3.

According to ( Hoenig et al.,1996) ,The composition of environmental matrices varies from purely
inorganic (e.g. fly ash) to purely organic (e.g. fats), but generally they are an intermediate
combination of these extremes. This means that total dissolution of samples usually analyzed cannot
be achieved in one step using a single reagent, but often several steps and several reagents are
necessary. The choice of reagents depends on the matrix composition. Organic samples are usually
brought into solution by some type of oxidation process followed by an acid digestion of the residue
obtained, as well as of the

initial inorganic part of the matrix. As most often silicates, carbonates and oxides form the major
components of this residue, hydrofluoric acid is a very important agent (decomposition of the
silicates), together with nitric, hydrochloric, perchloric and sometimes sulphuric and phosphoric
acids. In general, two major groups of procedures may be distinguished

1. Dry ashing procedures, which include ashing at relatively elevated temperatures (450-550°C) by
air oxygen at atmospheric pressure (sometimes using some ashing aids to improve procedure
efficiency and to minimize volatilization losses). Usually many samples can be processed
simultaneously and reproducibly. Also, low temperature ashing (about 100°C) under a low pressure
(about 100 Pa) by activated oxygen (cold plasma) may be included in this group in spite of the actual
absence of commercially available devices.

2. Wet digestion procedures, where the organic part of the sample is oxidized in the aqueous phase
by heating in the presence of oxidizing agents (usually combinations of acids and hydrogen
peroxide).

It also mentioned about fusion procedures using alkali metal hydroxides, carbonates or borates as
melting reagents. They are generally set apart for applications in which the objective is the
determination of main matrix elements in samples which are insoluble in acids. Nevertheless,
alkaline fusions are often used for geological and industrial purposes because they allow a
subsequent efficient solubilization of both main matrix and trace elements. Common methods of
fusion generally require four to eight times as much reagent as sample. The amounts of fluxing
reagents added are tvery important and are consequently a potential source of contamination in
trace element analysis. For this reason the fluxing agents utilized must be of very high purity.
Concerning analysis itself, the possible drastic change of the initial matrix implies particular caution
because the 'new' matrix elements introduced via the fluxing reagents can also become a new
source of interference.
4.

According to ( Hoenig et al.,1996),The most innovative source of energy for wet digestion
procedures is microwaves. Because the heating takes place inside the digestion mixture, microwave
digestion is more efficient than with conventional means of heating. Using microwaves, both the
speed and the efficiency of decomposition for some types of samples considered difficult to
solubilize are often improved. Additionally, automation becomes possible with some
instrumentation. We again distinguish between closed systems (microwave ovens using PTFE
bombs) and open systems (focused microwaves using an open vessel with a reflux, made of
borosilicate glass, quartz or PTFE). The advantage of the latter is the possibility to mineralize larger
amounts of organic samples (up to 2 g). Basically, the temperatures involved in wet oxidation
methods are very much lower than in dry ashing. The volatilization losses or retentions caused by
reactions between the analyte and vessel are thus very much less frequent. On the other hand,
incomplete solubilization of the sample is often reported and the good choice of a procedure and
adequate mineralization agents is critical. Another undesirable mechanism of importance during wet
digestions is the possible coprecipitation of the analyte with a precipitate formed in the digestion
mixture. The best known example is coprecipitation of lead on calcium sulphate precipitates formed
when a sample high in calcium is digested with a mixture containing sulphuric acid.

References

Hoenig, M., & De Kersabiec, A. M. (1996). Sample preparation steps for analysis by atomic
spectroscopy methods: Present status. Spectrochimica Acta - Part B Atomic Spectroscopy, 51(11),
1297–1307. https://doi.org/10.1016/0584-8547(96)01507-8