Closed vessel microwave-assisted wet digestion with simultaneous control of pressure and temperature in all vessels |
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Authors: | M Zischka Peter Kettisch Andreas Schalk and Günter Knapp |
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Institution: | (1) Institute for Analytical Chemistry, Micro- and Radiochemistry, Technical University Graz, Technikerstrasse 4, A-8010 Graz, Austria, AT;(2) Anton Paar GmbH, K?rtnerstra?e 322, A-8052 Graz, Austria, AT |
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Abstract: | A novel system for microwave-assisted wet digestion in closed vessels is described. Six pressure vessels made of quartz or
Hostaflon? TFM are placed in a special rotor in a microwave oven. During sample decomposition the pressure and temperature are measured
in each vessel, and the data are transferred from the rotor by means of infrared light to the control unit. This means that
no pneumatic or electronic connections to the vessels need to be established, providing very easy handling. The temperature
history of each vessel is recorded; so the progress of each sample digestion may be reconstructed later on. Thus the requirements
for quality control in sample digestion are available for the first time. For sample digestion at 75 bar and up to 280° C,
quartz vessels with 50 mL volume are used. Depending on the matrix, the maximum sample loading capacity is 1.2 g. TFM-vessels
with 100 mL volume work at 30 bar up to 240° C. The performance of the digestion system was tested with twelve standard reference
materials. The results closely matched the certified values.
Received: 18 September 1997 / Revised: 3 November 1997 / Accepted: 6 November 1997 |
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