Determination of Ash
Determination of Ash
Determination of Ash
B.K.K.K.Jinadasa
(GS/M.Sc./FOOD/3608/08)
Determination of Ash 2
Introduction
Ash is the inorganic residue remaining after the water and organic matter have been removed by
heating in the presence of oxidizing agents, which provides a measure of the total amount of
minerals within a food. Analytical techniques for providing information about the total mineral
content are based on the fact that the minerals (the “analyte”) can be distinguished from all the
other components (the “matrix”) within a food in some measurable way. The most widely used
methods are based on the fact that minerals are not destroyed by heating, and that they have a
low volatility compared to other food components. Ash contents of fresh foods rarely exceed 5%,
although some processed foods can have ash contents as high as 12%, e.g., dried beef.
Dry ashing
Wet ashing
– Use of a special device for ashing that uses a vacuum and an electromagnetic
field.
– The oxygen from the air oxidizes sample heated in the electromagnetic field.
– Since the temperature is lower than a muffle furnace, volatilization is much lower.
Refers to ash that is insoluble in acids. This is usually silicates primarily from soil, and generally
not tested for in foods.
Sample preparation is extremely important because of the small (2-3g) sample sizes used
(error rates higher).
It is important to use very pure water if further analysis is expected (specific elemental analysis).
High lipid samples should be pretreated (usually by drying) due to spattering or foaming.
QUARTZ crucibles are resistant to acids and halogens at high temperatures but not alkali.
Porcelain crucibles are heat stable but readily crack, however, since they are cheap they are
commonly used.
Steel crucibles are resistant and stable but are a possible source of contamination of iron,
chromium, and possibly other metals.
Materials
Muffle furnace
Weighing balance
Desiccator
Tongs
Glows (thermal)
Procedure
5g of sample (black tea) was weighed into a clean dry pre weighed silica dish.
Then the sample was ignited slowly over a Bunsen flame in a fume cupboard until no more
fumes are evolved.
Then the dish was transferred to muffle furnace and incinerated until it was free of black carbon
particles and turn into white in colour. (About three hours)
Dish was removed carefully and cooled in a desiccator. Weight was taken after cooling. Process
of ashing, cooling and weighing was repeated till no further loss in weight was indicated.
This process was done to three samples of black tea (5g each)
To get the dry weight of the sample another sample (2 g each) were weighed into pre weighed
stainless steel dish and kept in oven at 105°C for three hours. Then the samples were cooled and
weighed. Process of drying was repeated until a constant weight was obtained.
Determination of Ash 6
This is the HCl acid insoluble fraction of ash expressed as a percentage of the total ash.
Materials
Steam bath
Litmus paper
Desiccator
Muffle furnace
Procedure
Ash content which was obtained from the above practical was taken in separately and 25mL of
10% HCL was added to it separately. Then it was heated 5 min on a steam bath and heated for 10
minutes.
Sample was filtered through an ash less filter paper and washed with hot water and cold water
until the washings are free from acid.
The filter paper containing the ash was carefully folded and placed in the porcelain dish and
ignited in the muffle furnace, cooled and weighed until a constant weight is obtained.
Weight of dish + Acid Weight of dish (g) Weight of Ash (g) % of Acid
Insoluble Ash (g)------------- Insoluble Ash
--------(1) ----------(2) ---------------(2-1)
40.7215 40.6857 0.0358 0.7548
46.3550 46.3192 0.0358 0.7661
39.0425 39.0021 0.0404 0.7979
03
= 0.7729 g
Discussion
In the determination of Acid Insoluble Ash, care must be taken to prevent splitting of the content
when boiling the residues with solvent and during filtering.
Platinum dishes are used because they are stable at high temperature and can be cleaned easily
with dilute HCl acid.
Ashing over an open flame requires constant attention. So the initial stage of ashing must be
done by open flame.
A prolonged ashing fails to give carbon free ash the residue should be moistened, dried and
reheated until a white gray ash remains.
Dry ashing is the most satisfactory method if no loss occurs at temperatures up to about 500Co.
Determination of Ash 9
References:
Fennema, Owen. R., 1996.Food chemistry, 3rd Ed, Marcel Dekker, Inc. New York.
http://www.css.cornell.edu/compost/calc/moisture_content.html