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CENTRO UNIVERSITÁRIO NEWTON PAIVA FACULDADE DE CIÊNCIAS EXATAS E TECNOLÓGICAS CURSO ENGENHARIA QUÍMICA CARLA FRANCIELE LOURENÇO SOUZA ITALO SOARES DA SILVA OLIVEIRA TATIANA CAROLINA DE OLIVEIRA COSTA DESTILAÇÃO FRACIONADA BELO HORIZONTE 2020.2 1. INTRODUÇÃO O espectrômetro FTIR funciona devido a interação das ondas eletromagnéticas com a matéria. A radiação eletromagnética apresenta a dualidade onda-partícula. A natureza ondulatória manifesta-se por meio da interferência, dispersão, polarização e coerência da radiação eletromagnética. A radiação emitida pelo aparelho interage com o material de três maneiras distintas: absorção, emissão e espalhamento de radiação. As moléculas apresentam formas tridimensionais, com distâncias de ligações químicas e ângulos de ligações definidas. A compreensão da estrutura molecular, irá dizer as propriedades de cada material e é de grande importância para seu uso na química. (JUNIOR, 2003) O FTIR é atualmente o modelo mais rápido, preciso, produtivo e mais acessível do que os outros modelos de espectrômetro comparados a ele. Ele é capaz de operar nas três regiões do infravermelho (FIR, MIR e NIR), possibilitando a substituição dos elementos de acordo com a região de interesse. (JUNIOR, 2003) O espectrômetro FTIR é composto por uma unidade é a unidade interferométrica que contém o divisor de feixe, um espelho fixo e um espelho móvel. A imagem 1 mostra o mostra o esquema de um espectrômetro FTIR. (JUNIOR, 2003) Imagem 1 - Esquema de um espectrômetro FTIR Fonte: Canevarolo Junior O espectrômetro FTIR possui vários acessórios acoplados que resultam em um espetro de IR de boa qualidade de amostras de diferentes estados físicos, formas e morfologias. Não é necessária manipulação da amostra para a leitura de seu espectro IR para garantia de resultados satisfatórios. Os modos de espectro mais utilizados são transmissão ou absorção, refletância total atenuada (ATR), refletância difusa (DRIFTS), fotoacústico no infravermelho (PAS), refletância especular e microscopia no infravermelho. (JUNIOR, 2003) A interpretação espectral é feita a partir da análise das características das bandas geradas a partir do gráfico de ondas eletromagnéticas geradas pelo espectrômetro, onde se é observado aspectos como à: intensidade relativa, à largura, à forma, ao deslocamento, ao desdobramento e à frequência da banda. A partir da leitura desses aspectos, é possível obter indicações sobre mudanças estruturais, sobre efeitos de conjugação com grupos adjacentes, os efeitos de ligação de hidrogênio e os acoplamentos com outras vibrações normais na amostra. (JUNIOR, 2003) A transformada de Fourier é importante durante o processo de obtenção do interferograma do espectro IR, pois este passa pela equação da transformada de Fourier, que é feita pelo próprio programa no computador, onde é obtido o espectro de intensidade versus número de ondas, facilitando o processo de leitura e interpretação dos resultados. (JUNIOR, 2003) O processo de Refletância Total Atenuada (ATR) é utilizado geralmente em polímeros em forma de filme, folha plana, chapa plana, líquido ou em solução, em que a amostra está em contato com a superfície de cristal do espectrômetro, com ele é possível se obter espectros IR de boa qualidade. (JUNIOR, 2003) Já o processo de Refletância Difusa (DRIFTS) é usado para se obter o espectro IR de amostras em forma de pó ou material solido com uma boa qualidade. O acessório utilizado para a leitura do