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

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 (C CD) spectrometer and atomic absorption spectrometer were employed to follow the evolution of absorption spectra (200-400 nm), light scattering and emi ssion. Molecular bands of NO and NO2 were observed below 1000 degrees C. Ma gnesium atomic absorption at 285.2 nm appeared at approximately 1500 degree s C in all types of furnaces. The intensity and shape of Mg atomization pea k indicated a faster vapor release in pyrocoated than in Ta-lined tubes. Li ght scattering occurred only in the pyrocoated tube with Ar purge gas. At 1 500-1800 degrees C it was observed together with Mg absorption using either gas-flow or gas-stop mode. At 2200-2400 degrees C the scattering was persi stent with gas-stop mode. Light scattering at low temperature showed maximu m 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 t he pyrocoated tube, using Ar or He purge gas. The emission lines were ident ified as Mg P-3(o)-D-3 triplet having 3.24 eV excitation energy. The emitti ng species were distributed close to the furnace wall. The emitting layer w as thinner in He than in Ar. The experimental data show that a radial therm al gradient occurs in the cross section of the pyrocoated tube contemporane ously to the vaporization of MgO. This behavior is attributed to the reacti on of the sample vapor with the graphite on the tube wall. The estimated va riation of temperature within the cross section of the tube reaches more th an 300-400 degrees 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 cau se the spatial condensation of sample vapor that induces the light scatteri ng. (C) 1999 Elsevier Science B.V. All rights reserved.