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Lab 4a - Loss on Ignition

The document outlines the Loss on Ignition (LOI) analysis procedure for determining the organic matter content in soil samples using a muffle furnace. It details the necessary equipment, materials, and step-by-step procedures for conducting the experiment, including precautions to avoid errors. Additionally, it includes post-lab questions and a data sheet for recording results.

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24 views

Lab 4a - Loss on Ignition

The document outlines the Loss on Ignition (LOI) analysis procedure for determining the organic matter content in soil samples using a muffle furnace. It details the necessary equipment, materials, and step-by-step procedures for conducting the experiment, including precautions to avoid errors. Additionally, it includes post-lab questions and a data sheet for recording results.

Uploaded by

winfredometey
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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Lab 4a – Loss on Ignition

INTRODUCTION
Loss on Ignition (LOI) analysis is used to determine the organic matter content (% OM) of a soil
sample. This is a relatively simple procedure compared to others used to determine % OM. It does
not involve the use of any chemicals, only the use of a muffle furnace. LOI calculates % OM by
comparing the weight of a sample before and after the soil has been ignited. Before ignition the
sample contains OM, but after ignition, all that remains is the mineral portion of the soil. The
difference in weight before and after ignition represents the amount of the OM that was present in the
sample.

For LOI you can either place samples in porcelain crucibles or small metal tins. There is no significant
effect on the use of either. However, if you wish to analyze more than 20 samples at a time you may
want to use metal tins for consistency in analysis. When performing this analysis, it is important to
keep track of your samples after you have placed them in either the crucibles or tins. If you are using
the crucibles, they may have a label either carved on the side or written on the bottom. You are free
to re-label them if you wish. No, the type of labeling you use since the temperature gets very high
and burns off the labels. Always make sure you record your samples with their respective tin or
crucible labels.

After objects, such as crucibles, have been heated in an oven they can be cooled in a desiccator to
room temperature. A partial vacuum is created within a desiccator when closed, and care must be
taken when opening it to not let a rush of air knock anything over. Humidity of this atmosphere is
usually the factor that is being considered. Objects, such as crucibles, can pick up moisture from the
air. This causes an increase in water content in an object and can produce errors when weighing. By
using a desiccator, objects are allowed to equilibrate in an environment of low or controlled moisture.
This allows us to avoid errors associated with weighing water along with an object. Figure 1 shows
a crucible containing some material being stored in the desiccator after an experiment.

Figure 1. Image of a crucible stored in a desiccator

EQUIPMENT AND MATERIALS


To conduct this experiment, we will be using the following equipment:
• Weighing balance
• Furnace
• Desiccator
• Tongs
• Oven Safe Gloves

The materials to be used include;


• 40g Soil sample
• Sieve size (2 mm size)
• Spatula
• Porcelain crucibles
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MSE 359/METE 355 Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi
PROCEDURE
1. Heat crucibles for 1 hour at 375°C in a furnace. Cool in the open to about 150°C. Place in a
desiccator, cool for 30 minutes, and weigh.
a. This will be the crucible weight.
2. Have soil samples you wish to perform LOI experiments on prepared in advance.
a. Samples must be 2 mm in size or finer. Mineral soils can be sieved with a 2 mm sieve.
Forest floor samples with large particulate material must be ground to a 2 mm size (see
appendix C for further instructions on grinding)
3. Samples can then be placed in trays to be oven-dried at 105°C for 24 hours.
a. Remember to label trays with sample ID, or record the label on a tray to correspond to sample
ID.
4. Take samples out of the oven after oven-drying and place them in a desiccator.
5. Bring the desiccator to a scale capable of precision to 0.001 g.
6. Weigh 5.000 g ± 0.001 g of each oven-dried sample and place each into a crucible.
a. This will be the pre-ignition weight.
b. Ensure to record the number of each crucible corresponding to each sample
7. Place crucibles back in the desiccator after being weighed.
8. Transport samples to the furnace in the desiccator. Place crucibles in the furnace.
9. Turn the furnace on.
a. The LOI process requires a slow temperature increase of 5°C/min.
10. Allow the furnace to heat to 375°C.
11. After the furnace has reached the desired temperature allow the samples to heat for at least 16
hours (overnight). Heat them long enough to ensure that the samples have been fully heated.

Post-Ignition Work:
12. When sufficient time has passed turn off the furnace, and allow the samples to cool to ~150
°C.
13. Check the temperature of the furnace by turning it back on and reading the display.
a. Remember to turn it off when you’re done or you will start to heat the samples again.
14. When cooled to ~150°C remove samples from the oven and place in a desiccator using tongs.
15. Wait 30 min then remove the samples from the desiccator and weigh the samples for their
post-ignition weight.
16. Remember to subtract the crucible weight from the post-ignition weight.
17. Calculate % OM using the following equation:
𝑝𝑟𝑒 − 𝑖𝑔𝑛𝑖𝑡𝑖𝑜𝑛 𝑤𝑒𝑖𝑔ℎ𝑡 (𝑔) − 𝑝𝑜𝑠𝑡 − 𝑖𝑔𝑛𝑖𝑡𝑖𝑜 𝑤𝑒𝑖𝑔ℎ𝑡 (𝑔)
% 𝑂𝑀 = × 100
𝑝𝑟𝑒 − 𝑖𝑔𝑛𝑖𝑡𝑖𝑜𝑛 𝑤𝑒𝑖𝑔ℎ𝑡 (𝑔)

Precautions
• Be cautious when handling hot equipment and samples to avoid burns or accidents.
• Avoid opening the furnace or disturbing the samples during the heating.
• Allow the crucibles with heated samples to cool down to room temperature in a desiccator
before handling to prevent moisture absorption.

RESULTS AND ANALYSIS


At the end of the experiment, the student is expected to;
1. Compute the weight of the post-ignition soil sample
2. Analyze and discuss the result of the discrepancies in the pre-and post-ignition sample weight
3. Calculate the percent organic matter
4. In a tabular form, summarize your final results.
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MSE 359/METE 355 Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi
POST LAB QUESTIONS
1. What is the purpose of the Loss on Ignition (LOI) test in soil analysis?
2. How does the LOI method help determine the amount of organic matter in a sample?
3. What are the possible sources of error in an LOI experiment, and how can they be minimized?
4. How do temperature and duration of heating affect the LOI results?
5. Can the LOI method be used to differentiate between different types of organic matter in a
sample? If so, how?
6. What are the advantages and limitations of using the LOI method in soil analysis compared
to other techniques?

LOSS ON IGNITION
DATA SHEET
Date Tested:
Tested By:
Experiment Name:
Sample Description:

Sample number 1 2 3
Mass of empty crucible (grams)
Pre - Ignition weight (grams)
Post - Ignition weight (grams)
Organic Matter (OM%)

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MSE 359/METE 355 Materials/Metallurgical Characterization Lab, Materials Engineering Department, KNUST, Kumasi

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