Practical 7: Determination of Ash
Practical 7: Determination of Ash
Practical 7: Determination of Ash
INTRODUCTION
In this study, there are two methods were used to determine the ash content, which is
the dry ashing method and Acid insoluble ash method. The dry ashing method is a method
were usually performed by placing the sample in an open inert vessel and destroying the
combustible portion of the sample by thermal decomposition using a muffle furnace. (venture,
2019) In this method ashing temperature was used is 5500C. While for acid-insoluble ash
method, the content of acid-insoluble ash is the proportion of a sample that is not hydrolyzed
by 72% sulphuric acid and is not subsequently volatilized upon the incineration of this acid-
insoluble residue.
OBJECTIVE
MATERIALS
Porcelain dish, analytical balance, Bunsen burner, oven, muffle furnace and tongs
Hydrochloric acid, porcelain dish, watch glass, ashless filter paper, analytical balance and
Bunsen burner
METHODS
Each dried porcelain dish was labelled clearly by using carbon pencil on the bottom of
each porcelain dish. Five grams of homogenized food sample was weighed and placed into
the porcelain dish. The dried sample then was burned gently by using Bunsen burner until
smoke is no longer evolved when heated strongly. The dish was placed in a muffle furnace
and heated at 5500C for 3 hours until whitish ash is obtained. The dish then removed, cooled
in a desiccator and was weighed after it attaining the room temperature.
The ash obtained from dry ashing was boiled with 25ml dilute hydrochloric acid for 5
minutes. The insoluble matter was collected by filtering through an ashless filter paper and the
insoluble matter was washed thoroughly with hot water until it is acid-free. The filter paper then
ignited in the original dish. The dish was cooled and weighed.
RESULTS
In this ash analysis determination, there is two methods that been used which are dry
ashing method and acid insoluble ash method. In the dry ashing method, it is a common
procedure to determine the total mineral content of foods. While for the acid insoluble ash
method is used to determine a part of the total mineral of the food. In this method, the porcelain
dish was used. It is resistant to acids and halogens but not alkali at high temperature and it
also can withstand 12000C. For the dry ashing method, the principle is to remove water and
organic matter by heating the sample with the presence of the oxidizing agent, which provides
a measure of the total amount of minerals within a food. During the heating process, water
and other volatiles material are vaporized and organic substances are burned in the presence
of oxygen in the air to carbon dioxide, water and Nitrogen gas (Lenz, 2017). Most of the
minerals are converted to oxides, sulfate, phosphates, chloride or silicates. Although, most
minerals have low volatility at these high temperatures, some are volatile and may be partially
lost. Based on table 1.1 the ash content between those two samples is significantly different.
This clearly portrayed, that Lipton tea has a low mineral compared to Boh. In this
method, the precaution step needs to be done especially during the ignition of the sample
using the Bunsen burner. The possibility of the ash to fly away from the crucible is high so it
is recommended to partially closed the crucible and ensure the environment is not too windy.
If the ash is flying away it will affect the results and underestimation of minerals will occur.
Next, for the acid insoluble ash method, dilute hydrochloric acid was used to digest organic
matter. The acid needs to be boiled for 5minutes after the addition of ash is to ensure that the
organic matter is completely digested, leaving only mineral oxides in solution. In this analysis,
ashless filter paper need to be used for filtration, if normal filter paper been used which also
causes the production of ash during ignition will cause overestimation to occurs. From this
analysis, the insoluble ash basically the inorganic matter of ash which are silica, oxalates, and
carbonates. From this analysis basically, we can calculate the acid-soluble ash by using
formula. By knowing the acid insoluble ash, adulteration of food samples can be detected. By
this method as referring to table 1.2, it also shows that Boh tea is high in mineral compared to
Lipton tea.
QUESTIONS
CONCLUSION
In conclusion, the % ash content of Lipton tea and Boh tea is 0.3% and 5.7% while for the %
acid-soluble ash for Lipton is 0.08% and for Boh is 5.4%.
References
L.Perring. (2019). Determination of ash content of milk-based powders by Energy Dispersive.
Microchemical journal, 162-167.
venture, W. I. (2019, June 8). Ashing procedures. Retrieved from Inorganic ventures:
https://www.inorganicventures.com/trace-analysis-guide/ashing-procedures
APPENDIX
g ash per 100g the total sample = Weight of ash/ weight of sample X 100
= 0.3%
0.011
= x 100
5.0101
= 0.22%
0.011
= x 100
0.0148
= 74.32%
= 0.3 – 0.22
= 0.08%
School of Industrial
Technology
Faculty of Applied
Sciences
__________________________________________________
______
FST 556
Laboratory Title: Determination of ash
Date of experiment: 4.11.2019
Laboratory Group: AS2464C
MARK: