Effect of magnesium nitrate vaporization on gas temperature in the graphite furnace

摘要

The vaporization of magnesium nitrate was observed in longitudinally-heated graphite atomizers, using pyrocoated and Ta-lined tubes and filter furnace, Ar or He as purge gas and 10-200-#mu#g samples. A charge coupled device (CCD) spectrometer and atomic absorption spectrometer were employed to follow the evolution of absorption spectra (200-400 nm), light scattering and emission. Molecular bands of NO and NO_2 were observed below 1000 deg C. Magnesium atomic absorption at 285.2 nm appeared at approximately 1500 deg C in all types of furnaces. The intensity and shape of Mg atomization peak indicated a faster vapor release in pyrocoated than in Ta-lined tubes. Light scattering occurred only in the pyrocoated tube with Ar purge gas. At 1500-1800 deg C it was observed together with Mg absorption using either gas-flow or gas-stop mode. At 2200-2400 deg C the scattering was persistent with gas-stop mode. Light scattering at low temperature showed maximum intensity near the center of the tube axis. Magnesium emission at 382.9 383.2 and 383.8 nm was observed simultaneously with Mg absorption only in the pyrocoated tube, using Ar or He purge gas. The emission lines were identified as Mg ~3P deg - ~3D triplet having 3.24 eV excitation energy. The emitting species were distributed close to the furnace wall. The emitting layer was thinner in He than in Ar. The experimental data show that a radial thermal gradient occurs in the cross section of the pyrocoated tube contemporaneously to the vaporization of MgO. This behavior is attributed to the reaction of the sample vapor with the graphite on the tube wall. The estimated variation of temperature within the cross section of the tube reaches more than 300-400 deg C for 10 #mu#g of magnesium nitrate sampled. The increase of gas temperature above the sample originates a corresponding increase of the vaporization rate. Fast vaporization and thermal gradient together cause the spatial condensation of sample vapor that induces the light scattering.