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91.
Borut Smodiš 《Mikrochimica acta》1996,123(1-4):303-309
Neutron activation analysis is one of the analytical techniques often used for certification of reference materials. The k0-based method of instrumental neutron activation analysis can also be applied in intercomparison runs in the certification process and therefore it is desirable to know its accuracy in advance. Possible systematic errors related to the application of nuclear data at given neutron flux rate parameters, that can affect the uncertainties of the results obtained by this specific method, are elucidated and error propagation factors calculated for a typical irradiation position in the TRIGA Mark II reactor of the Jozef Stefan Institute. It was found that these uncertainties are at the level of 1–2% on the average. 相似文献
92.
R.K.B GoverN.D. Withers S. AllenR.L. Withers J.S.O. Evans 《Journal of solid state chemistry》2002,166(1):42-48
SnP2O7 is a member of the ZrP2O7 family of materials, several of which show unusual thermal expansion behavior over certain temperature ranges and which show a number of displacive phase transitions on cooling from high temperature. Here we describe the structural properties of SnP2O7 from 100 to 1243 K as determined by X-ray and neutron powder diffraction. These studies reveal that SnP2O7 shows two phase transitions in this temperature range. At room temperature the material has a pseudo-cubic 3×3×3× superstructure. Electron diffraction studies show that the symmetry of this structure is P213 or lower. On warming to ∼560 K it undergoes a phase transition to a structure in which the subcell reflections show a triclinic distortion; above 830 K the subcell reflections show a rhombohedral distortion. Significant hysteresis in cell parameters is observed between heating and cooling. The structure of SnP2O7 is discussed with references to other members of the AM2O7 family of materials. 相似文献
93.
Precise determination of d-spacings and compositional ratio of cellulose Iα and Iβ in various native cellulose samples was successfully carried out by synchrotron-radiated X-ray diffraction and time-of-flight
(TOF) neutron diffraction from quasi-powder specimens. X-ray diffraction peaks were separated by the deconvolution method
using six types of profile function: Gaussian, Lorentzian, intermediate Lorentzian, modified Lorentzian, pseudo-Voigt, and
Pearson VII. In terms of R-factors, the pseudo-Voigt function gave the best fit with the observation, and was used for determination
of d-spacings. The numerical results for Valonia cellulose were: dIα (1 0 0) = 0.613 nm; dIβ (1 1 0) = 0.603 nm; dIβ (1 1 0) = 0.535 nm; dIα (0 1 0) = 0.529 nm; Iα content = 0.65. The differences determined between dIα (1 0 0) and dIβ (1 1 0) and between dIβ (1 1 0) and dIα (0 1 0) were similar to those previously reported. Comparison between unresolved peaks for the two types of cellulose samples
revealed a small but definite difference between dIα (1 1 0) and dIβ (2 0 0). The TOF neutron diffractometry using deuterated samples confirmed this difference.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
94.
This study examines the reagent gas pressure and ion source temperature dependence for dimethyl ether chemical ionization (DME CI) mass spectra recorded with an external source ion trap mass spectrometer (ITMS). Information for better controls of the reagent gas pressure in order to obtain fair CI spectra is provided. The origin of M+? ions observed in DME CIMS is discussed in detail. Furthermore, the ion source temperature effect on the DME CI is also investigated. 相似文献
95.
The alkali sodium ferrate (IV) Na4FeO4 has been prepared by solid-state reaction of sodium peroxide Na2O2 and wustite Fe1−xO, in a molar ratio Na/Fe=4, at 400°C under vacuum. Powder X-ray and neutron diffraction studies indicate that Na4FeO4 crystallizes in the triclinic system P−1 with the cell parameters= a=8.4810(2) Å, b=5.7688(1) Å, c=6.5622(1) Å, α=124.662(2)°, β=98.848(2)°, γ=101.761(2)° and Z=2. Na4FeO4 is isotypic with the other known phases Na4MO4 (M=Ti, Cr, Mn, Co and Ge, Sn, Pb). The solid solution Na4FexCo1−xO4 exists for x=0-1 and we have followed the evolution of the cell parameters with x to determine the lattice parameters of the triclinic cell of Na4FeO4. A three-dimensional network of isolated FeO4 tetrahedra connected by Na atoms characterizes the structure. This compound is antiferromagnetic below TN=16 K. At 2 K the magnetic cell is twice the nuclear cell and the magnetic structure is collinear (μFe=3.36(12) μB at 2 K). This black compound is highly hygroscopic. In water or on contact with the atmospheric moisture it is disproportionated in Fe3+ and Fe6+. The Mössbauer spectra of Na4FeO4 are fitted with one doublet (δ=− 0.22 mm/s, Δ=0.41 mm/s at 295 K) in the paramagnetic state and with a sextet at 8K. These parameters characterize Fe4+ high-spin in tetrahedral FeO4 coordination. 相似文献
96.
Yasuhiro Ono Ryuji IshikawaYuzuru Miyazaki Yoshinobu IshiiYukio Morii Tsuyoshi Kajitani 《Journal of solid state chemistry》2002,166(1):177-181
The layered oxide thermoelectric material β-Na0.67CoO2 has been studied by powder neutron diffraction, electric and magnetic measurements. This compound includes an edge-sharing CoO6 slab and a highly vacant Na+ sheet in a unit cell (space group symmetry C2/m, a=4.9023(4) Å, b=2.8280(2) Å, c=5.7198(6) Å and β=105.964(6)° at 300 K). The evaluated formal valence of cobalt ion, +3.33(1), is ascribed to the coexistence of Co3+ and Co4+ in the ratio 2:1. Polycrystalline β-Na0.67CoO2, a p-type thermoelectric material, exhibits metallic behavior of the electric resistivity below 300 K. The Curie-Weiss-type magnetic susceptibility indicates antiferromagnetic interactions between magnetic cobalt ions in the edge-sharing CoO6 slab. 相似文献
97.
