mesa, Jose; Pizarro, Jose; Bazan, Begona; Arriortua, Maria; Rojo, Teofilo

2006-01-01

The exchange of the Li + (1), Na + (2) and K + (3) alkaline cations in the layered HNi(PO 4 ).H 2 O was carried out starting from a methanolic solution containing the Li(OH).H 2 O hydroxide for (1) and the M(OH) (M=Na and K) hydroxides together with the (C 6 H 13 NH 2 ) 0.75 HNiPO 4 .H 2 O phases for (2) and (3). The compounds are stable until, approximately, 280 o C for (1) and 400 deg. C for phases (2) and (3), respectively. The IR spectra show the bands belonging to the water molecule and the (PO 4 ) 3- oxoanion. The diffuse reflectance spectra indicate the existence of Ni(II), d 8 , cations in slightly distorted octahedral geometry. The calculated Dq and Racah (B and C) parameters have a mean value of Dq=765, B=905 and C=3895cm -1 , respectively, in accordance with the values obtained habitually for this octahedral Ni(II) cation. The study of the exchange process performed by X-ray powder diffraction indicates that the exchange of the Li + cation in the lamellar HNi(PO 4 ).H 2 O phase is the minor rapid reaction, whereas the exchange of the Na + and K + cations needs the presence of the intermediate (C 6 H 13 NH 2 ) 0.75 HNiPO 4 .H 2 O intercalate in order to obtain the required product with the sodium and potassium ions. The Scanning electronic microscopy (SEM) images show a mean size of particle of 5μm. The Li + exchanged compound exhibits small ionic conductivity (Ωcm -1 is in the 10 -8 -10 -9 range) probably restrained by the methanol solvent. Magnetic measurements carried out from 5K to room temperature indicate antiferromagnetic coupling as the major interaction in the three phases. Notwithstanding the Li and K phases show a weak ferromagnetism at low temperatures

PEMODELAN KONDUKTIVITAS ION DALAM STRUKTUR Li2Sc3(PO43 (Modeling Ionic Conductivity in Li2Sc3(PO43 Structure

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Akram La Kilo

2011-11-01

Full Text Available ABSTRAK Fasa Li2Sc3(PO43 merupakan material konduktor superionik yang dapat diaplikasikan sebagai baterai yang dapat diisi ulang (rechargeable. Ion Li+ dalam struktur Li2Sc3(PO4 dapat mengalami migrasi dari posisi terisi ke posisi kosong. Penelitian ini telah memodelkan migrasi ion Li+ dalam struktur Li2Sc3(PO4 dengan menggunakan metode bond valence sum (BVS. Metode ini dapat memprediksi bilangan oksidasi suatu atom berdasarkan jarak dengan atom-atom tetangga. Source code berbasis BVS yang digunakan adalah JUMPITER yang mensimulasi efek gaya listrik eksternal yang bertindak pada ion litium sehingga nilai BVS litium dapat dipetakan terhadap jarak. Hasil simulasi menunjukkan bahwa konduksi ion Li+ dapat terjadi pada arah [010], [101], dan [120]. Namun, lintasan konduksi ion Li+ lebih mudah terjadi pada arah [120] atau bidang ab dengan nilai maksimum BVS adalah 0,982. ABSTRACT g-phase of Li2Sc3(PO43 is a lithium super ionic conductor which can be applied as a rechargeable lithium battery. Lithium ions of g-Li2Sc3(PO43 can migrate from occupied site to vacant site. In this research, simulation of Li+ ions migration in the structure of g-Li2Sc3(PO43 carried out using bond valence sum (BVS to predict the oxidation state of Li+ion based on the distance of the ion to neighboring atoms. BVS-based code used JUMPITER to simulate the effect of external electrical force acting on the lithium ions to produce the lithium BVS value which can be mapped to the distance. The simulation results shows that Li+ ion conduction can be occurred on [010], [101], and [120] directions. However, the Li ion conduction pathway occur more easily in the direction of [120] or ab plane with the BVS maximum value is 0.982.

Mechanical and thermal-expansion characteristics of Ca10(PO46(OH2-Ca3(PO42 composites

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Ruseska G.

