Fundamentals of Analytical Chemistry: 8th ed.

Chapter 36

Chapter 36

36-1 Dry ashing is carried out by igniting the sample in air or sometimes in oxygen. Wet

ashing is done by heating the sample in an aqueous medium containing such oxidizing

agents as H2SO4, HClO4, HNO3, H2O2, or some combination of these.

36-2 A flux is a solid salt, usually containing an alkali metal cation, that liquefies upon heating

to a red heat. It is used to decompose refractory materials and render them soluble in

aqueous solution.

36-3 B2O3 or CaCO3/NH4Cl

36-4 Refractory metal oxides are generally decomposed by potassium pyrosulfate, K2S2O7.

36-5 When hot concentrated HClO4 comes in contact with organic materials or other

oxidizable substances, explosions are highly probable.

36-6 (a) Samples for halogen determination may be decomposed in a Schöniger combustion

flask, combusted in a tube furnace in a stream of oxygen, or fused in a peroxide bomb.

(b) Samples for the determination of sulfur are treated in same way as described in part

(a).

(c) Samples for nitrogen determination are decomposed in hot concentrated H2SO4 in a

Kjeldahl flask or oxidized by CuO in a tube furnace in the Dumas method.

(d) Samples for heavy metal determination may be dry ashed by ignition in a hot flame or

wet ashed with an oxidizing solution such as nitric acid, sulfuric acid, perchloric acid, or

some combination thereof.

Fundamentals of Analytical Chemistry: 8th ed. Chapter 36

36-7 The advantages of microwave decomposition include speed, higher temperatures

developed, elimination of loss of volatile components, and opportunity for automation of

the process.

36-8 The major limitations of closed-vessel, high pressure microwave digestion include the

risk of explosion when alloys and metals are digested, an inability to reach sufficiently

high temperatures to decompose organic materials, and limited sample sizes of less than 1

g.