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1

Thermal properties of multinuclear Ti(IV) and Zr(IV) carboxylate derivatives using thermal analysis and variable temperature MS and IR methods

Piszczek P., Grodzicki A., Richert M., Radtke A.

Materials Science Poland

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2005

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Vol. 23, No. 3

663--670

EN

Studies of thermal properties of multinuclear Ti(IV) and Zr(IV) carboxylates of general formulas [Ti8O8(O2CBu)16] (1) and [Zr6O8(O2CBu)12] (2), which can be used as a potential source compounds, to produce TiO2 and ZrO2 thin layers, were carried out. Thermogravimetric methods (TG/DTG/DTA), mass spectrometry (MS-EI), and variable temperature infrared spectroscopy (VT-IR) have been used in order to determine the thermal decomposition pathway, identification of the volatile titanium and zirconium species in vapors, and determination their thermal stability. Moreover applications of Ti(IV) and Zr(IV) compounds in MOCVD experiments, as a potential metal oxide precursors, have been discussed.

2

Synthesis and Characterization of New Thiocyanato Bridged Complexes with the General Formula [MLn}3[Cr(NCS)6]2.mH2O, where M=Cu(II), Ni(II), Co(II); L=Various Substituted Imidazoles

Wrzeszcz G., Dobrzańska L., Grodzicki A., Rozpłoch F.

Polish Journal of Chemistry

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2003

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Vol. 77 / nr 2

147-156

EN

New thiocyanato bridged complexes of the type [CuL4]3[Cr(NCS)6]2_mH2O [L = 1-methylimidazole (1-Meim), 2-methylimidazole (2-Meim), 1,2-dimethylimidazole (1,2- Me2im)] and [M(1-Meim)6]n[{M(1-Meim)4Cr(NCS)6}2n]_mH2O (M = Ni(II), Co(II) were prepared by the reaction of [Cr(NCS)6]3- with the appropriate [MLn]2+ complex in an aqueous solution and characterized by elemental and thermal analysis, IR, UV-VIS, EPR and temperature variable magnetic susceptibility. The presence of NCS bridges between M(II)-Cr(III) centres is evident from IR spectra. The electronic spectra correlate with proposal of different composition of Cu3Cr2 and M3Cr2(M = Ni, Co) systems. The parameters determined from temperature dependence on magnetic susceptibility (80-300 K) indicate weak or negligible antiferromagnetic interaction for obtained Cu(II)-Cr(III), Ni(II)-Cr(III) and Co(II)-Cr(III) systems. Thermal decomposition after dehydration is multistage and yields CuO + CuCrO2 and MIIO+MIICr2O4 as final products, respectively.

3

Synthesis, Spectroscopy and Magnetism of New -Thiocyanato Polynuclear Copper(II)-Chromium(III) Complexes

Dobrzańska L., Wrzeszcz G., Grodzicki A., Rozpłoch F.

Polish Journal of Chemistry

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2001

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Vol. 75, nr 11

1689-1694

EN

New heteropolynuclear complexes with general formula [Cu(diamine)2]3 [Cr(NCS)6]2źnH2O, where diamine = N,N-dimethylethylenediamine (1,2-dmen), N,N-dimethylethylenediamine (1,1-dmen), N,N-diethylethylenediamine (1,2-deen), N,N-diethylethylenediamine (1,1-deen), 1,3-diaminopropane (tn) were obtained by reactions of [Cr(NCS)6]3– with the corresponding cationic Cu(II) complexes: [Cu(diamine)2]2+ and characterized by spectroscopic methods and magnetic measurements. The formation of end-to-end thiocyanato bridges between tetragonal Cu(II) and pseudo-octahedral Cr(III) is evident from IR and UV-VIS spectra by appearance of new components of ni(CN) band and shifts in the absorption maxima assigned to copper d-d transitions in comparison with corresponding mononuclear complexes. The EPR spectra measured at room temperature on solid samples show broad, symmetric signal at g = 2.02–2.03.Variable-temperature magnetic susceptibility measurements reveal the presence of weak antiferromagnetic interactions in [Cu(1,1-deen)2]3[Cr(NCS)6]2H2O and [Cu(tn)2]3[Cr(NCS)6]22H2O.

