Total (total) method

(Ref: Method 3052, December 1996)

This method is applicable to the microwave-assisted acid extraction/dissolution method

of sediments, sludges, soils and oils for the following elements
Al* Sb* As Ba* Be* B Cd Cr* Co Cu Fe* Pb Mg*
Mn Hg Mo Ni K Se Ag* Na Sr Tl V* Zn
 Elements which typically require addition of HCl for better performance. However, hydrochloric
acid is known to interfere with some instrumental analysis methods such as flame atomic
absorption (FLAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES).
The presence of hydrochloric acid may be problematic for graphite furnace atomic absorption
(GFAA) and inductively coupled plasma mass spectrometry (ICP-MS).

Methodology
1. Take 0.500gm soil in a microwave vessel and add 9 ± 0.1 ml conc. nitric acid and
3 ± 0.1 ml conc. hydrofluoric acid under fume hood. Samples with higher
concentrations of silicon dioxide (> 70%) may require higher concentrations of
hydrofluoric acid (> 3 ml HF). Alternatively samples with lower concentrations of
silicon dioxide (<10% to 0%) may require much less hydrofluoric acid (0.5 ml to
0 ml).
2. Seal the vessel according to the manufacturer’s direction.
3. The digestion period should be 15 min: the temperature of each sample should
rise to 180 ± 5oC in 5.5 ± 0.25 and remain at 180 ± 5oC for 9.5 min.
4. At the end of the microwave digestion, allow the vessel to cool for a minimum of
5 min before removing them from the microwave system. When sufficiently cool
to handle, carefully uncap the vessels.
5. To make the digested sample particle free do the filtration and dilute the digest to
a known volume.
6. The digest is now ready for analysis for elements of interest using appropriate
elemental analysis techniques (FLAA and GFAA or ICP-MS, ICP-AES).