2006-01-01

Full Text Available Three types of composites consisting of Ca10(PO46(OH2 and Ca3(PO42 with composition: 75% (wt Ca10(PO46(OH2: 25%(wt Ca3(PO42; 50%(wt Ca10(PO46(OH2: 50%(wtCa3(PO42 and 25 %(wt Ca10(PO46(OH2: 75%(wt Ca3(PO42 were the subject of our investigation. Sintered compacts were in thermal equilibrium, which was proved by the absence of hysteresis effect of the dependence ΔL/L=f(T during heating /cooling in the temperature interval 20-1000-200C. Sintered compacts with the previously mentioned composition possess 26-50% higher values of the E-modulus, G-modulus and K-modulus indicating the presence of a synergism effect. Several proposed model equations for predicting the thermal expansion coefficient in dependence of the thermal and elastic properties of the constitutive phases and their volume fractions, given by: Turner, Kerner, Tummala and Friedberg, Thomas and Taya, were used for making correlations between mechanical and thermal-expansion characteristics of the Ca10(PO46(OH2 - Ca3(PO42 composites. Application of the previously mentioned model equations to all kinds of composites leads to the conclusion that the experimentally obtained results for the thermal expansion coefficient are in an excellent agreement with the theoretical calculated values on account of the volume fraction of each constitutive phase and with all applied model equations, with a coefficient of correlation from 98.16-99.86 %.

Preparation and characterization of high surface area activated carbon from Fox nut (Euryale ferox shell by chemical activation with H3PO4

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Arvind Kumar

Full Text Available Activated carbons were prepared from Fox nutshell by chemical activation with H3PO4 in N2 atmosphere and their characteristics were studied. The effects of activation temperature and impregnation ratio were examined. N2 adsorption isotherms characterized the surface area, total pore volume, micropore volume and pore size distribution of activated carbons. Activated carbon was produced at 700 °C with a 1.5 impregnation ratio and one hour of activation time has found 2636 m2/g and 1.53 cm3/g of highest BET surface area and total pore volume, respectively. The result of Fourier-infrared spectroscopy analysis of the prepared activated carbon confirmed that the carbon has abundant functional groups on the surface. Field emission scanning electron micrographs of the prepared activated carbon showed that a porous structure formed during activation. Keywords: Activated carbons, Fox nutshell, Chemical activation, H3PO4, Activated carbon, Surface chemistry, Porous structure

Noninvasive, near infrared spectroscopic-measured muscle pH and PO2 indicate tissue perfusion for cardiac surgical patients undergoing cardiopulmonary bypass

Science.gov (United States)

Soller, Babs R.; Idwasi, Patrick O.; Balaguer, Jorge; Levin, Steven; Simsir, Sinan A.; Vander Salm, Thomas J.; Collette, Helen; Heard, Stephen O.

2003-01-01

OBJECTIVE: To determine whether near infrared spectroscopic measurement of tissue pH and Po2 has sufficient accuracy to assess variation in tissue perfusion resulting from changes in blood pressure and metabolic demand during cardiopulmonary bypass. DESIGN: Prospective clinical study. SETTING: Academic medical center. SUBJECTS: Eighteen elective cardiac surgical patients. INTERVENTION: Cardiac surgery under cardiopulmonary bypass. MEASUREMENTS AND MAIN RESULTS: A near infrared spectroscopic fiber optic probe was placed over the hypothenar eminence. Reference Po2 and pH sensors were inserted in the abductor digiti minimi (V). Data were collected every 30 secs during surgery and for 6 hrs following cardiopulmonary bypass. Calibration equations developed from one third of the data were used with the remaining data to investigate sensitivity of the near infrared spectroscopic measurement to physiologic changes resulting from cardiopulmonary bypass. Near infrared spectroscopic and reference pH and Po2 measurements were compared for each subject using standard error of prediction. Near infrared spectroscopic pH and Po2 at baseline were compared with values during cardiopulmonary bypass just before rewarming commenced (hypotensive, hypothermic), after rewarming (hypotensive, normothermic) just before discontinuation of cardiopulmonary bypass, and at 6 hrs following cardiopulmonary bypass (normotensive, normothermic) using mixed-model analysis of variance. Near infrared spectroscopic pH and Po2 were well correlated with the invasive measurement of pH (R2 =.84) and Po2 (R 2 =.66) with an average standard error of prediction of 0.022 +/- 0.008 pH units and 6 +/- 3 mm Hg, respectively. The average difference between the invasive and near infrared spectroscopic measurement was near zero for both the pH and Po2 measurements. Near infrared spectroscopic Po2 significantly decreased 50% on initiation of cardiopulmonary bypass and remained depressed throughout the bypass and

The Role of pH in PEG-b-PAAc Modification of Gadolinium Oxide Nanostructures for Biomedical Applications

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Eva Hemmer

2012-01-01

Full Text Available Upconversion and near-infrared emitting Gd2O3:Er3+,Yb3+ nanostructured phosphors (nanoparticles and nanorods for applications in bioimaging have been synthesized by precipitation methods and hydrothermal treatment. Variation of the material synthesis conditions (additives and pH allows controlling particle size (40 nm to μm range and rod aspect ratio (5 to 18. It was shown that PEG-b-PAAc (poly(ethylene glycol poly(acrylic acid block polymer is suitable to provide the required chemical durability, dispersion stability, and noncytotoxic behaviour for biomedical applications, where the coating of Gd2O3 with a protecting and biocompatible layer is essential in order to prevent the release of toxic Gd3+ ions. Physicochemical properties of the Gd2O3:Er3+,Yb3+ nanostructures modified with PEG-b-PAAc have been investigated by TG-DTA, FT-IR, and DLS revealing a strong influence of modification conditions, namely, pH of the reaction media, on the nature of the PEG-b-PAAc layer.

Uncommon potential hysteresis in the Li/Li2xVO(H2-xPO4)2 (0 ≤ x ≤ 2) system

International Nuclear Information System (INIS)

Dubarry, M.; Gaubicher, J.; Guyomard, D.; Wallez, G.; Quarton, M.; Baehtz, C.

2008-01-01

Physical and electrochemical investigations of vanadium phosphates, Li 2x VO(H 2-x PO 4 ) 2 (0 + /Li + ionic exchange from VO(H 2 PO 4 ) 2 to Li 2 VO(HPO 4 ) 2 leads to grain decrepitation. Further ionic exchange toward formation of Li 4 VO(PO 4 ) 2 lowers the symmetry. As inferred from potentiodynamic cycling correlated to ex situ and in situ X-ray diffraction (XRD), the system Li/Li 4 VO(PO 4 ) 2 shows several phase transformations that are associated with thermodynamical potential hysteresis that span from roughly 15 mV to more than 1.8 V. Small hysteresis are associated with topotactic reactions and with V V /V IV and V III /V II redox couples. Large potential hysteresis values (>1 V) were observed when oxidation of V III to V IV is involved

The effect of pH on bromelain partition from Ananas comosus by PEG4000/phosphate ATPS

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Juliana Ferrari Ferreira

2011-02-01

Full Text Available In this work, the thermodynamic equilibrium and applying of PEG4000/Phosphate ATPS on the purification of bromelain extracted from pineapple was studied. A rigorous study of the equilibrium curves and tie-line length from PEG4000/phosphate ATPS were done for the pH 6-11 at 25ºC. Results showed that there was augment in the PEG and salt contents with the high pH value from PEG4000/Phosphate ATPS and two-phase formation needed only increasing the PEG content. Two tie-line length at pH 11 from PEG4000/Phosphate ATPS were optimal condition for bromelain purification, one on composition of 14% PEG and 13% salt and other at 12.6% PEG and 12.2% salt, while a 25-62 folds of enzyme was found. SDS-PAGE electrophoreses had one band only, which showed that bromelain was purified. Optimum conditions of bromelain use were found at pH 7 and between 30-40ºC.

Americium and plutonium in phosphates of trigonal structure (NZP type) Am1/3[Zr2(PO4)3] and Pu1/4[Zr2(PO4)3

International Nuclear Information System (INIS)

Bykov, D.M.; Orlova, A.I.; Tomilin, S.V.; Lizin, A.A.; Lukinykh, A.N.

2006-01-01

Am 1/3 [Zr 2 (PO 4 ) 3 ] and Pu 1/4 [Zr 2 (PO 4 ) 3 ] phosphates are synthesized and are investigated by X-ray diffraction method. Compounds have triclinic lattices and lattice parameters are determined. Possibility of actinide inclusion into hollows of framework of NZP type is shown for the first time. It is proposed that inclusion of Pu and Am highly-charged cations into framework hollows decreases crystal structure symmetry up to primitive trigonal one. Rate of Pu leaching from ceramics on Pu 1/4 [Zr 2 (PO 4 ) 3 ] basis are measured [ru

