Objective
To determine the ash content of food samples using the gravimetric method
Background
The gravimetric method is one of the most widely used techniques for determining the ash content of
foods. It involves the complete incineration of a food sample to remove all organic matter, leaving
behind only the inorganic residue or ash. The weight of this residue is then measured and expressed as a
percentage of the original sample weight. The process involves the following four steps:
(1) Sample Preparation
1. A representative sample of the food is carefully selected and weighed accurately.
2. Solid samples are ground to a homogenous powder prior to ashing.
3. High-moisture foods are dried to reduce water content and prevent spattering during ashing.
4. High-fat foods are defatted with a solvent to facilitate the release of water and prevent
spattering.
2) Incineration
1. The dried sample is placed in a crucible.
2. The crucible containing the sample is placed in a furnace or muffle furnace and subjected to high
temperatures (typically around 550-600°C) for several hours.
3. During incineration, all organic components of the sample, including carbohydrates, proteins,
fats, and other organic compounds, are completely oxidized or burned off, leaving behind only
the inorganic ash.
(3) Cooling and Weighing
1. After the specified incineration period, the crucible containing the sample residue is removed
from the furnace and allowed to cool in a desiccator to prevent moisture absorption.
2. Once cooled to room temperature, the crucible and residue are weighed again accurately.
(4) Calculation
The ash content is calculated as the weight of the residue (ash) divided by the weight of the original
sample, multiplied by 100 to express the result as a percentage.
Advantages
The gravimetric analysis offers several advantages, including its simplicity, accuracy, and reliability. It
allows for the complete combustion of organic matter, ensuring that all inorganic components are
retained in the ash residue. Additionally, gravimetric analysis is relatively unaffected by interferences
from other substances present in the sample, making it suitable for a wide range of food matrices.
Disadvantages
However, the gravimetric method also has some limitations. It can be time-consuming, requiring
prolonged heating periods to ensure complete combustion. Moreover, certain minerals such as Fe, Se,
Pb, and Hg may be partially volatilized during the incineration process, potentially leading to an
underestimation of the true ash content. Despite these limitations, the gravimetric method remains a
valuable tool for determining ash content in foods, particularly when high accuracy and precision are
required.
Materials
1. Crucibles
2. Desiccator
3. Digital scale
4. Spatula
5. Muffle furnace
6. Food samples
Method
1. Collect a clean crucible and weigh it on a digital scale
2. Tare (zero) the scale
3. Transfer 5 grams of the food sample assigned to you by your instructor. Note: You may not get
exactly 5 grams. Make sure to record the precise amount shown on the scale
4. Repeat the above with another sample to make sure that you replicate the test
5. Place both crucibles in the muffle furnace and close the furnace door
6. Set the temperature of the furnace to 550oC and burn the sample for 12-18 hours
7. Turn off the furnace and allow it to cool to at least 250oC
8. Open the door gently to avoid losing ash that may be fluffy
9. Using tongs, transfer the crucibles to a desiccator
10. Cover the crucibles and close the desiccator
11. Cool to room temperature and then weigh
12. Calculate the ash content and record your findings
