Radiation damage to lyophilized mineral solutions during electron probe analysis: quantitative study of chlorine loss...

The quantitative effects of beam current-density and sample mass-thickness on the loss of chlorine which occurs from lyophilized solutes of micro-droplets of mineral salt solutions irradiated in an electron probe analyser were studied. Results are reported for chlorine loss from lyophilized deposits with mass-thickness varying between 5 and 50 mg mm-2 for NaCl salts and 5 and 80 mg mm-2 for KCl salts. Electron accelerating voltage was kept constant at 15 kV. The range of beam current-density (I/S, current/sample surface area) was from 0.1 to 1.5 A mm-2. Samples were irradiated for 1200 s. The results show that under some conditions there is a period of stable chlorine signal before chlorine loss occurs. This is observed between 0.1 and 1 A mm-2, for a period which can last several hundred seconds depending on beam current-density and sample mass-thickness. For each value of I/S, however, no stable chlorine signal can be observed for samples whose mass-thickness exceeds a value negatively correlated with I/S. The curves of decrease of characteristic chlorine X-ray signal (expressed as per cent of count rate in the initial counting interval) versus irradiation time can be fitted by the sum of two exponentials with half lives T1 and T2. In NaCl, T1 and T2 values are highly correlated with I/S but not with mass-thickness. In KCl, T1 is correlated only with mass-thickness and T2 only with I/S. Mixing plasma with mineral solutions prevents chlorine loss.