Resolution of TBP-H/sub 2/MBP-HDBP-H/sub 3/PO/sub 4/. Application to UO/sub 2/(NO/sub 3/)/sub 2/-TBP, Th(NO/sub 3/)/sub 4/-TBP, and ZrO(NO/sub 3/)/sub 2/-TBP systems. [Separation of dibutyl phosphoric acid, monobutylphosphoric acid and orthophosphoric acid from tri-butylphosphate

Energy Technology Data Exchange (ETDEWEB)

Pires, M A.F.; Abrao, A

1981-04-01

Several schemes for the separation of dibutylphosphoric acid (HDBP), monobutylphosphoric acid (H/sub 2/MBP) and orthophosphoric acid (H/sub 3/PO/sub 4/) as hydrolytic and radiolytic degradation products from tri-n-butylphosphate (TBP) were studied. For the resolution of a HDBP, H/sub 2/MPB and H/sub 3/PO/sub 4/ mixture in TBP-diluent, or in TBP-diluent-heavy metal nitrate (U-VI, Th-IV or Zr-IV), techniques such as ion exchange chromatography, ion chromatography and separation onto a chromatographic alumina column were investigated. For the identification, determination and analytical resolution following up for the several systems studied, techniques such as refraction index measurement, electrical conductivity measurement, molecular spectrophotometry and gas chromatography were applied. Special emphasis was given to the separation using alumina column where the HDBP acid was retained and eluted selectively for its separation from TBP-varsol-uranyl nitrate mixtures. This analytical procedure was applied to the samples coming from the Uranium Purification Pilot Plant in operation at the Centro de Engenharia Quimica (IPEN).

3 D Co3 (PO4 )2 -Reduced Graphene Oxide Flowers for Photocatalytic Water Splitting: A Type II Staggered Heterojunction System.

Science.gov (United States)

Samal, Alaka; Swain, Smrutirekha; Satpati, Biswarup; Das, Dipti Prakasini; Mishra, Barada Kanta

2016-11-23

The design, synthesis, and photoelectrochemical characterization of Co 3 (PO 4 ) 2 , a hydrogen evolving catalyst modified with reduced graphene oxide (RGO), is reported. The 3 D flowerlike Co 3 (PO 4 ) 2 heterojunction system, consisting of 3 D flowerlike Co 3 (PO 4 ) 2 and RGO sheets, was synthesized by a one-pot in situ photoassisted method under visible-light irradiation, which was achieved without the addition of surfactant or a structure-directing reagent. For the first time, Co 3 (PO 4 ) 2 is demonstrated to act as a hydrogen evolving catalyst rather than being used as an oxygen evolving photoanode. In particular, 3 D flowerlike Co 3 (PO 4 ) 2 anchored to RGO nanosheets is shown to possess dramatically improved photocatalytic activity. This enhanced photoactivity is mainly due to the staggered type II heterojunction system, in which photoinduced electrons from 3 D flowerlike Co 3 (PO 4 ) 2 transfer to the RGO sheets and result in decreased charge recombination, as evidenced by photoluminescence spectroscopy. The band gap of Co 3 (PO 4 ) 2 was calculated to be 2.35 eV by the Kubelka-Munk method. Again, the Co 3 (PO 4 ) 2 semiconductor displays n-type behavior, as observed from Mott-Schottky measurements. These RGO-Co 3 (PO 4 ) 2 conjugates are active in the visible range of solar light for water splitting and textile dye degradation, and can be used towards the development of greener and cheaper photocatalysts by exploiting solar light. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Efficient SO2 capture by amine functionalized PEG.

Science.gov (United States)

Yang, Dezhong; Hou, Minqiang; Ning, Hui; Zhang, Jianling; Ma, Jun; Han, Buxing

2013-11-07

Polyethylene glycols (PEGs) are a class of non-toxic, non-volatile, biocompatible, and widely available polymers. In this work, we synthesized N-ethyl-N-(2-(2-(2-methoxyethoxy)ethoxy)ethyl)-2-aminoethanol (EE3AE) that combines the properties of PEG and amines, and N-decyl-N-ethyl-2-aminoethanol (DEAE). Their performances to capture SO2 were studied at different temperatures, pressures, and absorption times. The interaction between the absorbents and SO2 were characterized by NMR and FTIR techniques. It was demonstrated that both EE3AE and DEAE could absorb SO2 efficiently, and there existed chemical and physical interactions between the absorbents and SO2. In particular, the absorption capacity of EE3AE could be as high as 1.09 g SO2 per g EE3AE at 1 atm. The absorption capacity of EE3AE was much larger than that of DEAE because the ether group in the EE3AE interacted with SO2 more strongly than the alkyl group in the DEAE. The SO2 absorbed by EE3AE could be stripped out by bubbling N2 or by applying a vacuum and the EE3AE could be reused. Moreover, both absorbents exhibited a high SO2-CO2 selectivity.

Influence of preparation conditions on porous structures of olive stone activated by H{sub 3}PO{sub 4}

Energy Technology Data Exchange (ETDEWEB)

Yavuz, Reha; Akyildiz, Hanife [Istanbul Technical University, Chemical and Metallurgical Engineering Faculty, 34469 Maslak, Istanbul (Turkey); Karatepe, Nilguen; Cetinkaya, Eda [Istanbul Technical University, Institute of Energy, Renewable Energy Division, 34469 Maslak, Istanbul (Turkey)

2010-01-15

An olive factory residue was used as a precursor in the preparation of granular activated carbon by chemical activation with H{sub 3}PO{sub 4}. Effects of final activation temperature, time, and H{sub 3}PO{sub 4} concentration used in the impregnation stage on the porous development were investigated. SO{sub 2} adsorption experiments were also performed for some of the activated carbon samples to represent their adsorption performance. Activation at low temperature represented that micropores were developed first at early stages of the temperatures. Mesoporosity developed at around 250 C, enhanced up to 400 C, and then started to decrease due to possibly shrinking of pores. The optimum temperature for olive stone was found to be around 400 C on the basis of total pore volume and BET surface area. It was clearly demonstrated that H{sub 3}PO{sub 4} concentration used in the impregnation stage was not only effective for development of surface area and pore volumes but also an effective tool for tailoring the pore structure and size distribution. (author)

Disorder-derived, strong tunneling attenuation in bis-phosphonate monolayers

International Nuclear Information System (INIS)

Pathak, Anshuma; Bora, Achyut; Tornow, Marc; Liao, Kung-Ching; Schwartz, Jeffrey; Schmolke, Hannah; Jung, Antje; Klages, Claus-Peter

2016-01-01

Monolayers of alkyl bisphosphonic acids (bisPAs) of various carbon chain lengths (C4, C8, C10, C12) were grown on aluminum oxide (AlO x ) surfaces from solution. The structural and electrical properties of these self-assembled monolayers (SAMs) were compared with those of alkyl monophosphonic acids (monoPAs). Through contact angle (CA) and Kelvin-probe (KP) measurements, ellipsometry, and infrared (IR) and x-ray photoelectron (XPS) spectroscopies, it was found that bisPAs form monolayers that are relatively disordered compared to their monoPA analogs. Current–voltage (J–V) measurements made with a hanging Hg drop top contact show tunneling to be the prevailing transport mechanism. However, while the monoPAs have an observed decay constant within the typical range for dense monolayers, β mono   =  0.85  ±  0.03 per carbon atom, a surprisingly high value, β bis   =  1.40  ±  0.05 per carbon atom, was measured for the bisPAs. We attribute this to a strong contribution of ‘through-space’ tunneling, which derives from conformational disorder in the monolayer due to strong interactions of the distal phosphonic acid groups; they likely form a hydrogen-bonding network that largely determines the molecular layer structure. Since bisPA SAMs attenuate tunnel currents more effectively than do the corresponding monoPA SAMs, they may find future application as gate dielectric modification in organic thin film devices. (paper)

First-principles study of paraelectric and ferroelectric CsH2PO4 including dispersion forces: Stability and related vibrational, dielectric, and elastic properties

Science.gov (United States)

Van Troeye, Benoit; van Setten, Michiel Jan; Giantomassi, Matteo; Torrent, Marc; Rignanese, Gian-Marco; Gonze, Xavier

2017-01-01

Using density functional theory (DFT) and density functional perturbation theory (DFPT), we investigate the stability and response functions of CsH2PO4 , a ferroelectric material at low temperature. This material cannot be described properly by the usual (semi)local approximations within DFT. The long-range e--e- correlation needs to be properly taken into account, using, for instance, Grimme's DFT-D methods, as investigated in this work. We find that DFT-D3(BJ) performs the best for the members of the dihydrogenated alkali phosphate family (KH2PO4 , RbH2PO4 , CsH2PO4 ), leading to experimental lattice parameters reproduced with an average deviation of 0.5%. With these DFT-D methods, the structural, dielectric, vibrational, and mechanical properties of CsH2PO4 are globally in excellent agreement with the available experiments (<2 % MAPE for Raman-active phonons). Our study suggests the possible existence of a new low-temperature phase of CsH2PO4 , not yet reported experimentally. Finally, we report the implementation of DFT-D contributions to elastic constants within DFPT.

Examination of the Effects of Activated Carbon Produced from Coal Using Single-Step H3PO4/N2+H2O Vapor Activation on the Adsorption of Bovine Serum Albumin at Different Temperatures and pH Values

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Atakan Toprak

2017-12-01

Full Text Available This study examined protein adsorption equilibrium and kinetics on activated carbon (AC that we obtained from coal by single-step H3PO4 activation under N2+H2O vapor at 800 °C. Surface properties, pore size distribution, and volumes of AC were determined using the volumetric method with N2 adsorption at 77 K. Also, the textural properties were characterized by SEM-EDAX and XRD. The zeta potential values were measured to elucidate the electrostatic interactions between the protein and AC. The obtained AC discrete system was also used as an adsorbent for adsorbing bovine serum albumin (BSA from aqueous solution. The effects of pH (4.0, 5.0, and 7.4 and temperatures (20, 30 and 40 °C on the adsorption of BSA on AC were examined. The surface area, micropore, mesopore and total pore volumes of AC were found to be 1175 m2/g, 0.477 cm3/g, 0.061 cm3/g and 0.538 cm3/g, respectively. The optimum temperature for AC in BSA adsorption was found to be 40 °C and the pH was found to be 4.0. The highest BSA adsorption was found to be 159 mg/g and pH to be 4.0. The experimental equilibrium data were compared with the Langmuir and Freundlich models and found to be compatible with both models. The adsorption process is best described by the pseudo-first-order kinetic model. As a result, it was found out that AC obtained by single step H3PO4/N2+H2O vapor activation is an effective adsorbent for the adsorption of BSA from aqueous solution.

Photoluminescence and thermoluminescence properties of Tb3+ doped K3Gd(PO4)2 nanophosphor

International Nuclear Information System (INIS)

Gupta, Palvi; Bedyal, A.K.; Kumar, Vinay; Khajuria, Y.; Lochab, S.P.; Pitale, S.S.; Ntwaeaborwa, O.M.; Swart, H.C.

2014-01-01

Energy level diagram of Tb 3+ ion in the K 3 Gd(PO 4 ) 2 host lattice. - Highlights: • First time, a detailed TL and PL study on undoped and Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor. • Combustion method was employed to synthesize the Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor. • Mechanism of excitation and emission in undoped and Tb 3+ doped K 3 Gd(PO 4 ) 2 nanophosphor was given. - Abstract: Tb 3+ doped nanoparticulate K 3 Gd(PO 4 ) 2 phosphor was prepared by combustion method using urea as a fuel. The structure, optical and luminescent properties of the phosphor were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy (DRS), photoluminescence spectroscopy (PL), and thermoluminescence (TL) spectroscopy. In undoped K 3 Gd(PO 4 ) 2 , the excitation and emission peaks at 273 nm and 323 nm belongs to the 8 S 7/2 → 6 I J(J=7/2) and 6 P J(J=7/2) → 8 S 7/2 transitions of Gd 3+ while green emission was observed in the Tb 3+ doped K 3 Gd(PO 4 ) 2 . TL study was carried out after exposing the samples to γ-radiations (0.1–5 kGy) in the K 3 Gd(PO 4 ) 2 :Tb 3+ (1.5 mol%). The calculated kinetic parameters were compared with different methods. The band gap of the phosphor was estimated as 5.80 eV. The green shade of the Tb 3+ ion with the CIE coordinates (x, y) as (0.29, 0.54) was in good agreement with the well known green phosphors

Facile sonochemical synthesis and morphology control of CePO{sub 4} nanostructures via an oriented attachment mechanism: Application as luminescent probe for selective sensing of Pb{sup 2+} ion in aqueous solution

Energy Technology Data Exchange (ETDEWEB)

Shiralizadeh Dezfuli, Amin [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Ganjali, Mohammad Reza, E-mail: ganjali@khayam.ut.ac.ir [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Biosensor Research Center, Endocrinology and Metabolism Molecular–Cellular Sciences Institute, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of); Norouzi, Parviz [Center of Excellence in Electrochemistry, Faculty of Chemistry, University of Tehran, Tehran (Iran, Islamic Republic of); Biosensor Research Center, Endocrinology and Metabolism Molecular–Cellular Sciences Institute, Tehran University of Medical Sciences, Tehran (Iran, Islamic Republic of)

2014-09-01

CePO{sub 4} nanostructures with hexagonal phase were controllably synthesized using Ce(NO{sub 3}){sub 3} reaction with NH{sub 4}H{sub 2}PO{sub 4} through a sonochemical method by simply varying the reaction conditions. By adding ethanol and polyethylene glycol (PEG), coral-reef nanostructures (CRNs) were synthesized and controlling over pH caused to nanorods/nanowires. Oriented attachment (OA) is proposed as dominant mechanism on the growth of nanostructures which is in competition with Ostwald ripening (OR). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD) and field-emission scanning electron microscopy (FE-SEM), respectively. The luminescent properties of CePO{sub 4} with different morphologies have been studied. Among the nanostructures, nanoparticles with the highest intensity of fluorescent have been used as luminescent probe for selective sensing of Pb{sup 2+} ion in aqueous solution. - Highlights: • Facile sonochemical method has been used for synthesis of CePO{sub 4} nanostructures. • Coral-reef as a new morphology of nanostructures is introduced. • CePO{sub 4} NPs have been used as luminescent probe for selective sensing of Pb{sup 2+} ion.

pO2 and pCO2 increment in post-dialyzer blood: the role of dialysate.

Science.gov (United States)

Sombolos, Kostas I; Bamichas, Gerasimos I; Christidou, Fotini N; Gionanlis, Lazaros D; Karagianni, Anna C; Anagnostopoulos, Theodoros C; Natse, Taïsir A

2005-11-01

Blood returning from a dialyzer during hemodialysis has a higher pO2 and pCO2 content than blood entering the dialyzer, and this has been attributed to the dialysate. The present study investigates this phenomenon. Acid-base and blood-gas parameters (pH, pO2, pCO2 and HCO3) were measured in three groups of stable chronic hemodialysis patients (A, B, and C) undergoing high-flux hemodialysis. In group A (n = 15), "arterial" (a) and "venous" (v) samples were withdrawn simultaneously before dialysis (samples A0), 5 min after circulation of the blood with the dialysate in the by-pass mode (samples A5), and 5 min after high-flux hemodialysis at a zero ultrafiltration rate (samples A10). In group B (n = 11) (a) and (v) samples were withdrawn simultaneously before dialysis (samples B0), 5 min after isolated-ultrafiltration with closed dialysate ports ("isolated-closed" ultrafiltration) (samples B5), and 5 min after high-flux hemodialysis at a zero ultrafiltration rate (samples B10). In group C (n = 14), after an initial arterial blood sample withdrawal before hemodialysis (sample C0), high-flux hemodialysis at a zero ultrafiltration rate was initiated. Five minutes later, blood and dialysate samples were withdrawn simultaneously from the hemodialysis lines (samples C5). In all cases blood and dialysate (bicarbonate) flow rates were set at 0.300 and 0.700 L/min, respectively. FLX-18 hemodialyzers (membrane PEPA 1.8 m2) were used in this study. Analysis of variance revealed significant changes only in venous samples. A comparison of arterial and venous samples revealed no differences between groups A and B before the initiation of dialysis (A0a vs. A0v and B0a vs. B0v, P = NS). The pO2 content was higher in A5v samples than in A5a samples (83.5 +/- 11.2 vs. 88.8 +/- 14.0 mm Hg, P pO2, pCO2, and HCO3 in comparison to A10v samples (P pO2 and pCO2 values in A5v and A10v samples increased by 6.3% and 12.1% and by 1.29% and 52% in comparison to corresponding values of A5a and A10

Effect of VO43− substitution for PO43− on electrochemical properties of the Li3Fe2(PO4)3 cathode materials

International Nuclear Information System (INIS)

Yang, Yonggang; Zhang, Yongguang; Hua, Zhengshen; Wang, Xin; Peng, Huifen; Bakenov, Zhumabay

