Crude Ash Determination

Date: 23 DEEMBER 2020

1. Theory and Background:
The objective of this experiment was to study the percentage amount of ASH present in
the food sample crushed biscuits after undergoing ignition using muffle furnace. ASH is
the inorganic residue remaining after the water and organic matter have been removed by
heating in the presence of oxidizing agents. It provides a measure of the total amount of
minerals found within a food sample.
There are two major types of ashing which are dry ashing and wet ashing. In this
experiment, dry ashing technique was performed. Dry Ashing is a procedure usually
performed by placing the sample in an open inert vessel and destroying the combustible
(organic) portion of the sample by thermal decomposition using a muffle furnace to
obtain the inorganic material. Typical ashing temperatures are 500 to 600 °C. On the
other hand, Wet Ashing is a procedure for oxidizing organic substances by using
oxidizing agents and acids or their combinations to achieve specific elemental analysis.
Determination of the ash and mineral content of foods is important for several reasons:
 Nutritional labeling: The concentration and type of minerals present must often
be provided on the label of a food.
 Quality.  The quality of many foods depends on the concentration and type of
minerals they contain, including their taste, appearance, texture and stability.
 Microbiological stability. High mineral contents are sometimes used to retard the
growth of certain microorganisms.
 Nutrition:   Some minerals are essential to a healthy diet (e.g., calcium,
phosphorous, potassium and sodium) whereas others can be toxic (e.g., lead,
mercury, cadmium and aluminum)

 Processing. It is often important to know the mineral content of foods during

processing because this affects the physicochemical properties of foods.
Finally, the percentage of ASH can be calculated by the following formula

 Weight (g) crucible with ash after ignition - weight (g) of empty crucible X 100
Weight (g) original food sample

2. Experimental Procedure:
Apparatus:
 Muffle furnace
 Porcelain crucibles
 Analytical balance
 Desiccator with desiccant
Procedure
 1. Accurately weigh a previously ignited porcelain ashing crucible
2. Accurately weigh 2 g of well-mixed food sample (biscuit) into the crucible
3. Ignite crucible and contents in a muffle furnace set at 850 °C for 30 minutes until light
grey ash results
4. Transfer crucible to a desiccator to cool to room temperature
5. Weight the crucible and its contents (ash)
Weight of empty crucible (g)= 22.44g
Weight of original food sample (g)=2g
Weight of crucible + ash (g)=23.01g
% crude ash = (23.01-22.44) *100/2 = 28.5%

3. Questions and Discussions:

1) What does ash represent in the sample?
Ash refers to the inorganic residue remaining after either ignition or complete
oxidation of organic matter in foodstuff.
2) What do we mean by “ashing a sample”?
Ashing a sample means removing the organic part from it so that the inorganic
one remains.
3) Can you think of another method to ash the sample besides dry ashing? If yes,
then explain when should we use it to ash samples?
Besides dry ashing, we have the wet ashing which is a procedure for oxidizing
organic substances by using acids and oxidizing agents or their combinations. Wet
ashing is often preferable to dry ashing as a preparation for specific elemental
analysis when we want to decrease the volatilation of some minerals of the
sample so we use wet ashing instead of dry ashing, and because the oxidation
time is short.
4) What would happen if the ashing temperature is increased?
First the ash yield decreases as the temperature increases, and second some
chemical compositions fates at a high ashing temperature.
4. References:
Li J., Zhu M., Zhang D. (2016) Effect of Ashing Temperature on the Physicochemical
Properties of Zhundong Lignite Ashes Prepared in a Muffle Furnace. In: Yue G., Li S
(eds) Clean Coal Technology and Sustainable Development. Springer, Singapore.