material geralmente é acoplado ao espectrômetro, dependendo do modelo do fabricante e consiste em um suporte de amostra cilíndrico de diâmetro aproximado de 13 mm e profundidade aproximada de 3 mm, dois espelhos plano e dois espelhos do tipo elipsoidal geminado cobrindo o suporte de amostra. (JUNIOR, 2003) 2. RESULTADOS E DISCUSSÕES A partir dos dados obtidos em laboratório pela técnica de espectroscopia de infravermelho FTIR, foi possível fazer o gráfico 1, que mostra a relação entre absorbância e número de ondas. Gráfico 1 – Espectro do Epoxi Araldite Fonte: Próprios autores O grupo epóxi geralmente apresenta tem bandas características, que podem ser observadas nas regiões próximas a 1250 cm-1, 950-860 cm-1 e de 865-785 cm-1. A primeira banda, de 1250 cm-1, corresponde a deformação do axial simétrica do anel epóxi. A segunda banda, de 916 cm-1, pode ser atribuída à deformação axial assimétrica do anel. A terceira, de 830 cm-1, é característica à deformação simétrica no plano da ligação C-0-C. (PEREIRA, FILHO, VECCHIA, 2005) A tabela 2 apresenta os principais grupos funcionais característicos do espectro de FTIR. Tabela 2 - Absorções características de grupos funcionais de epóxi Fonte: PEREIRA, FILHO, VECCHIA 3. CONCLUSÕES 4. REFERÊNCIAS CANEVAROLO JUNIOR, Sebastião V.. Técnicas de caracterização de polímeros. 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9.2136999999999997E-2 9.2919000000000002E-2 9.3704999999999997E-2 9.4742999999999994E-2 9.4334000000000001E-2 9.1170000000000001E-2 8.9068999999999995E-2 8.8695999999999997E-2 8.9245000000000005E-2 9.1102000000000002E-2 9.2660999999999993E-2 9.2755000000000004E-2 9.2000999999999999E-2 9.1832999999999998E-2 9.1349E-2 9.0584999999999999E-2 9.1236999999999999E-2 9.24 15999999999998E-2 9.2439999999999994E-2 9.4025999999999998E-2 9.3981999999999996E-2 9.2621999999999996E-2 9.1841999999999993E-2 9.1023999999999994E-2 9.0005000000000002E-2 9.0370000000000006E-2 9.0783000000000003E-2 9.2158000000000004E-2 9.3656000000000003E-2 9.3607999999999997E-2 9.2322000000000001E-2 9.3479000000000007E-2 9.7345000000000001E-2 0.10056900000000001 9.8936999999999997E-2 9.7556000000000004E-2 9.6323000000000006E-2 9.5583000000000001E-2 9.4986000000000001E-2 9.4795000000000004E-2 9.6166000000000001E-2 9.7730999999999998E-2 9.7734000000000001E-2 9.7778000000000004E-2 9.7311999999999996E-2 9.7298999999999997E-2 0.100304 0.106198 0.106097 0.10036299999999999 9.9072999999999994E-2 0.100267 0.10168199999999999 0.102822 0.10255 0.103085 0.103066 0.102862 0.105221 0.10860400000000001 0.111901 0.116718 0.11112900000000001 0.10281700000000001 0.102669 0.104753 0.105585 0.106959 0.11040800000000001 0.11218500000000001 0.110849 0.11099000000000001 0.11133800000000001 0.111232 0.11222500000000001 0.112277 0.111138 0.11115899999999999 0.118007 0.123598 0.11956700000000001 0.11787599999999999 0.12074600000000001 0.118848 0.115992 0.11685 0.120284 0.121943 0.12206400000000001 0.13198499999999999 0.14158699999999999 0.132936 0.124124 0.13012000000000001 0.131025 0.122349 0.117946 0.11792800000000001 0.121963 0.126939 0.140541 0.15223500000000001 0.149981 0.14691699999999999 0.13791800000000001 0.12772 0.124357 0.13083700000000001 0.12986300000000001 0.122826 0.12595300000000001 0.13028100000000001 0.131436 0.130993 0.13003500000000001 0.13033800000000001 0.132408 0.12832499999999999 0.126606 0.12956599999999999 0.1341 0.13650399999999999 0.139847 0.14189499999999999 0.14072299999999999 0.13780500000000001 0.13315099999999999 