2016-01-01

Graphical abstract: VO 4 3− –substituted Li 3 Fe 2 (PO 4 ) 3 samples were prepared by sol-gel method. The VO 4 3− substitution remarkably improves the rate capability and cycling performance of the Li 3 Fe 2 (PO 4 ) 3 due to improved conductivity and enhanced lithium ion diffusion. - Highlights: • Mixed anion effect was used to improve electrochemical properties of Li 3 Fe 2 (PO 4 ) 3 . • The VO 4 3− substitution improved rate capability and cyclability of Li 3 Fe 2 (PO 4 ) 3 . • The Li 3 Fe 2 (PO 4 ) 2.55 (VO 4 ) 0.45 material shows the excellent electrochemical performance. - Abstract: In this research, VO 4 3− substitution was used to improve electrochemical properties of the Nasicon Li 3 Fe 2 (PO 4 ) 3 cathode material. The VO 4 3− substitution resulted in formation of a homogeneous compound Li 3 Fe 2 (PO 4 ) 3-x (VO 4 ) x in a composition range of x ≤ 0.45; further introduction of VO 4 3− led to precipitation of some other phases. It was shown that the VO 4 3− substituted samples presented discharging capacity higher than that of bare non-substituted Nasicon and the reported Ti 4+ and Mn 2+ doped ones. The Li 3 Fe 2 (PO 4 ) 2.55 (VO 4 ) 0.45 material exhibited excellent cycling stability and rate capability, and retained a capacity of 91.8 mAh g −1 after 60 cycles at 2C charge-discharge rate. This value is one of the highest reported to date for the Li 3 Fe 2 (PO 4 ) 3 compound, and was about 48% higher than that of the latter. The electrochemical performance enhancements for the VO 4 3− substituted samples were attributed to the reduction of charge transfer resistance, increase of electrical conductivity, and fast lithium ion diffusion behavior. Hence, the obtained results proved that the VO 4 3− anion substitution for PO 4 3− is a powerful technique to improve the electrochemical performance of the studied Nasicon compound.

Complex phosphates in the Li(Na)3PO4-InPO4 systems

International Nuclear Information System (INIS)

Potapova, A.M.; Zimina, G.V.; Smirnova, I.N.; Novoselov, A.V.; Spiridonov, F.M.; Stefanovich, S.Yu.

2008-01-01

Subsolidus sections in the systems Li 3 PO 4 -InPO 4 (950 deg C) and Na 3 PO 4 -InPO 4 (800, 900, and 1000 deg C) have been studied by X-ray powder diffraction. The compound Li 3 In(PO 4 ) 2 has been synthesized, and the NASICON-type solid solution Li 3(1-x) In 2+x (PO 4 ) 3 (0.67 ≤ x ≤ 0.80) has been found to exist. In the system Na 3 PO 4 -InPO 4 , the solid solution Na 3(1-x) In x/3 PO 4 (0 ≤ x ≤ 0.2) and two complex phosphates exist: Na 3 In(PO 4 ) 2 and Na 3 In 2 (PO 4 ) 3 . These complex phosphates are dimorphic, with the irreversible-transition temperature equal to 675 and 820 deg C, respectively. Na 3 In(PO 4 ) 2 degrades at 920 deg C. Ionic conductivity has been measured in some phases in the system [ru

Crystal structures of Th(OH)PO4, U(OH)PO4 and Th2O(PO4)2. Condensation mechanism of M(IV)(OH)PO4 (M= Th, U) into M2O(PO4)2

International Nuclear Information System (INIS)

Dacheux, N.; Clavier, N.; Wallez, G.; Quarton, M.

2007-01-01

Three new crystal structures, isotypic with β-Zr 2 O(PO 4 ) 2 , have been resolved by the Rietveld method. All crystallize with an orthorhombic cell (S.G.: Cmca) with a = 7.1393(2) Angstroms, b = 9.2641(2) Angstroms, c 12.5262(4) Angstroms, V = 828.46(4) (Angstroms) 3 and Z = 8 for Th(OH)PO 4 ; a = 7.0100(2) Angstroms, b = 9.1200(2) Angstroms, c = 12.3665(3) Angstroms, V 790.60(4) (Angstroms) 3 and Z = 8 for U(OH)PO 4 ; a 7.1691(3) Angstroms, b 9.2388(4) Angstroms, c = 12.8204(7) Angstroms, V 849.15(7) (Angstroms) 3 and Z = 4 for Th 2 O(PO 4 ) 2 . By heating, the M(OH)PO 4 (M Th, U) compounds condense topotactically into M 2 O(PO 4 ) 2 , with a change of the environment of the tetravalent cation that lowers from 8 to 7 oxygen atoms. The lower stability of Th 2 O(PO 4 ) 2 compared to that of U 2 O(PO 4 ) 2 seems to result from this unusual environment for tetravalent thorium. (authors)