Experiment 2 ASH DETERMINATION

GROUP MEMBERS:
PEDROSO
MALAPIT
SANTOS
URBINA
MUNDAS
ENRIQUEZ
Experiment No. 2
ASH DETERMINATION
Objectives:
At the end of this activity, students will be able to;
1. Compute the total ash from the weight of the plant sample taken
2. Determine the percentage or acid-insoluble ash from the weight of the plant
sample taken.
3. To know the importance of ash determination in the pharmaceutical field.
Introduction:
.
Ash refers to the inorganic residue remaining after either ignition or complete
oxidation of organic matter in a food sample. The ash level of a product is determined
via proximate analysis for nutritional evaluation, and it is a critical quality attribute for
specific food items. Additionally, ashing is the initial step in preparing a sample for
elemental analysis.
The burning off of organic materials, leaving inorganic minerals, is the analysis of
ash content in foods. This aids in determining the amount and kind of minerals in food,
which is significant because mineral content can affect food physiochemical qualities as
well as microbial development.
Moreover, the ash value is useful in determining authenticity and purity of the
drug and also these values are important quantitative standards.
Materials: dried plant material

Ashless filter paper
Dilute HCL
Ethyl alcohol
Procedure:
A.DETERMINATION OF THE TOTAL ASH CONTENT
1. Accurately weigh a quantity of the ground drug representing from 2 to 4 g of the

dried plant material in tared plain crucible
2. Incinerate at a low temperature, for it to become very dull red and until it is free of
carbon.
3. Cool and determine the weight of the ash.
4. If a carbon-free ash cannot be obtained in this manner, exhaust the charred

mass with hot water, collect the insoluble residuer on an ashless filter paper
incinerate and filter until carbon-free ash is obtained.
5. Add the filtrate.
6. Evaporate it to dryness.
7. Heat the whole to a dull dryness.
8. If, again, a carbon-free ash cannot be obtained in this manner, cool the crucible.
9. Add 15mL of alcohol to break up the ash with a glass rod
10. Burn off the alcohol and again heat the whole to dull redness.
11. Cool and weigh the ash
12. Compute the perfect of the total ash from the weight of the plant sample taken.
EXAMPLE: https://youtu.be/n2Qwb8Pw8YE
B. DETERMINATION OF ACID-INSOLUBLE ASH CONTENT
1. Boil the ash obtained in Procedure A with 25mL of dilute HCL for 5 minutes.
2. Collect the insoluble matter on an ashless filter paper
3. Wash with hot water
4. Ignite, cool and weigh
5. Determine the percentage or acid-insoluble ash from the weight of the plant
sample taken.
EXAMPLE: https://youtu.be/JecqdeVUTpE
DATA:
1. Weight of the plain crucible = 34.5 g
2. Weight of plain crucible + plant material = 34.5 g + 4 g = 38.5 g
3. Weight of plant sample alone =4g
4. Weight of plain crucible + ash = 34.5 + 0.2 = 34.7 g
5. Weight of plain crucible - acid insoluble ash = 34.5 – 0.18 g = 34.3 g
6. Weight of ash alone = 0.2 g
7. Weight of acid-insoluble ash alone = 0.18 g
8. % total ash = 5%
9. % Acid-insoluble ash = 4.5 %

Formulas:8
% total ash = weight of ash x 100

Wt. of the plant sample
% Acid-Insoluble Ash = wt. of acid-insoluble ash x 100

Computation:
% total ash = weight of ash x 100

0.2 𝑔 𝑥 100
=
4𝑔
% total ash = 5%
% Acid-Insoluble Ash = wt. of acid-insoluble ash x 100

0.18 𝑔 𝑥 100
=
4𝑔
% Acid-Insoluble Ash = 4.5%

Conclusion:
We had conducted a theoretical experiment using guava leaves as our

plant material in determining total ash content and acid-insoluble content. In this
experiment we used 4g of guava leaves to incinerate at low temperature until free of
carbon then cool and weigh to collect the insoluble residue and obtain the carbon-free
ash. After the whole process we yield 5% of total ash. For the second procedure in
getting the acid-insoluble ash we boiled the obtained ash from the procedure A with
diluted HCL for 5 minutes and we collected the insoluble matter on an ashless filter
paper and wash it with hot water to ignite, cool, and weigh to determine the acid-
insoluble ash which we yield 4.5%.
According to Mallillin (2002) the standard total ash content of the Psidium
guajava Linneranges from 10%-12% and the Acid-insoluble ash content ranges from
0.1%-0.5%.
This concludes that there could be human error for our data results does not conform to
the standard total ash content and acid-insoluble ash content.
Questions:
1. What is the importance of determining the ash content of a drug?
Ash values are helpful in determining the quality and purity of crude drugs,
especially in powder form. The objective of ashing vegetable drugs is to remove
all traces of organic matter, which may otherwise interfere in an analytical
determination. On incineration, crude drugs normally leave an ash usually
consisting of carbonates, phosphates and silicates of sodium, potassium, calcium
and magnesium.
2. Name the possible inorganic plant constituents of the total ash obtained from the
sample drug used?
According to Okunrobo, Imafidon, and Alabi (2011) the possible inorganic

plant constituents of guava leaves are calcium, magnesium, potassium, sodium, and
iron.
3. What is the purpose of heating the crucible to dull redness until constant weight is
obtained?
The purpose of heating the crucible is to remove moisture and ensure that the
crucible is completely dry as any water present may affect the reading. Besides, the
high heat that will be required to bring them to a constant weight will erase such
markings and, more importantly, will have an uncertain effect on their weight. The
crucible lids do not need to be brought to a constant weight, but they should be
clean.
4. What is the possible content of the ash present?
Ash consists of extraneous solids, residues of organometallic compounds in

solution, and salts dissolved in water present in the fuel. These salts may be
compounds of sodium, vanadium, aluminium, nickel, calcium, magnesium, silicon,
iron, etc.
5. What is the possible composition of the acid-insoluble ash?
Acid-insoluble ash consists primarily of silica and silicates. When present in the
finished paper or paperboard, the material can have an abrasive effect on punches,
knives, slitters and dies which come into contact with paper during finishing operations.
REFERENCES;
Heating a Crucible to Constant Weight. (2019, June 6). California State University
Dominguez Hills. https://chem.libretexts.org/@go/page/77629
Your Article Library (April 22, 2015). Determination of Ash Values.

https://www.yourarticlelibrary.com/medicine/ayurvedic/determination-of-ash-
values/49966
Sarkar, D. K. (2015). Thermal Power Plant: Fuels and Combustion.

https://www.sciencedirect.com/topics/engineering/ash-
content#:~:text=Ash%20consists%20of%20extraneous%20solids,%2C%20silicon%2C
%20iron%2C%20etc. Ash Content - an overview | ScienceDirect Topics
Dr. D. Julian McClements. (2003). Analysis of Ash and Minerals.

https://people.umass.edu/~mcclemen/581Ash&Minerals.html
ISO (Jan 15,2021) ISO 776:2011 https://www.iso.org/obp/ui/#!iso:std:52672:en
Okunrobo, L., Imafidon, K., & Alabi, A. (2011). Phytochemical, Proximate and Metal
Content Analysis of the Leaves of Psidium guajava Linn (Myrtaceae). International
Journal of Health Research, 3(4). Retrieved from
https://www.researchgate.net/publication/272338071_Phytochemical_Proximate_and_
Metal_Content_Analysis_of_the_Leaves_of_Psidium_guajava_Linn_Myrtaceae
Mallillin, E. (2002). Standardization of guava leaves Psidium guajava Linne (Family

Myrtaceae). Retrived from http://scinet.dost.gov.ph

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GROUP MEMBERS:

3. To know the importance of ash determination in the pharmaceutical field.

Materials: dried plant material

A.DETERMINATION OF THE TOTAL ASH CONTENT

1. Accurately weigh a quantity of the ground drug representing from 2 to 4 g of the

3. Cool and determine the weight of the ash.

4. If a carbon-free ash cannot be obtained in this manner, exhaust the charred

5. Add the filtrate.

7. Heat the whole to a dull dryness.

9. Add 15mL of alcohol to break up the ash with a glass rod

11. Cool and weigh the ash

2. Collect the insoluble matter on an ashless filter paper

3. Wash with hot water

4. Ignite, cool and weigh

1. Weight of the plain crucible = 34.5 g

2. Weight of plain crucible + plant material = 34.5 g + 4 g = 38.5 g

3. Weight of plant sample alone =4g

4. Weight of plain crucible + ash = 34.5 + 0.2 = 34.7 g

5. Weight of plain crucible - acid insoluble ash = 34.5 – 0.18 g = 34.3 g

6. Weight of ash alone = 0.2 g

7. Weight of acid-insoluble ash alone = 0.18 g

9. % Acid-insoluble ash = 4.5 %

% total ash = weight of ash x 100

% Acid-Insoluble Ash = wt. of acid-insoluble ash x 100

% total ash = weight of ash x 100

% Acid-Insoluble Ash = wt. of acid-insoluble ash x 100

% Acid-Insoluble Ash = 4.5%

We had conducted a theoretical experiment using guava leaves as our

1. What is the importance of determining the ash content of a drug?

According to Okunrobo, Imafidon, and Alabi (2011) the possible inorganic

4. What is the possible content of the ash present?

Ash consists of extraneous solids, residues of organometallic compounds in

5. What is the possible composition of the acid-insoluble ash?

Your Article Library (April 22, 2015). Determination of Ash Values.

Sarkar, D. K. (2015). Thermal Power Plant: Fuels and Combustion.

Dr. D. Julian McClements. (2003). Analysis of Ash and Minerals.

ISO (Jan 15,2021) ISO 776:2011 https://www.iso.org/obp/ui/#!iso:std:52672:en

Mallillin, E. (2002). Standardization of guava leaves Psidium guajava Linne (Family

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