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Neste trabalho foi investigada a aplicacao da sintese mecanoquimica para promover reacoes na amostra e sintetizar novos compostos visando aumentar as intensidades de emissao de elementos presentes em suspensoes de argilas e materiais refratarios quando introduzidas em espectrometro de emissao optica com plasma acoplado indutivamente com configuracao axial. A hipotese formulada e que e possivel gerar compostos mais volateis durante a moagem e esses novos compostos causam aumento da intensidade dos sinais de emissao para os analitos em suspensoes introduzidas no plasma. A acao de dois modificadores, LiBO 2 e Na 2 CO 3 , adicionados durante a etapa de moagem foi investigada. As argilas e materiais refratarios foram moidos juntamente com os modificadores quimicos durante 2 h usando um moinho de bolas de alto impacto com recipiente e bolas de carbeto de tungstenio. As suspensoes foram preparadas dispersando as argilas e os materiais refratarios modificados em solucao 10% v v -1 HNO 3 e, posteriormente, sonicadas em banho de ultra-som para melhorar a homogeneizacao. Os compostos produzidos durante a etapa de moagem foram caracterizados por difracao de raios X e analise termogravimetrica. Ambas as tecnicas indicaram a formacao de novos compostos nas argilas e materiais refratarios por sintese mecanoquimica. Os efeitos da modificacao quimica foram avaliados pelas mudancas nas intensidades de emissao dos analitos Al, Ca, Fe, K, Mg, P, Si e Ti. Ambos modificadores causaram aumento na sensibilidade para todos os analitos de ate 665% (Na 2 CO 3 ) e 583% (LiBO 2 ) quando comparados as intensidades dos sinais de emissao obtidos para os analitos nas suspensoes preparadas com as amostras sem modificacao quimica. The developed work investigated the application of mechanochemical synthesis for promoting reactions in the samples and for synthesizing new compounds for increment of emission intensities of analytes in clays and refractory materials slurries in inductively coupled plasma optical emission spectrometry with axial viewing. The hypothesis is that it is possible to generate more volatile compounds during the grinding step and these new compounds will increase the intensities of emission signals for slurries introduced in the plasma. The action of two chemical modifiers, LiBO 2 and Na 2 CO 3 , added during the grinding step was evaluated. The clays and refractory materials mixed with the chemical modifier were ground for 2 h using a high impact ball mill with a tungsten carbide grinding container and balls. Slurries were prepared by dispersing the modified clays and refractory materials in 10% v v -1 HNO 3 solution and by shaking them in an ultrasonic bath to ensure good dispersion. The compounds produced during the grinding step were characterised by X-ray diffraction and thermogravimetric analysis. Both techniques indicated the formation of new compounds in clays and refractory materials by mechanochemical synthesis. Chemical modification effects were evaluated by changes of the emission intensities of Al, Ca, Fe, K, Mg, P, Si, and Ti. Both modifiers caused increments of sensitivities for all analytes in up to 665% (Na 2 CO 3 ) and 583% (LiBO 2 ) compared to the emission signals for analytes present in slurries prepared using samples ground without adding modifiers.

journal of the brazilian chemical society

Clay and refractory materials slurries in inductively coupled plasma optical emission spectrometry: effects of mechanochemical synthesis on emission intensities of analytes