Why maintaining a very low dilution factor
Analytical chemists are being required to measure lower and lower
levels of trace metals in samples. This frequently requires the analyst
to make measurements near the method detection limit which usually
result in decreased accuracy and precision. Closed-vessel microwave
digestion techniques require a minimum volume of 10 mL to achieve
accurate temperature monitoring of the reaction conditions. Ideally,
modern spectroscopic techniques require samples submitted for
analysis to have acid concentration of 1 to 5% v/v. This requires samples that were digested with 10 mL of acid to be diluted by a
factor of 500 to achieve the 1 to 2% acid content necessary for
ICP analysis. These large dilution factors often result in some of the
analytes becoming non-detectable.
These large dilutions are often overcome by maximizing the
sample size relative to the amount of digestion acid. This approach
works well for samples that do not contain a large amount of organic
material. For samples with high organic content this is usually not an
option because the reaction gases (CO2 and NOx) produced during
the digestion can cause the microwave vessel to vent when larger
sample sizes (greater than 0.5 grams) are used. Recent advances in
understanding of microwave-assisted sample preparation have led to
the development of vessel inside vessel technology as a means to
improving method detection limits for high organic samples.
The Vessel inside vessel technology provides better reaction control.
Controlling reaction kinetics is especially important when trying to
digest large quantities (0.5 to 1.0 g) of organic material because the
potential for auto-catalytic decomposition increases. Moreover, it helps control these self-sustaining
auto-catalytic reactions by providing a heat sink for the energy liberated
during oxidization.