P. Berastegui S. HullF.J. Garc? Garc? J. Grins 《Journal of solid state chemistry》2002,168(1):294-305
The structures of the oxyorthogermanate La2(GeO4)O and the apatite-structured La9.33(GeO4)6O2 have been refined from powder neutron diffraction data. La2(GeO4)O crystallizes in a monoclinic unit cell (P21/c) and is cation stoichiometric in contrast to previous reports. La9.33(GeO4)6O2 crystallizes in a hexagonal unit cell (P63/m) and the powder diffraction data show anisotropic peak broadening that is observed in electron diffraction patterns as incommensurate diffuse spots at hkq reciprocal planes (with q=1.6-1.7) and can be attributed to a correlated disorder in the “apatite channels”. This compound was doped up to a nominal composition close to M2La8(GeO4)6O2 with M=Ca, Sr, Ba. The dopant ions preferentially occupy the 4f sites as the number of La vacancies decreases. The measured ionic conductivity of La9.33(GeO4)6O2 is about 3 orders of magnitude larger than for La2(GeO4)O at high temperatures and decreases with increasing dopant content from the highest value of about 0.16 S cm−1 at 1160 K. 相似文献
98.
Motokawa R Annaka M Nakahira T Koizumi S 《Colloids and surfaces. B, Biointerfaces》2004,38(3-4):213-219
By employing small-angle neutron scattering (SANS), we investigated the microstructures of, poly(N-isopropylacrylamide) (PNIPA)-block-poly(ethylene glycol) (PEG) (NE) in deuterated water D2O, as related to macroscopic behaviors of fluidity, turbidity and synerisis. SANS revealed following results: (i) microphase separation occurs at around above 17 °C in a temperature range of transparent sol below 30 °C. In the microdomain appeared in the transparent sol state, both block chains of PNIPA and PEG are swollen by water; (ii) for the NE solution of polymer concentration Wp > 3.5% (w/v), corresponding to opaque gel above 30 °C, a percolated structure, i.e., network-like domain is formed by NE as a result of macrophase separation due to dehydration of the PNIPA chains. As the temperature increases toward 40 °C, the network domain is squeezed along a direction parallel to the NE interface, which leads to increase of the interfacial thickness given by swollen PEG chains and to the macroscopic synerisis behavior. 相似文献
99.
Substitution of Pb for Bi in the recently characterized mixed-valence lead-platinum oxide PbPt2O4 was attempted and a Pb1−xBixPt2O4 solid solution was obtained for 0≤x≤0.3. Powder X-ray diffraction study showed that all substituted compounds crystallize with similar triclinic unit cell and PbPt2O4 lattice parameters. The structural model of Pb0.7Bi0.3Pt2O4 was refined from powder X-ray diffraction data using the Rietveld method and the results indicate the same crystal structure than PbPt2O4 with one mixed Pb/Bi atomic site. Neutron diffraction realized on the two limit compositions of the solid solution (x=0 and 0.3) allowed to confirm the PbPt2O4 and Pb0.7Bi0.3Pt2O4 stoichiometries. Mean oxidation degree of Pt atoms in the [PtO4] infinite chains decreases from +3 for PbPt2O4 to +2.7 for Pb0.7Bi0.3Pt2O4. Conductivity measurements show a metallic behavior for all the compositions except the limit composition x=0.3 for which a semiconducting behavior appears. 相似文献
100.
Julieta Marrero Griselda Polla Raúl Jiménez Rebagliati Rita Plá Darío Gómez Patricia Smichowski 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
Different techniques were selected for comprehensive characterization of seven samples of fly ashes collected from the electrostatic precipitator of the San Nicolás thermal power plant (Buenos Aires, Argentina). Particle size was measured using laser based particle size analyzer. X-ray diffraction powder (XRD) analysis and scanning electron microscopy (SEM) were used to characterize the mineral phase present in the matrix consisting basically of aluminosilicates and large amounts of amorphous material. The predominant crystalline phases were mullite and quartz. Major and minors elements (Al, Ca, Cl, Fe, K, Mg, Na, S, Si and Ti) were detected by energy dispersive X-ray analysis (EDAX). Trace elements (As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Se, V and Zn) content was quantified by inductively coupled plasma optical emission spectrometry (ICP OES). Different acid mixtures and digestion procedures were compared for subsequent ICP OES measurements of the dissolved samples. The digestion procedures used were: i) a mixture of FH + HNO3 + HClO4 (open system digestion); ii) a mixture of FH + HNO3 (MW-assisted digestion); iii) a mixture of HF and aqua regia (MW-assisted digestion). Instrumental neutron activation analysis (INAA) was employed for the determination of As, Ba, Co, Cr, Ce, Cs, Eu, Fe, Gd, Hf, La, Lu, Rb, Sb, Sc, Sm, Ta, Tb, Th, U and Yb. The validation of the procedure was performed by the analysis of two certified materials namely, i) NIST 1633b, coal fly ash and ii) GBW07105, rock. Mean elements content spanned from 41870 μg g− 1 for Fe to 1.14 μg g− 1 for Lu. The study showed that Fe (41870 μg g− 1) ? V (1137 μg g− 1) > Ni (269 μg g− 1) > Mn (169 μg g− 1) are the main components. An enrichment, with respect to crustal average, in many elements was observed especially for As, V and Sb that deserve particular interest from the environmental and human health point of view. 相似文献