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Presidente Vice-Presidente Secretãrio-Geral Diretor Executivo Diretor CONSELHO DIRETOR DA ACIESP LOl'RIVAL CARMO MONACO Presidente ADOLPHO JOSE MELFI Vice-Presidente LUCIANO FRANCISCO PACHEXX) DO AMARAL Secretãrio-Geral SHIGUEO HATANABE Diretor Executivo GERALDO VICENTINI Diretor Executivo Adjunto e Diretor Tesoureiro Interino CRODOHALDO PAVAN OSCAR SALA MEMBROS EFETIVOS (POR AREA) ALBERTO CARVALHO DA SILVA Biociências LOUKIVAL CARMO MONACO Ciências Aplicadas SÉRGIO MASCARENHAS OLIVEIRA Física VIKTOR LEINZ (IN MEMORIAN) Geociâncias CÂNDIDO LIMA DA SILVA DIAS Matemática LUCIANO FRANCISCO PACHECO DO AMARAL Química MEMBROS SUPLENTES (POR AREA) MARIO RUBENS GUIMARÃES MONTENEGRO - Biociências WALTER BORZANI - Ciências Aplicadas HORÃCIO CARLOS PANEPUCCI - Física APOLPHO JOSÉ MELFI - Geociências GIlüERTO FRANCISCO LOIBEL - Matemática GERALDC VICENTINI - Química PESSOAL ADMINISTRATIVO DA ACIESP MARTA STOCKL RUB IA VALDETE BAUCH SELMA DOMINGUES R. REZENDE MOACIR MORAES PASSOS OSVALDO CESAR DE OLIVEIRA VIII SIMPÓSIO ANUAL DA ACADEMIA DE CIÊNCIAS DO ESTADO DE SAO PAULO Patrocínio FUNDAÇÃO DB AMPARO A PESQUISA DO ESTADO DB SAO PAULO (PAPESP) CONSELHO NACIONAL DE DESENVOLVIMENTO CimilFlO) E TfiCNCXftnCO(CNPq) COMPANHIA DE PROMOÇÃO B PESQUISA DO ESTADO DB SAO PAULO (HWJLET) CONSELHO REGIONAL DE QUÍMICA - 4- REGIÃO (CRQ-45 RBGlAO) Organização e Realização ACADEMIA DE CIÊNCIAS DO ESTADO DB SÃO PAULO Local e Data INSTITUTO DE PESQUISAS TECNOLÓGICAS 9 A 14 DE OUTUBRO DB 1983 Comissão Organizadora GERALDO VICENTINI - Coordenador Geral ADOLFO MAX ROTHSCHILD - Coordenador do tema: "Pesquisa e Desenvolvimento delnsumos para aProdução de Fármacos" LÊA BARBIERI ZINNER - Coordenadora do teroai "Química das Terras Raras" ANDRÉ LUIZ PARANHOS PERCNHNI - Coordenador do tema: "Biologia Celular" ROMEU CARDOSO GUIMARÃES - Coordenador do tema: "Evolução Biológica" I APRESENTAÇÃO O VIII Simpósio Anual da Academia de Ciências do Es- tado de São Paulo realizou-se entre os dias 9 e 14 de outubro de 1983 nas dependências do Instituto de Pesquisas Tecnológi- cas, Cidade Universitária, Universidade de São Paulo, São Pau Io. O evento cientifico, de caráter interdisciplinar, foi rea lizado concomitantemente com o XXIV Congresso Brasileiro de Qulnvica, havendo temas de interesse comum. Os Anais do VIII Simpósio Anual da ACIESP deverão apresentar o material colhido durante os trabalhos, consistin do de conferências plenárias, seminá--'OF , trabalhos originais, mesas redondas, painéis de discussão, etc. No presente volu- me são apresentados duas Conferências Plenárias e um Seminá- rio, que foram ministrados por eminentes cientistas, os pro- fessores Lauri Niinistô, da Helsinki University of Technology, Helsinki, Finlândia e Gregory R, Choppin, da Florida State University, Tallahassee, Florida, U.S.A.. Foram apresentados, oralmente, vinte e cinco trabalhos originais, dos quais somen te catorze estão contidos neste volume dos Anais dedicado ã Química das Terras Raras. Os editores e a Diretoria da ACIESP agradecem às en tldades que patrocinaram a realização do VIII Simpósio (FAPESP, CNPq, PROMOCET, CRQ-4^ região) e a impressão deste volume (FAPESP) e ao Instituto de Pesquisas Tecnológicas pela cessão de seus anfiteatros ÍNDICE 1. APRESENTAÇÃO I 2. CONFERÊNCIAS PLENÁRIAS (PLENARY LECTURES): 2.1. Preparation and Characterization of Rare Earth Lund nescent Compounds - L. Nilnistfi 1 2.2. Solution Chemistry of the Lanthanide Elements - 6. R. Choppin 24 3. SEMINÁRIO (SEMINAR) 3.1. Rare Earth Sulfates and Selenates L. Niinisto 43 4. TRABALHOS ORIGINAIS (ORIGINAL PAPERS) 4.1. Obtenção de Neodlmio e Lantânio de Alta Purezaa par- tir de uma Mistura de Cloretos de Terras Raras (Sepa- ration and Preparation of Highly Pure Neodymium and Lanthanum from a Natural Mixed Rare Earth Chlorides)* C.A.S. Queiroz e A.Abrão 57 4.2. Determinação Individual dos Lantanídeos em fixidos ítrio e Praseodlmio por Espectrofotometria de Abscr. ção Atômica em Forno de Graf it:. (Individual Determi nation of Lanthanidep in Yttrium and Praseodimium Oxides by Graphite Furnace Atomic Absorption Spectro photometry) - C.R.Modenesi e A.Abrão 74 4.3. Determinação de Gd, Sm, Eu e Dy em Compos to.i de Urâi nio por Espectrofotometria de Absorção Atômica em Forno de Grafita (Determination of Gd, Sm, Eu and Dy in Uranium Compounds by Graphite Furnace Atomic Absorption Spectrophotometry) - CR. Modenesi e A. Abrio 87 4.4. Diphenyl-phosphynil-morpholide (DPPM)Latthanide Trifluoroacetate Adducts. Considerations About Preparation and Characterization - L.R.F. Carva lho and D.J.Kim 95 4.5. Addition Compounds Between Lanthanide (III) and Yttrium (III) Methanesulfonates (MS)and 3-picoline- N-oxide (3-picNO) - L.B.Zinnerand J.R.Matos ... 104 4.6. Compostos de Adição entre Alguns Fosfinõxidos e Hexafluorofosfatos de Lantanldeos(III) (Addition Compounds Between some Phosphine-oxidea and Lan thanide (III) Hexafluorophosphates) -A.M.Silva, S.M.Melo, E.F.Souza e M.A.Almeida 115 4.7. Aliphatic Amine Oxides as Ligands. 1. Adducts Trimethylamine-N-oxide with some Lanthanide Per chlorates - L.C.Garla, V.H.Betarello, G.Chieri- cato Jr. and W.F. De Giovani 133 4.8. N,N-Dimethylformamide (DMF) Adducts of Lanthanide Trifluoroacetates - G.Vicentini and M.G. da Sil_ va 145 4.9. Aplicação de Complexos Lantahldeos na Purifica- ção do Di-iso-butilsulfóxido (Application of Lanthanide Complexes in the Purification of Di- iso-butilsulfoxide) - V.K.Lakatos Osório, S. A. Q.Martinez e R.M.X. Silva 156 4.10. Interaction between Diethylenetrithiodiacetic Acid (H2T) and Derivatives and Trivalent Lanthanide Ions. Aspects of the Coordination and Bonding Site - J.E.X.Matos, S.M.Melo and E.M.G.Fontenele 175 4.11. Configuration of Equivalent f Electrons. Some Considerations about the Classification of the Terms. - A.B.Nascimento and G.Vicentini 185 4.12. Considerations about Crystal Field Parameters, k 3+ B , in Nd Complexes in a Cubic Symmetry-A.B. Nascimento, W.N.Brito and G.Vicentini 20S 4.13. Crystal Field Parameters for Diphenylphosphinamide (DPPA) Europium Àdducts of Formula Eu(ClQ.)-.6DPPA and Eu(PF,)3.6DPPA - A.B. Nascimento and 6. Vicen tini 210. 4.14. Utilização de Lantânio como Análogo do Actlnio na sua Determinação em Amostras Ambientais. Avaliação Critica (Use of Lanthanum as Actinivún Analog in De termination of Ambiental Samples. Crytical Valua- tion) -M.J.Campos, H.A.Trindade e E.Penna-Franca... 