PRACTICAL 2

DETERMINATION OF MOISTURE

Drying Method using Air Oven

Apparatus
Aluminium dish with covers, spatula, analytical balance, air oven, desiccators and tongs (or gloves).

Procedure
1. Dry an aluminium dish with cover for 3 hours in an oven at 105oC. Transfer the dish into the desiccator
to let it cool and weigh after it has attained room temperature.
2. Label dried aluminium dish with covers and weigh accurately.
3. Weigh approximately 5 g of homogenised sample into the aluminium dish.
4. Place the aluminium dish with sample uncovered in 100-105oC or 60oC oven overnight.
5. Replace cover of aluminium dish before remove it from the oven. Cool in dessicator and weigh soon
after attaining room temperature. Record the weight obtained.
6. Repeat the drying process (step 4 and 5) until constant weight is achieved.
7. Calculate percentage of moisture as described below.

Calculations
Calculate percentage moisture (wt/wt):
(Wt of wet sample + pan) - (Wt of dried sample + pan) x 100
(Wt of wet sample + pan) - (Wt of pan)

Drying Method using Vacuum Oven

Materials
Absolute alcohol, aluminium dish with covers, spatula, glass rod, sand, measuring cylinder, Pasteur
pipette, analytical balance, vacuum oven, desiccators and tongs (or gloves).

Methods
1. Obtain clean aluminium dish with lids and label clearly.
2. Weigh about 10 g sand into dishes.
3. Place dish (containing sand) along with lids and glass rods into an oven at 105oC for 30 min. Then cool
in dessicator for 30 min. Record the weight of each dish containing sand, lid and glass rod accurately.
4. Weigh approximately 5 g of homogenised sample into the aluminium dish.
5. Add about 5 ml of absolute alcohol and mix the content thoroughly with the glass rod
6. Place the dishes on a heating tray and stir occasionally until all of the absolute alcohol has evaporated.
7. Place the dish uncovered in a vacuum oven at 70oC and <100 mmHg for 24 hours. Leave the glass rod
in the dish.
8. Replace cover of aluminium dish before remove it from the oven. Cool in dessicator and weigh soon
after attaining room temperature. Record the weight obtained.
9. Repeat the drying process (step 5 and 6) until constant weight is achieved.
10. Calculate percentage of moisture as described in previous method.

Halogen Drying Method using Moisture Analyser

Materials
MB45 Halogen Moisture Analyser (Ohaus Corporation)(Figure 1), sample pan and spatula

Figure 1: Diagram of MB45 Halogen Moisture Analyser

(Adopted from MB45 Halogen Moisture Analyser Instruction Manual, Ohaus Corporation)

Methods
1. Press the ON/OFF button to switch on the Moisture Analyser. Make sure the air bubble in the LEVEL
INDICATOR is centred.
2. Press the TEST MENU button to edit the drying parameter based on the food sample.
Example of drying parameter for moisture determination of wheat flour
Drying Temperature : 150oC
Profile : Standard
Switch Off Time : 5 minutes
Display Set : % moist
Target weight : 5g
Program : Timed switch-off (5 min)
3. Open the cover of the instrument and clear the pan.
4. Place an empty sample pan in the pan handler and place the pan handler in the sample chamber.
Ensure that the tongue of the pan handler fits exactly in the slot of the draft shield element and the
sample pan lie flat in the pan handler.
5. Close the cover and press the TARE button to sets reading to zero.
6. Place about 5 g food sample, evenly distributed in the sample pan. Close the cover.
7. Press the START/STOP button to start the drying process.
8. At the end of the drying process, read the result display for % moisture and record the reading.
9. Open the cover and carefully lift the pan handler from the chamber to remove the sample.

Distillation Method using Dean & Stark Apparatus

Materials
Toluene, analytical balance, distillation apparatus, heating mantle, and graduated cylinder.

Methods
1. Weigh approximately 40 g sample (or enough to yield 2 to 5 ml H2O) (Note: You will need to know the
approximate water content so that the total volume of water extracted does not exceed 7 cm).
2. Transfer the sample quantitatively to the round bottom flask.
3. Add sufficient toluene to cover the sample completely (two third of flask or not less than 75 mL).
4. Attach the flask containing sample and solvent to the condenser by the side arm.
5. Fill the trap with toluene by pouring it through the condenser until it just fills the trap and begins to
flow into the flask.
6. Insert a loose non-absorbing cotton plug into the top of the condenser to prevent consideration of
atmospheric moisture in the condenser.
7. Turn on the water supply to the condenser; switch on the heating mantle to boil the sample. Reflux
about 2 drops per second until most of the water is collected in the trap then increase the reflux rate
to about 4 drops per second.
8. Continue refluxing until two consecutive readings of 15 minutes apart showed no changes.
9. Turn off the heating mantle and allow the apparatus to cool down.
10. Record the volume of water collected in the trap and calculates the percentage of moisture content.

Calculation
% moisture = Volume of water (ml) x 100
Weight of sample (g)

Questions
1. Why do you allow the sample to cool before weighing?
2. Comment the suitability of the method with the supplied samples.