4

Synthesis and Properties of New Bimetallic Complexes of General Formula: [Ni(diamine)2]3[Cr(NCS)6]2.nH2O

Dobrzańska L., Wrzeszcz G., Grodzicki A., Rozpłoch F.

Polish Journal of Chemistry

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2001

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Vol. 75, nr 6

909-914

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Synthesis and Characterization of Thiocyanato-Bridged Heteropolynuclear Chromium(III)-Copper(II) Complexes

Dobrzańska L., Wrzeszcz G., Grodzicki A., Rozpłoch F.

Polish Journal of Chemistry

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2000

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Vol. 74, nr 2

199-206

EN

Heteropolynuclear thiocyanate-bridged complexes were prepared in the reactions of aqueous solutions of K3[Cr(NCS)6] with copper(II) complexes of the type [CuX4]2+, where X=imidazole (imH), 4-methylimidazole (4-MeimH) and 2X= ethylenediamine (en). Solid products were formulated as (Cu(imH)4)3(Cr(NCS)6)2 *2H2O, (Cu(4-MeimH)4)3(Cr(NCS)6)2 *3H2O and (Cu(en)2)3(Cr(NCS)6)2 *2H2O on the basis of elemental analysis and spectral data (IR,UV-VIS). EPR spectra, variable temperature magnetic susceptibility and thermal properties in air were investigated, indicating that all complexes are polynuclear with thiocyanate bridges, exhibiting Curie-Weiss behavior between 80-300 K. Thermal decomposition is multistage and yields CuO and CuCrO2 as final products.

6

Synthesis and characterization of diantipyrylmethanium salts of some pseudo-tetrahedral anionic copper(II) complexes

Wrzeszcz G., Grodzicki A., Pawlak R., Rozpłoch F.

Polish Journal of Chemistry

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1998

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Vol. 72, nr 10

2232-2241

EN

The tetrachlorocuprate(II), tetrabromocuprate(II) and tetrakis(izothiocyanate)cuprate(II) complexes of diantipyrylmethanium cations have been prepared and formulated as (H2DAM)CuCl4, (H2DAM)CuBr4, and (HDAM)2Cu(NCS)4 on the basis of spectral data (IR, UV-VIS) and elemental analysis. The EPR spectra, variable temperature magnetic susceptibility and thermal properties in air have been investigated. The results indicate for all complexes a distored tetrahedral configuration. All studied complexes exhibited Curie-Weiss behaviour between 80-300 K. Thermal decomposition is a multistage process and yields CuO as final product.

7

Studies of Au(I) complexes with perfluorinated carboxylates and trimethylphosphine

Łakomska I., Grodzicki A., Szłyk E.

Polish Journal of Chemistry

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1998

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Vol. 72, nr 3

492-497

EN

Au(I) complexes of the type RCOOAuL, where R=C6F13, C7F15, C8F17, C9F19, C6F5, OOC(C3F6) and L - trimethylphosphine (Me3P) were synthesized and characterized by spectroscopic (IR, (13)C, (19)F, (31)P NMR) and thermal methods. Spectroscopic results favour two coordinated Au(I) with unidentate bonded trimethylphosphine and carboxylates, whereas in the case of hexafluoroglutarate a dimeric structure has been found. The mode of carboxylates binding was proposed basing on the chemical shift of COO group in (13)C NMR spectra and splitting of COO asymmetric and symmetric vibrations bands. Thermal decomposition proceeds in a multistage way that results in metallic gold. Decomposition temperatures and thermal stability of the studied complexes depend on the length of the perfluorinated chain.

8

Spectroscopic studies of Zn(II) halides complexes with 5,7-disubstituted derivatives of 1,2,4-triazolo-[1,5a]-pyrimidine

Szłyk E., Grodzicki A., Pazderski L., Sitkowski J.

Polish Journal of Chemistry

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1998

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Vol. 72, nr 1

55-60

EN

Complexes of ZnX2 (X=Cl, Br, I, SCN) with 5,7-dimethyl-1,2,4-triazolo-[1,5a]-pyrimidine, 5,7-diphenyl-1,2,4-triazolo-[1,5a]-pyrimidine and 5,7-di-tert-butyl-1,2,4-triazolo-[1,5a]-pyrimidine were prepared and characterized by IR (100-4000 cm-1) and 1H, 13C, 15N NMR spectroscopies. Spectral data suggest pseudo-tetrahedral configuration around Zn(II) atom with N-3 bonded heterocycles. Halides and thiocyanates (N bonded) are in terminal positions.

9

Litostratygrafia, petrografia i mineralogia kenozoicznych piasków złotonośnych Dolnego Śląska.

Grodzicki A.

Fizykochemiczne Problemy Mineralurgii

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1998

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Vol. 32

31-41

PL

Scharakteryzowano wystąpienia złota w luźnych okruchowych skałach występujących na Dolnym Śląsku. Zwrócono uwagę na litostratygrafię, petrografię i mineralogię tych utworów. dla celów ustalania litostratygrafii kenozoicznych osadów złotonośnych został opracowany przez Grodzickiego 'miernik czasu' oparty na zasadzie wzrostu entropii i teorii denudodezagregacji. Autor wyróżnił cztery etapy formowania się osadów złotonośnych. Do etapu I oligoceńsko-neogeńskiego należą osady o najwyższych koncentracjach złota i maksymalnych zawartościach Au w ziarnach. Współczynniki denudodezagregacji D mają tu bardzo wysokie wartości. Do etapu II- preglacyjnego zaliczone są osady o niższych koncentracjach złota, a współczynniki D mają mniejsze wartości. Utwory złotonośne etapu III (plejstoceńskiego) i IV (holoceńskiego) charakteryzują się najniższymi koncentracjami złota i najmniejszymi zawartościami Au w ziarnach.

EN

The paper describes gold occurrences in lose clastic rocks in Lower silesia (SW Poland). They have been exploited since ancient times. Particular attention was paid to lithostratigraphy, pertography and mineralogy , i, e. factor controlling gold concentration in sediments. Denudodisaggregation method was applied in the studies. four stages of gold placers formation were distinguished, with various origin, composition and gold content. According to the author's view, a particular role in formation of gold placers belonged to denudodisaggregation process. Its name proposed by A. Grodzicki, comes from Latin words: 'denudare' - uncover, 'aggregatus' - aggregate, 'disaggregation' - break-up of aggregates into basic particles i.e. monomineral grains. In order to establish lithostratigraphy of Cainozoic gold-bering sediments, A. Grodzicki prepared a time indicator based in the principle of entropy increase and the denudodisaggregation theory. It may be summarised in the following way: a ration of parent polymineral aggregates (A) in sediments to secondary, monomineral grains (Zm) is established and denudodisaggregation coefficients are calculated using suitable formulae give in the paper for individual grain fractions (d) as well as for the entire sediment D. The author distinguished four stages of gold placers formation in Lower Silesia. Differences between them consist in geomorphologic situation, petrographic composition, heavy minerals content, gold concentration and its chemical composition, as well as in denudodisaggregation coefficients D. To the 1 st, Oligocene-Neogene stage, belong sediments with the highest gold concentrations and maximum amounts of Au in grains, The sediments contain petrographic and mineral assemblages highly resistance to chemical an mechanical weathering. D coeffiicients reveal the highest values here. The 2nd, preglacial, stage includes sediments with high gold concentration whose grain contain less Au. They occur as usual on lower geomorphologic levels and their D coefficients are lower. Gold-bearing sediments of the 3rd (Pleistocene) and 4 th (Holocene) stages are charactrised by the lower Au concentrations in grains. They contain petrographic and mineralogical components which have little resistance against chemical and mechanical weathering with lower D coefficients have lower values.