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