LESSON: Determination of Ash content

I. Experiment Objectives:
- Understand and determine ash content using the gravimetric method.
- Apply the gravimetric drying method to determine the ash content in black
bean powder.
II. Principle:
- Ash content: Ash is the remaining component of food after burning all
organic substances. Ash is the only mineral salt found in food (hence the
term ash total)
- The gravimetric method for ash determination is based on the mass of the
remaining white ash after the sample is heated at a high temperature for a
long time to ensure that all organic matter has been completely
decomposed.
III. Apparatus and chemicals
1) Tools and equipment
- Analytical balance
- Dryer
- Crucibles
- Desiccator
- Temperature adjustable furnace
2) Samples and chemicals
- Black bean powder
- HNO3/H2O2
IV. Procedure:
Ash content:
- Wash crucibles and experimental equipment with distilled water.
- Place the crucible in a furnace. Heat it at 105 oC. Maintain this temperature
until the weight of the crucible stabilizes.
- Remove the crucible from the furnace and let it cool in a desiccator.
- Weigh the cooled crucible on an analytical balance. Record its weight.
- Add approximately 5g of the ground black bean sample to the crucible.
Weigh the crucible and sample. Record their weight.
 - Place the crucible and sample in the muffle furnace. Gradually heat them at
500 - 600 °C. Maintain this temperature until the ash turns white (about 6-7
hours).
- Wait for the muffle furnace temperature to drop to around 250 °C.
- Remove the crucible from the muffle furnace and place it in a desiccator to
cool to room temperature.
- Weigh the crucible and ash. Record their weight.
V. Result and comment:
1) Result
- Formula: X = (G2 – G) x 100 / (G1-G)
G: Crucible weight (g)
G1: Weight of crucible and sample before burning (g)
G2: Weight of crucible and sample after burning (g)
Before burning (G1) After burning (G2) % Ash
Sample number crucible(G) Sample Sum
1 44,2347 3,0278 47,2625 44,3745 4,61%
2 43,4992 3,0422 46,5414 43,6355 4,48%
3 37,7285 3,0161 40,7446 37,8693 4,66%

4 ,61+ 4 , 48+ 4 , 66
Mean = 3
= 4,58

SD =
√
(4 , 61−4 ,58)2 +(4 , 48−4 , 58)2 +(4 ,66−4 , 58)2
2
= 0,0930

0,0930
CV = 4 , 58 *100 = 2,0305%
4 ,58−4 ,6
%Erel = 4 ,6
∗100 = -0,4347%
 2) Comment
The experiment results deviate from the true value due to the following reasons:
- Positive error:
+ The sampling procedure involving removal from the desiccator for
weighing causes the sample to absorb moisture in reverse.
- Negative error
+ Sample loss due to handling
Error reducing method:
- Practice improving accuracy in handling.