Acid Digestion Using Microwave Oven

Table 4.9 Parameters for acid digestion using microwave oven...

The first step in analysing plastics for metals content in polymers by ICP-AES technique is that they must be prepared in solutions that are suitable for nebulization. There are four general methods applicable for sample preparation for metal analysis by ICP-AES and they are solvent dissolution of some plastics dry ashing using a muffle furnace acid digestion using a microwave oven and oxygen bomb combustion. 

ICP-MS measurements— Microwave digestion followed by ICP-MS was performed on SRM 1634c samples. About 0.2 g were digested in microwave oven using 6 mL nitric acid, 1 mL... 

Fadda, S., Rivoldini, A., and Cau, I. (1995). ICP-MS determination of 45 trace elements in whole coal using microwave oven acid digestion for sample preparation. Geostand. Newsl. 19(1), 41. 

Raw foods were freeze-dried and analyzed for carbon isotopes using mass spectrometry. Cooked foods were prepared following historic recipes, then were freeze-dried prior to analysis. For the trace element analysis, foods (both raw and cooked) were wet ashed using nitric acid in Teflon lined pressure vessels and digested in a CEM Microwave oven. Analysis of Sr, Zn, Fe, Ca and Mg was performed using Atomic Absorption Spectrometry in the Department of Geology, University of Calgary. 

Principles and Characteristics Instead of thermal initiation, microwave decomposition may be of use for sample preparation involving combustion or acid digestion. The advantages over thermal initiation lie in the shorter time needed (minutes instead of hours). Microwave oven digestion (MOD) systems are not analytical instruments. Functionally, they are chemical... 

Reactions were performed in sealed thick-walled glass tubes or in Teflon acid-digestion vessels, in domestic microwave ovens [13]. Teflon vessels can be used at pressures up to 14 atm, at temperatures below 250 °C, and are resistant to most commonly used chemicals, although they deform at temperatures >250 °C. 

Most average homes contain a microwave oven. Researchers have taken that same technology and applied it to sample extraction. Using microwave technology with acidic solutions has become a commonplace replacement for traditional acid digests. The sample is placed in a closed, chemical-resistant vessel and heated in a microwave. This process is much faster than hot-plate techniques and has become widely accepted by such agencies as the US EPA. 

More recently, microwave ovens have been used for sample dissolution. The sample is sealed in a Teflon bottle or a specially designed microwave digestion vessel with a mixture of suitable acids. The high-frequency microwave, temperature (ca. 100-250°C) and increased pressure have a role to play in the success of this technique. An added advantage is the significant reduction in sample dissolution time [25, 26],... 

The inspiration for pressure digestion studies came from a US Bureau of Mines report [76], which described how rapid dissolution of some mineral samples could be achieved using a microwave oven to heat samples of an acid mixture contained... 

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