Experiment 02

OBJECT
To perform loss on drying (LOD) by dry-oven method of CuSO4..5H2O (USPS/EP).

REQUIREMENTS
 Oven
 Petri dish
 Desiccator
 Weighing balance
 Tongs
 CuSO4..5H2O

THEORY
LOSS ON DRYING
Loss on drying is unspecific analytical technique removing not only water but all other volatile
impurities like alcohol etc from a sample.

The degree of drying depends upon:

1. Temperature
2. Drying time

LOD includes both bound and free water.

 Methods of LOD
There are three methods:

 Dry oven
 Direct flame
 Vacuum desiccator

 Applications of LOD
1. To analyse the microbial growth in food.
2. To find out flow properties of powders.

DESICCATOR
The desiccator is used to store dried samples ina dry atmosphere. It should not be used to dry an
object, but to maintain an already dried object indefinitely in a dried condition.

Usage
To open—slide lid horizontally across the top to one side until it comes off. Use one hand to hold the
bottom of the desiccator while using the other hand to grasp the knob.
To close—place lid partly on the top and slide across until desiccator is completely closed and then
rotate the lid gently in both directions.

Do not attempt to lift the lid off vertically.

Make sure the lid has enough grease around the ground glass rim- if necessary, spread Vaseline
uniformly on the lid.

DESICCANT
A hygroscopic substance used as a drying agent.

Types of desiccant
 Silica gel: silica gel is a granular, vitreous, porous form of silicon dioxide made synthetically
from sodium silicate. Used a desiccant, it works by a process called adsorption. The water in
the air actually absorbs between the tiny passages as the air passes through them. The water
molecules become trapped so that the air is dried out as it passes through the filter. The
process is reversible. If the silica desiccant is heated to 180°F, it will release the trapped
water. This process is called regenerating the trapped water.
 Activated alumina: used as a desiccant, it works by the process called adsorption.
 Porcelain
 Platinum
 Stainless steel
 Nickel
 Calcium oxide

PROCEDURE
1. Weigh 2 grams of CuSO4..5H2O accurately.
2. Transfer CuSO4..5H2O in petri dish and keep in a dry oven for 1 hour at 160°C.
3. After 1 hour take sample out from oven and then place it in a desiccator for 5-10 minutes.
4. Then weigh the powder again.

CALCULATIONS
𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
Percentage moisture = 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 × 100

5×18
= 250 × 100

=36%
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡−𝑤𝑒𝑖𝑔ℎ𝑡 𝑎𝑓𝑡𝑒𝑟 𝑑𝑟𝑦𝑖𝑛𝑔
Percentage LOD = 𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡
× 100

2−1.52
= 2
× 100

=24%
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑚𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑙𝑜𝑠𝑡
Number of moles= 𝑎𝑐𝑡𝑢𝑎𝑙 𝑤𝑒𝑖𝑔ℎ𝑡×𝑚𝑜𝑙.𝑤𝑡 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑢𝑛𝑑
⁄𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
 0.48
=2×250
⁄18

=3.33 mol

RESULT
The LOD of CuSO4..5H2O has been determined by the help of using dry-oven method. The
percentage moisture was calculated to be 36%. The percentage LOD was calculated to be 24%. The
number of moles was calculated to be 3.33 mol.

DISCUSSION
The result shows that the powder is pure because if there is any contamination or any purity issue then
the result will definitely deviate from the standard values.

QUESTIONS
Q1. What is the difference between LOD/moisture content and water content?

Ans. Water content is determined by the Karl Fischer titration method and it consists of only water.
The result does not contain any volatile matter except water.

Loss on drying (LOD) is determined by heating the sample below its melting point in an oven and it
includes all volatile matter including water content and solvent.

Q2. What if the given drug is not in powder form?

Ans. If the drug is solid and not powdered, then triturate it to reduce its particle size.

Q3. Why does silica change colour?

Ans.Blue silica contains cobalt chloride which imparts its colour changing properties. Whn the
maximum adsorption capacity is reached, its colour changes to pink.

Q4. What is a crucible?

Ans. A crucible is a container made of such a material that can withstand high temperatures. They are
mostly used for metal/glass preparation as well as many laboratory processes.

Q5. How is silica gel reusable?

Ans. Silica gel is reusable as once it turns pink, it is placed on hot air oven to remove the adsorbed
water molecules (moisture). When the silica turns blue again, it is reactivated and is ready to use.

Q6. How are crucible materials chosen?

Ans. Crucible materials are chosen on the basis of the melting point of substance being heated.
Crucibles should have a much higher melting point than the material and be able to withstand
temperatures even when white hot.

Q7. The applications of Loss ondrying?