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X-ray powder diffraction data for holmium nitrate pentahydrate

Published online by Cambridge University Press:  17 August 2012

J. Maixner  and
V. Bartůněk
J. Maixner*
Affiliation:
Central Laboratories, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague 6, Czech Republic
V. Bartůněk
Affiliation:
Department of Inorganic Chemistry, Institute of Chemical Technology Prague, Technická 5, 166 28 Prague 6, Czech Republic
*
a)Author to whom correspondence should be addressed. Electronic mail: jaroslav.maixner@vscht.cz
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Abstract

X-ray powder diffraction data, unit-cell parameters, and space group for the holmium nitrate pentahydrate Ho(NO3)3•5H2O are reported [a = 6.642(8) Å, b = 9.55(2) Å, c = 10.56(2) Å, α = 63.672(1)°, β = 84.622(2)°, γ = 76.085(2)°, unit-cell volume V = 582,74 Å3, Z = 2, space group P-1]. Ho(NO3)3•5H2O is isostructural with ytrium nitrate pentahydrate (PDF 01-75-2104) (ICDD, 2011). All measured lines were indexed and are consistent with the P-1 space group. No detectable impurities were observed.

Keywords

X-ray powder diffractionholmium nitrate pentahydrate
Type
New Diffraction Data
Information
Powder Diffraction , Volume 27 , Issue 3 , September 2012 , pp. 203 - 207
Copyright
Copyright © International Centre for Diffraction Data 2012

I. INTRODUCTION

Holmium (Ho) is an important element from the f-block elements of the periodic table, the so-called lanthanides. Ho has wide use for example in Ho lasers used in medicine (Suardi et al., Reference Suardi, Gallina, Salonia, Briganti, Deho, Zanni, Abdollah, Naspro, Cestari, Guazzoni, Rigatti and Montorsi2009; Helfand et al., Reference Helfand, Manvar, Auffenberg, Blackwell, Hartman and McVary2010) and in magnetic resonance imaging (MRI) contrast agents (Norek and Peters, Reference Norek and Peters2011). Ho compounds have interesting optical properties, such as changing of colors under different light sources, which could be used, for example, in glasses (Farok et al., Reference Farok, Saunders, Lambson, Kruger, Senin, Bartlett and Takel1996). Holmium oxide is used in spectrophotometry such as calibration filter (Macdonald, Reference Macdonald1964; Travis et al., Reference Travis, Zwinkels, Mercader, Ruiz, Early, Smith, Noel, Maley, Kramer, Eckerle and Duewer2002).

Holmium nitrate is usually a pale pink or pale yellow substance depending on light source similar to holmium oxide. It is usually in the form of pentahydrate. It is soluble in water and stable in air, and therefore is a suitable precursor for various chemical reactions (Yan and Chen, Reference Yan and Chen2001; Fox et al., Reference Fox, Ball, Harrington, Rollins and Wai2005).

II. EXPERIMENTAL

A. Synthesis

Holmium nitride was prepared by reaction of diluted (20 wt%) nitric acid with an abundant amount of holmium oxide. After reaction the solution has neutral pH. This solution was subsequently evaporated at a temperature of about 50 °C in an evaporator. When crystals started to form, the solution was removed from the evaporator and cooled to room temperature. Crystals obtained from the solution after filtration, were dried in air. The nitric acid used in this study was of p.a. quality, and holmium oxide (99.9% purity) was purchased from LACHEMA. All chemicals were used as received without further purification.

Formation of holmium nitride in the form of pentahydrate was confirmed by its absolute calcination in the furnace. The sample was heated to 1000 °C at 5 °C/min and then cooled spontaneously. Only holmium oxide remained (Balboul, Reference Balboul2000). The rest of the sample (57%) corresponds to absolute calcination of holmium oxide pentahydrate (Balboul, Reference Balboul2000).

B. Powder data collection

The diffraction pattern for holmium nitrate pentahydrate [Ho(NO3)3•5H2O] was collected at room temperature using an X'Pert PRO θ–θ powder diffractometer with parafocusing Bragg–Brentano geometry and CuKα 1 radiation (λ = 1.5406 Å, generator setting: 40 kV, 30 mA). An ultrafast X'Celerator detector was employed to collect XRD data over the angular range from 4° to 80° 2θ with a step size of 0.017° 2θ and a counting time of 81.28 s/step. The software package HighScore Plus V 3.0d (PANalytical, Almelo, Netherlands) was used to analyze the data, to fit the background, and to eliminate the Kα 2 component. The top of smoothed peak method was used to determine the peak positions and intensities of the diffraction peaks. Automatic indexing of the experimental XRD pattern was performed using DICVOL04 (Boultif and Louër, Reference Boultif and Louër2004).

III. RESULTS

The experimental powder diffraction pattern is depicted in Figure 1. Automatic indexing of results obtained using DICVOL04 show that Ho(NO3)3•5H2O is triclinic with space group P-1 and unit-cell parameters: a = 6.642(8) Å, b = 9.55(2) Å, c = 10.56(2) Å, α = 63.672(1)°, β = 84.622(2)°, γ =76.085(2)°, unit-cell volume V = 582,74 Å3, Z = 2, space group P-1 . The figures of merits are F 30 = 37.1(0.0165, 49) (Smith and Snyder, Reference Smith and Snyder1979) and M 20 = 12.3 (de Wolff, Reference de Wollf1968). All lines were indexed (Table I) and are consistent with the P-1 space group.

Figure 1. X-ray powder diffraction pattern of the Ho(NO3)3•5H2O, using CuKα 1 radiation (λ = 1.5406 Å).

TABLE I. Indexed X-ray powder diffraction data for Ho(NO3)3 • 5H2O. Only the peaks with I rel of 1 or greater are presented [a = 6.642(8) Å, b = 9.55(2) Å, c = 10.56(2) Å, α = 63.672(1)°, β = 84.622(2)°, γ = 76.085(2)°, unit-cell volume V = 582,74 Å3, Z = 2, space group P-1]. All lines were indexed and are consistent with the P-1 space group. The d-values were calculated using CuK α 1 radiation (λ = 1.5406 Å).

ACKNOWLEDGEMENTS

This work was supported by grant from the Grant Agency of the Czech Republic (GAČR 104/09/1497) and by Grant from the Ministry of Education Youth and Sports of the Czech Republic (MSM 6046137302).

References

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Figure 0

Figure 1. X-ray powder diffraction pattern of the Ho(NO3)3•5H2O, using CuKα1 radiation (λ = 1.5406 Å).

Figure 1

TABLE I. Indexed X-ray powder diffraction data for Ho(NO3)3 • 5H2O. Only the peaks with Irel of 1 or greater are presented [a = 6.642(8) Å, b = 9.55(2) Å, c = 10.56(2) Å, α = 63.672(1)°, β = 84.622(2)°, γ = 76.085(2)°, unit-cell volume V = 582,74 Å3, Z = 2, space group P-1]. All lines were indexed and are consistent with the P-1 space group. The d-values were calculated using CuK α1 radiation (λ = 1.5406 Å).