Fusion

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FUSION
* "Organics" refers to organic containing samples. Both the sodium and potassium
hydroxide/nitrate mixtures have been used for a wide variety of biological materials, soils, coal,
and organic samples.
** Na2CO3 fusions are very popular in the decomposition of minerals, silicates, refractories,

insoluble metal fluorides, etc. For example, brookite TiO2 will not be attacked by acids, and
Al2O3 is very resistant to acid attack.
SODIUM PEROXIDE FUSION
Sodium carbonate, sodium peroxide and sodium hydroxide is a potent mixture of three fluxes.
This very basic, strongly oxidizing mixture renders most refractory minerals soluble. Sodium
peroxide fusion is commonly used to decompose the most refractory minerals.
The fusion procedure described is a general method which allows the majority of samples to be
decomposed in a routine way. A ten to twenty-fold ratio of the NaOH flux to the sample weight
is required. The use of alkali metal hydroxides may liberate variable amounts of water during the
fusion process, causing the fusion melt to foam, froth and spatter in the worst cases. The
procedure therefore requires the formation of the NaOH melt prior to the addition of sample.
Fusion with hydroxides is used to decompose quartz, silicates, sand, clay, natural oxides, some
ores and rocks. The decomposition of silicates depends on the structure of the minerals
concerned. Layered clay minerals may react very rapidly, even at low temperatures (400–
430°C). Sodium hydroxide causes iron compounds to be reduced in the melt if the samples
contain silicates. Iron forms an alloy with nickel in proportion to the iron content of the mineral
sample. The addition of sodium peroxide allows complete oxidation of the sample for these
difficult matrices, especially when sulphides and chromites are in the samples.
Molten Salt Fusions
When dissolution with acids runs into difficulties, the analyst’s next recourse is usually a molten
salt fusion. This category of techniques is quite broad, with diverse fluxes ranging from acidic to
basic and from non oxidizing to strongly oxidizing. Vessel materials and heating modes also
vary widely, although they are often constrained by the nature of the flux.
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FUSION
Figure 7-1 A chart of molten salt flux properties
When we speak of molten salt fusions, “oxidizing” and “non oxidizing” carry their usual
meanings, but the terns “acidic” and “basic” are used in the Lewis sense of electron-pair acceptor
and electron-pair donor, respectively. Molten salt reaction are by their high-temperature nature
water free, but by intuitive analogy to aqueous systems we say that a sodium carbonate fusion is
a “basic fusion” or that a sodium bisulfate fusion is an “acidic fusion.” Figure 7-1 shows how
some common fluxes relate to one another in terms of these properties.
All fusions start with a dry mixture of the sample and the flux compound (or compounds). It is
usually very important that both the test portion and the flux are in a dry, finely divided form and
that they be mixed as intimately as possible before heat is applied. The weight ratio of flux to
sample is often critical; although, except where the flux contributes a very large blank to the
analyte measurement, it is seldom weighed to the same degree of accuracy as the sample.
Fusions are either conducted over a gas burner or in a muffle furnace, most often using a lid to
contain any spattering. The choice of vessel material is related to both the flux and sample
characteristics, as well as the analytical requirements. Frequently it is necessary to swirl the
molten contents with a pair of tongs to ensure a complete reaction. The cooled melt is either
leached with water which is then acidified, or it is leached directly with dilute acid.
Sodium Carbonate
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FUSION
The ignited stannic acid can also be dissolved by Freiberg-fusion (Na 2CO3 + S), while stannic
acid, which has not been ignited, obtained on evaporation with nitric acid, can be fused with
sodium sulphide (Na2S . 9H2O + S). The Freiberg-fusion can also be used directly for the
dissolution of tin alloys and natural sulpho salts. These procedures are not suitable for the fusion
of cassiterite, (SnO2). The most convenient method is to reduce cassiterite to the metal with
hydrogen at the temperature corresponding to a red glow, and to dissolve the metal by one of the
recommended methods. Cassiterite can also be smelted with sodium hydroxide. It is then
converted to sodium stannate and can easily be decomposed by acids.

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** Na2CO3 fusions are very popular in the decomposition of minerals, silicates, refractories,

SODIUM PEROXIDE FUSION

Molten Salt Fusions

Figure 7-1 A chart of molten salt flux properties

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