0.13417499999999999 0.13575999999999999 0.137517 0.13933599999999999 0.14067499999999999 0.14626700000000001 0.149175 0.15130099999999999 0.152554 0.15362100000000001 0.15540599999999999 0.156941 0.15784100000000001 0.15787399999999999 0.15711800000000001 0.15636 0.157748 0.15762899999999999 0.157024 0.156608 0.156282 0.15610299999999999 0.155893 0.15553600000000001 0.15490300000000001 0.154 21399999999999 0.153505 0.152527 0.151341 0.15029899999999999 0.14945800000000001 0.14866299999999999 0.14774599999999999 0.14305000000000001 0.14286499999999999 0.14400199999999999 0.142542 0.14082900000000001 0.13943800000000001 0.13821900000000001 0.13703499999999999 0.136021 0.13502900000000001 0.13411400000000001 0.133238 0.129966 0.12818399999999999 0.13187699999999999 0.132607 0.13349 0.134546 0.13567000000000001 0.13694799999999999 0.13793900000000001 0.13942499999999999 0.141351 0.14264399999999999 0.14535200000000001 0.147374 0.14918699999999999 0.150752 0.15212999999999999 0.15404899999999999 0.16050600000000001 0.161047 0.15757699999999999 0.158272 0.158915 0.16012199999999999 0.159577 0.159946 0.16136500000000001 0.16298199999999999 0.16223099999999999 0.158245 0.16586799999999999 0.16814899999999999 0.17184199999999999 0.17480799999999999 0.174954 0.173453 0.17089599999999999 0.16944500000000001 0.16922499999999999 0.16605300000000001 0.16096299999999999 0.157054 0.15343599999999999 0.15090700000000001 0.148975 0.14542099999999999 0.14176 0.139657 0.13775399999999999 0.136544 0.13575799999999999 0.13470499999999999 0.13344300000000001 0.132713 0.13211300000000001 0.13137399999999999 0.130354 0.12955700000000001 0.12904299999999999 0.12756100000000001 0.12820400000000001 0.12762599999999999 0.127108 0.126995 0.12703600000000001 0.12729799999999999 0.127195 0.12536900000000001 0.12656800000000001 0.12651899999999999 0.12606600000000001 0.12597800000000001 0.126 0.12614400000000001 0.12606700000000001 0.126223 0.126635 0.12675700000000001 0.12976399999999999 0.127248 0.12803 0.12873899999999999 0.12942100000000001 0.13014800000000001 0.13052800000000001 0.13072 0.13105800000000001 0.13224 0.13304299999999999 0.13348499999999999 0.134296 0.13499700000000001 0.13547699999999999 0.13550000000000001 0.13467599999999999 0.13492799999999999 0.138408 0.13902900000000001 0.13653599999999999 0.13674800000000001 0.136519 0.13667399999999999 0.13719999999999999 0.137629 0.137322 0.137242 0.13757900000000001 0.13888800000000001 0.13952600000000001 0.139595 0.13933400000000001 0.138761 0.13778299999999999 0.137485 0.13705899999999999 0.13663600000000001 0.135744 0.13504099999999999 0.13466700000000001 0.13459699999999999 0.13420299999999999 0.13327900000000001 0.131934 0.130747 0.12995799999999999 0.12935199999999999 0.12889999999999999 0.12845999999999999 0.127382 0.119616 0.12052400000000001 0.12606800000000001 0.12618299999999999 0.12596199999999999 0.126113 0.12665199999999999 0.127252 0.127555 0.127745 0.128026 0.12842100000000001 0.12884399999999999 0.129 0.12477100000000001 0.12842600000000001 0.129494 0.129353 0.12893499999999999 0.12873599999999999 0.12898000000000001 0.129439 0.128996 0.12443 0.12568199999999999 0.127138 0.129715 0.13245299999999999 0.128164 0.124056 0.12500600000000001 0.12698999999999999 0.128551 0.128607 0.12789 0.123677 0.122271 0.123304 0.121918 0.12045 0.12075900000000001 0.12339600000000001 0.127112 0.123249 0.121213 0.12003800000000001 0.119073 0.118391 Número de ondas (cm-1) Absorbância (λ)
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