EXPERIMENT 1

LOSS ON DRYING

Many pharmaceutical ingredients or raw materials are hydrates and contain water. Water

content determination is important in compliance with the quality control raw material evaluation or

screening. There are different methods in determining water content. These include: 1) Titrimetric

method using Karl Fischer reagent, in which the sulfur dioxide and iodine are dissolved in pyridine and

methanol, 2) Azeotropic-toluene distillation method, and 3) Gavimetric method such as loss om drying.

Loss on drying is used to determine the amount of water that will vaporize under given or

specified conditions such as temperature, duration time, or in vacuum using specified apparatus such as

pharmaceutical oven.

FIGURE 1. Pharmaceutical Oven

OBJECTIVE: To be able to perform and determine the water content of the substances using the

gravimetric method-loss on drying

APPARATUS/GLASSWARE: Weighing bottle, analytical balance, spatula, oven or as specified, desiccator

MATERIAL/SAMPLE: (To be assigned by the instructor)

PROCEDURE

1. Mix and accurately weigh the substance to be tested, and, unless otherwise directed in the

individual monograph, conduct the determination on 1 to 2g of sample. If the test specimen is in

the form of large crystals, reduce the particle size to about 2mm by quickly crushing.

2. Tare a weighing bottle that has been washed thoroughly and dried for 30mins same with the

conditions to be used with the material, but has been cooled to room temperature in the

desiccator.

3. Put the material in the weighing bottle and accurately weigh the weighing bottle with the

contents.

4. Uniformly distribute the material using a spatula, and cover.

5. Put the weighing bottle in the oven which is set at and meets the required conditions, removing

the cover, leaving the cover in the oven.

6. Dry the material at the temperature and time or/ and with other required conditions.

7. Then open the oven, cover immediately the weighing bottle and allow to cool to room

temperature in the desiccator.

8. Weigh the weighing bottle with content.

9. If specimen under test is capsule, used a portion of the mixed contents of not less than 4

capsules.

10. If specimen under test is tablet, use powder form not less than 4 tablets, ground to a fine

powder.

11. Where drying in vacuum over a desiccant is directed, a vacuum desiccator is to be used. Ensure

the desiccant is kept fully effective by frequent replacing.

12. After gaining the room temperature, weigh and compute the percentage loss in drying.
WORKSHEET

Name :_________________________________ Date :________

Group No. :______________________________ Score :_______

EXPERIMENT 1

LOSS ON DRYING

DATA AND RESULT:

Weight of the weighing bottle (A) _________________________________________

Weight of the weighing bottle and contents (before drying) (B) :_________________________

Weight of the weighing bottle and contents (after drying) (C) :___________________________

COMPUTATION:

((B−C)−A) x 100
%Loss on drying =
(B−A)

CONCLUSION:
QUESTIONS/S:

!. What is/are the importance of determining the water content of pharmaceutical raw materials/
products?

2. Draw the apparatus used in the Toluene Distillation Method and label its parts