Clay and Refractory Materials Slurries in Inductively Coupled Plasma Optical Emission Spectrometry: Effects of Mechanochemical Synthesis on Emission Intensities of Analytes


  • Mirian C. Santos Universidade Federal de São Carlos
  • Ana Rita A. Nogueira Universidade Federal de São Carlos
  • Joaquín A. Nóbrega Universidade Federal de São Carlos


Mechanochemical synthesis, slurry, ICP OES, clays, refractory materials


Abstract. 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, LiBO2 and Na2CO3, 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 HNO3 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% (Na2CO3) and 583% (LiBO2) compared to the emission signals for analytes present in slurries prepared using samples ground without adding modifier.


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Author Biographies

Mirian C. Santos, Universidade Federal de São Carlos

Departamento de Química

Ana Rita A. Nogueira, Universidade Federal de São Carlos

Departamento de Química

Joaquín A. Nóbrega, Universidade Federal de São Carlos

Departamento de Química


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