215 ÍNDICE DE AUTORES Abrão, A., 57, 84, 87 Almeida, M.A., 115 Betarello, V.H., 133 Brito, W.N., 205 Campos, M.J., 215 Carvalho, L.R.F., 95 Chiericato, Jr., G., 133 Choppin, G.R., 24 De Giovani, W.F., 133 Fontenele, E.M.G., 175 Garla, L.C., 133 Kim, D.J., 95. Lakatos Osório, V.K., 156 Martinez, S.A.Q., 156, Matos, J.E.X., 175, Matos, J.R. 104, Melo, S.M., 115, 175 Modenesi, C.R., 74, 87 Nascimento, A.B., 135, 205, 210 Niinistô, L., 1, 43 Penna-Franca, E., 215 Queiroz, C.A.S., 57 Silva, A.M., 115 Silva, M.G., 145 Silva, R.M.X., 156 Souza, E.F., 115 Trindade, H.A., 215 Vicentini, G., 145, 205 Zinner, L.B. 104 .1. PREPARATION AMD CHARACTERIZATION OP RARE EARTH UMINBSCBR COMPOUNDS LAURI NIINIST0 Laboratory of Inorganic and Analytical Chemistry, Helsinki University of Technology, SF-02150 Espoo 15, Finland ABSTRACT The luminescence of rare earths and its Industrial appli- cations are briefly discussed. The synthesis of activated rare earth oxysulfldes and oxyhalides is described. Following anal- ytical techniques for the characterization of the phosphors are discussed: thermal analysis, spark source mass spectrometry, fluorescence spectroscopy, X-ray- diffraction, electron micro- scopy and luminescence lifetime measurements. 1. INTRODUCTION The fifteen elements from lanthanum to lutetium as well as yttrium, and also to some extent scandium, are characteri- zed by great chemical and physical similarities which are due to their electronic configuration. However, the applications of rare earth elements in science and technology are mainly based on their differencies rather than on similarities. This is also true for rare earth luminescent natnrials which have a wide range of applications because rare earth ions in differ- ent hosts result in materials with quite different properties. Some examples of the industrial applications of rare earth luminescence are listed in Table 1. It is mi intention to give in this lecture a brief ac- count, based on our recent work, on two groups of rare earth .2. luminescent compounds, namely the oxysulfides and oxyhalides which both have at the moment several important industrial applications. I shall emphasize the preparation and characteri- zation of these materials but before going further I shall discuss by way of introduction the luminescence phenomenon in rare earth compounds. 2. LUMINESCENCE OF RARE EARTH IONS Luminescence is electromagnetic radiation which is emit- ted from a luminescent material called phosphor when it is subjected to some sort of excitation. Usually form of excita- tion is uv, cathodo, or X-ray radiation but it may be in some cases even heat or friction; this is called thermo- and tribo- luminescence, respectively. Figure 1 illustrates in a diagram- matic way the physical processes which may be involved in luminescence when an activator ion (A) is incorporated in a crystalline host lattice (M) and the system includes also sensi- tizer ions (S). exc, em em. \ / \ / /heat \ heat Tig. 1. The luminescence process in crystalline lattice (M) incorporating activator (A) and sensitizer (S) ions, after Blasse and Bril [1], .3. Tahle 1. Examples of Industrial Applications of Rare Earth Luminescent Materials. TV and CR tubes 3+ Eu :Y2O2S TV red phosphor 3+ Ce :Y3A15O12 flying-spot scanner Lightning applications Eu :YVO, high pressure Hg vapor lamps + Eu sY2O3 three-band fluorescent lamos 3+ 3+ Ce ,Tb :MgAl11019 - " - X-ray screens Eu +tBaFCl X-ray intensifying screens 3+ Tb iGd202S - " - Tb3+*Gd0Br - " - In rare earth compounds luminescence was discovered quite early. Georges Urbain, the discoverer of the last stable rare earth lutetium, reported that trivalent euro- pium in gadolinium oxide host lattice gave efficient lumi- nescent response to both X-ray and UV-excitation. That discovery was madeias early as in 1909 [2].
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