PRACTICAL 7: DETERMINATION OF ASH

INTRODUCTION

Ash content is a key parameter, providing proximate information for nutritional

evaluation, and is widely accepted as an index of refinement of foods. Ash is the inorganic
residue remaining after that water and organic matter has been removed by heating in the
presence of air, which provides a measure of the total amount of minerals within a food. Indeed
minerals are not destroyed by heating, and furthermore, most of them present lower volatility
compared to other food components. According to literature, the ash constituents include
mostly potassium, sodium, calcium, and magnesium, but also smaller quantities of iron,
copper, manganese, and zinc as well as other elements present in lower traces. (L.Perring,
2019).

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

1. To determine % ash content of tea samples

2. To determine % acid-soluble ash of tea samples

MATERIALS

Dry Ashing Method

Porcelain dish, analytical balance, Bunsen burner, oven, muffle furnace and tongs

Acid Insoluble Ash Method

Hydrochloric acid, porcelain dish, watch glass, ashless filter paper, analytical balance and
Bunsen burner
METHODS

Dry Ashing Method

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.

Acid Insoluble Ash Method

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

Table 1.1 Dry Ashing Method

Sample Weight of Weight of Weight of Weight of Weight of % ash

crucible crucible + sample (g) crucible + ash (g) content
(g) sample (g) ash (g)
Lipton 66.6936 71.7263 5.0101 66.7084 0.0148 0.3000
Boh 63.0046 73.4667 5.0333 63.2899 0.2853 5.7000

Table 1.2 Acid Insoluble Ash Method

Sample Weight of Weight of g Acid g Acid % acid

crucible + acid insoluble ash insoluble ash soluble ash
acid insoluble ash / 100 g / 100 g total
insoluble ash (g) sample ash
(g)
Lipton 66.7046 0.0110 0.2200 74.3240 0.0800
Boh 63.0189 0.0143 0.2840 5.0120 5.4000
DISCUSSION

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

1. How do you know when the ash is free from carbon

By looking at the color of ash, if it is blackish it means the carbon is present. But if it is
greyish or whitish it is free from carbon
 2. Why is the sample needed to be heated over a Bunsen burner before heating in a
muffle furnace?
To accelerate the heating process

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.

Lenz, H. (2017). Analysis of Ash and Minerals. UK: MaClement press.

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

=0.0148 g / 5.0101 g X 100

= 0.3%

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑖𝑛𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ

g acid insoluble ash/ 100 g of total sample = x 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

0.011
= x 100
5.0101

= 0.22%

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑖𝑛𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ

g acid insoluble ash/ 100 g of total ash = x 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑎𝑠ℎ

0.011
= x 100
0.0148

= 74.32%

Acid soluble ash% = %Total ash- % Acid insoluble as

= 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

Name : Muhammad Shafiq Bin Mustafa

Student ID : 2018401924
Group : AS2464C

MARK: