Serveur d'exploration sur le nickel au Maghreb

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Decomposition thermique et etude vibrationnelle de NiNa4(P3O9)2.6H2O

Identifieur interne : 000A15 ( Main/Exploration ); précédent : 000A14; suivant : 000A16

Decomposition thermique et etude vibrationnelle de NiNa4(P3O9)2.6H2O

Auteurs : K. Sbai [Maroc] ; A. Atibi [Maroc] ; A. Charaf [Maroc] ; M. Radid [Maroc] ; Amor Jouini [Tunisie]

Source :

RBID : Pascal:02-0569748

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English descriptors

Abstract

We have studied the dehydration and the calcination under atmospheric pressure of cyclo-triphosphate tetrahydrate of nickel and sodium, NiNa4(P3O9)2.6H2O, between 25 and 700°C by thermal analyses (TG, DTA) infrared spectrometry and X-ray diffraction. This study allows us the identification and the crystallographic characterization of a new phase, NiNa4(PO3)6, obtained between 350 and 450°C. NiNa4(PO3)6 crystallizes in the triclinic system, P-1, with the following unit cell parameters a=6.157(3) Å, b=6.820(6) A, c=10.918(6) A, α=80.21(5)°, β=97.80(9)°, γ=113.49(3)°, V=409.8 Å3, Z=1, M(19)=25 and F(19)=48 (0.0095; 42). The calcination of NiNa4(PO3)6, between 500 and 600°C, leads to a mixture of long-chain polyphosphates NiNa(PO3)3 and NaPO3. The kinetic characteristics of the dehydration of NiNa4(P3O9)2.6H2O were determined and discussed. The vibrational spectrum of the title compound, NiNa4(P3O9)2.6H2O, was interpreted in the domain of the stretching vibrations of the P3O9 rings, on the basis of its crystalline structure and in the light of the calculation of the normal IR frequencies of the P3O9 ring with D3h symmetry.


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Le document en format XML

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<title xml:lang="fr" level="a">Decomposition thermique et etude vibrationnelle de NiNa
<sub>4</sub>
(P
<sub>3</sub>
O
<sub>9</sub>
)
<sub>2</sub>
.6H
<sub>2</sub>
O</title>
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<title xml:lang="fr" level="a">Decomposition thermique et etude vibrationnelle de NiNa
<sub>4</sub>
(P
<sub>3</sub>
O
<sub>9</sub>
)
<sub>2</sub>
.6H
<sub>2</sub>
O</title>
<author>
<name sortKey="Sbai, K" sort="Sbai, K" uniqKey="Sbai K" first="K." last="Sbai">K. Sbai</name>
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<inist:fA14 i1="01">
<s1>Laboratoire de Recherches de Chimie-Physique Générale, Faculté des Sciences Ben M'Sik, B.P. 7955</s1>
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<sZ>1 aut.</sZ>
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<sZ>3 aut.</sZ>
<sZ>4 aut.</sZ>
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<author>
<name sortKey="Atibi, A" sort="Atibi, A" uniqKey="Atibi A" first="A." last="Atibi">A. Atibi</name>
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<s1>Laboratoire de Recherches de Chimie-Physique Générale, Faculté des Sciences Ben M'Sik, B.P. 7955</s1>
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<title level="j" type="main">Journal of thermal analysis and calorimetry</title>
<title level="j" type="abbreviated">J. therm. anal. calorim.</title>
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<title level="j" type="main">Journal of thermal analysis and calorimetry</title>
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<textClass>
<keywords scheme="KwdEn" xml:lang="en">
<term>Cyclophosphate</term>
<term>Differential thermal analysis</term>
<term>Hydrates</term>
<term>Infrared spectrometry</term>
<term>Nickel Metaphosphates</term>
<term>Pyrolysis</term>
<term>Raman spectrometry</term>
<term>Sodium Metaphosphates</term>
<term>Thermal analysis</term>
<term>Thermogravimetry</term>
<term>X ray diffraction</term>
</keywords>
<keywords scheme="Pascal" xml:lang="fr">
<term>Pyrolyse</term>
<term>Nickel Métaphosphate</term>
<term>Sodium Métaphosphate</term>
<term>Phosphate cyclique</term>
<term>Hydrate</term>
<term>Spectrométrie Raman</term>
<term>Spectrométrie IR</term>
<term>Diffraction RX</term>
<term>Analyse thermique</term>
<term>Analyse thermique différentielle</term>
<term>Thermogravimétrie</term>
<term>NiNa4(P3O9)2</term>
<term>Na Ni O P</term>
<term>Cyclotriphosphate</term>
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<front>
<div type="abstract" xml:lang="en">We have studied the dehydration and the calcination under atmospheric pressure of cyclo-triphosphate tetrahydrate of nickel and sodium, NiNa
<sub>4</sub>
(P
<sub>3</sub>
O
<sub>9</sub>
)
<sub>2</sub>
.6H
<sub>2</sub>
O, between 25 and 700°C by thermal analyses (TG, DTA) infrared spectrometry and X-ray diffraction. This study allows us the identification and the crystallographic characterization of a new phase, NiNa
<sub>4</sub>
(PO
<sub>3</sub>
)
<sub>6</sub>
, obtained between 350 and 450°C. NiNa
<sub>4</sub>
(PO
<sub>3</sub>
)
<sub>6</sub>
crystallizes in the triclinic system, P
<sub>-1</sub>
, with the following unit cell parameters a=6.157(3) Å, b=6.820(6) A, c=10.918(6) A, α=80.21(5)°, β=97.80(9)°, γ=113.49(3)°, V=409.8 Å
<sup>3</sup>
, Z=1, M(19)=25 and F(19)=48 (0.0095; 42). The calcination of NiNa
<sub>4</sub>
(PO
<sub>3</sub>
)
<sub>6</sub>
, between 500 and 600°C, leads to a mixture of long-chain polyphosphates NiNa(PO
<sub>3</sub>
)
<sub>3</sub>
and NaPO
<sub>3</sub>
. The kinetic characteristics of the dehydration of NiNa
<sub>4</sub>
(P
<sub>3</sub>
O
<sub>9</sub>
)
<sub>2</sub>
.6H
<sub>2</sub>
O were determined and discussed. The vibrational spectrum of the title compound, NiNa
<sub>4</sub>
(P
<sub>3</sub>
O
<sub>9</sub>
)
<sub>2</sub>
.6H
<sub>2</sub>
O, was interpreted in the domain of the stretching vibrations of the P
<sub>3</sub>
O
<sub>9</sub>
rings, on the basis of its crystalline structure and in the light of the calculation of the normal IR frequencies of the P
<sub>3</sub>
O
<sub>9</sub>
ring with D
<sub>3h</sub>
symmetry.</div>
</front>
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<affiliations>
<list>
<country>
<li>Maroc</li>
<li>Tunisie</li>
</country>
<region>
<li>Gouvernorat de Monastir</li>
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<name sortKey="Sbai, K" sort="Sbai, K" uniqKey="Sbai K" first="K." last="Sbai">K. Sbai</name>
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<name sortKey="Radid, M" sort="Radid, M" uniqKey="Radid M" first="M." last="Radid">M. Radid</name>
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<region name="Gouvernorat de Monastir">
<name sortKey="Jouini, A" sort="Jouini, A" uniqKey="Jouini A" first="A." last="Jouini">Amor Jouini</name>
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