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1.
Anal Chem ; 89(5): 3169-3176, 2017 03 07.
Article in English | MEDLINE | ID: mdl-28221759

ABSTRACT

A new fast decomposition procedure for solid samples was developed. In this study, we investigated decomposition of samples by lithium borates fusion in combination with salicylic acid. The method described shortens the time required for the sample to be digested and loaded to a resin to up to 2 h, and it was especially suitable for alpha spectrometry measurements in emergency situations. Additionally, the method results in high radiochemical recoveries and when compared to other digestion methods (classical digestion utilizing mineral acids, microwave digestion, and lithium borates fusion in combination with polyethylene glycol (PEG)) gives comparable activity concentration values. The method used was applied to various reference materials with inorganic and organic matrices as well as widely varying amounts of uranium radioisotopes content. The results obtained were compared with reference and literature values and show that the proposed method can be successfully implemented on various types of samples.


Subject(s)
Borates/chemistry , Lithium Compounds/chemistry , Salicylic Acid/chemistry , Animals , Bivalvia/chemistry , Bivalvia/metabolism , Microwaves , Polyethylene Glycols/chemistry , Radiometry , Seaweed/chemistry , Seaweed/metabolism , Soil/chemistry , Spectrometry, X-Ray Emission , Uranium/chemistry
2.
Acta Chim Slov ; 62(2): 249-54, 2015.
Article in English | MEDLINE | ID: mdl-26085404

ABSTRACT

Three new crystal forms of a mononuclear cobalt(II) chloride with 3-pyridinemethanol (3PM), CoCl2(3PM)4, have been prepared: triclinic (P1̄) and monoclinic (P21/c) polymorphs and its dihydrate which crystallises in the triclinic P1̄ space group. The three crystal forms differ by the orientation of 3PM ligands in the mononuclear entities and consequently in their packing arrangements. All three forms crystallise concomitantly. Their crystal structures have been determined at 150K.

3.
Acta Crystallogr C ; 68(Pt 12): m359-62, 2012 Dec.
Article in English | MEDLINE | ID: mdl-23221248

ABSTRACT

A new polymorph of a mononuclear nickel(II) acetate complex with 2-(pyridin-2-yl)ethanol ligands, [Ni(CH(3)COO)(2)(C(7)H(9)NO)(2)], has been prepared and structurally characterized. Its molecular structure resembles the structures of two previously reported polymorphs in that the Ni(II) atom is located on an inversion centre and is coordinated by pairs of acetate and 2-(pyridin-2-yl)ethanol ligands. The acetate anions are coordinated in a monodentate manner, while the 2-(pyridin-2-yl)ethanol ligands are coordinated in a bidentate chelating mode involving the endocyclic N atom and the hydroxy O atom of the ligand side chain. A strong bifurcated intramolecular hydrogen-bond interaction was observed involving the hydroxy O atom as donor and both acetate O atoms as acceptors. No classical intermolecular hydrogen-bond contacts were observed. However, the crystal packing is effected through π-π and C-H...π interactions, giving rise to a different packing arrangement. A brief comparison of the three polymorphic forms is presented.

4.
Acta Chim Slov ; 59(3): 478-83, 2012 Sep.
Article in English | MEDLINE | ID: mdl-24061300

ABSTRACT

A new mononuclear nickel(II) acetate with 2-pyridineethanol, Ni(ac)2(2-PyEtOH)2 has been prepared. The reaction product is a mixture of two polymorphic forms that crystallize concomitantly: triclinic (PI) and monoclinic (P21/c). Their structures have been determined at 150 K. The molecular structure of the mononuclear complex shows similar geometry in both polymorphic structures but they differ notably in the arrangement of mononuclear entities in space. The crystal densities are significantly different, nevertheless they behave as concomitant polymorphs.

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