Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
(STKM 2311)
GROUP: D1
DATE: 10 / 10 / 2016
Water is the major component of most foods and has various functional properties.
The functional properties of water in foods include acting as a diluents and carrier of
hydrophilic food ingredients, providing a medium for chemical and enzymatic
reactions, and dispersing and solvent action. Water also accounts for food moisture
content. Moisture is the amount of water present in a food. Most water in foods is
called free water. Free water acts as the solvent in foods and retains its physical
properties. It can be removed by drying foods. Adsorbed water is another type that is
held tightly in cell walls or protoplasm. Bound water, sometimes called as water of
hydration, is the third form of water in food. It is chemically bound, and is sometimes
known as “water of crystallization”.
The methods used in this laboratory are oven method, infra-red method and reflux
distillation. Oven method is the method whereby the amount of moisture is
determined by calculating the difference between the weight before and after drying.
It is simple and is used as a standard method for many kinds of foods. In infra-red
method, drying involves the penetration of heat into the food sample enables water to
evaporate fairly quickly. As for reflux distillation, toluene is used as solvent which is
less dense than water and at 110.6C, has a boiling point slightly higher than water. A
vaporous emulsion of water in toluene when it started to boil during distillation and
will rise and condensation occurs. Initially, the emulsion which collects in the
Bidwell-Sterling moisture trap is turbid as the emulsion inverts and become toluene
dispersed in water. As the apparatus cools to room temperature, the turbidity clears
and the volume of water in the trap can be measured.
The principle of ashing is to burn off the organic matter and to determine the
inorganic matter which remains. All kinds of food is applicable in this method by
heating temperature of 525℃ to 600℃. The ash in the food basically is determined by
weighing the dry mineral residue of organic materials. There are three major of ashing
are available: dry ashing for the majority of samples, wet ashing (oxidation) for
samples with high fat content (meat products) as preparation for elemental analysis,
and low temperature plasma ashing for preparation of samples when volatile
elemental analyses are conducted.
In this laboratory, dry ashing is used. Dry ashing refers to the use of a muffle
furnace which functions in maintaining temperatures of 500 to 600C. Water volatiles
are vaporized and organic substances are burned in the presence of oxygen in air. The
ash consists of oxides and salts of anions like phosphates, chlorides and sulphates and
cations like sodium, potassium and magnesium.
2.0 OBJECTIVES
1. To learn and understand the method of determining the moisture content minced
meat using oven method.
2. To learn and understand the method of determining the moisture content in flour
using infra-red method.
3. To learn and understand the method of determining the moisture content in
margarine through reflux distillation.
3.0 APPARATUS AND MATERIAL
The dish (containing the sand and glass rod) and the lid are weighted.
5g sample is weighted into the dish. The meat is spread evenly with the glass rod in
the dish.
The lid is replaced and the dish and its content are weighted (W1).
The dish with its lid is placed slipped to one side and later on dried for 16 hr or
overnight at 105C.
After drying, a pair of tongs is used to transfer the dish and lid to the desiccators to
cool (approx. 45min). The dish, lid and its dried content are reweighted.
The dish is replaced with its lid partially covered in the oven for 1 hr. It is transferred
to the desiccators to cool, and the dish, lid and its content are weighted again. This
step is repeated until a constant weight is obtained (W2)
Method 2: Infra-red method
The disposable aluminum pan liner is pre-dried at 100C overnight and left to cool in
desiccators.
The intra-red meter is balanced at zero level.
10g flour is weighted accurately and it is spread evenly onto the pan liner.
The dish with sample is placed on the infra-red meter dish holder and the heater is
switched on in the moisture meter.
The percentage of moisture loss every minute is noted down as shown on the display
panel until no further changes in moisture content is detected.
The moisture balance is allowed to cool before repeating the experiment.
A graph is plotted showing “Moisture loss (g) against time (min).
10g sample is weighted approximately onto a piece of aluminum foil and well
wrapped.
The sample is placed in distillation flask and is covered completely with solvent.
It is brought to a boil and is distilled slowly at first, then at increased rate.
A long glass rod is used to dislodge water that adhered to the walls of the caliberated
tube so it collects in the bottom of the tube.
After no more water has distilled from the sample, the apparatus is allowed to cool to
ambient temperature before measuring the volume of water in the trap
B. Determination of Ash Content
1) Determination of total ash in tea leaves
Porcelain crucibles with lids are pre-ignited around 450-550C overnight in a
muffle furnace, cooled in a desiccators and weighted after reaching room
temperature.
5g of tea leaves is weighted approximately in a crucible with its lid. It is done in
duplicates.
The sample is heated in the crucible with its lid slipped to one side on an electric
heating mantle in a fume hood till fumes are no longer produced.
The sample is placed in a cooled muffle furnace and the temperature is increased.
The sample is heated in the muffle furnace overnight at 450-550C.
Using safety tongs, the crucible is quickly transferred to dessicator. The crucible is
allowed to cool prior to weighting.
Duplicate determinations are made and the average ash content in the sample is
calculated.
2) Water-soluble and water-insoluble ash
25mL hot distilled water is added to a crucible containing ash.
The crucible is covered and heated slowly on a heating mantle till nearly
boiling.
It is filtered on ashless filter paper and is rinsed with hot distilled water several
times till 60mL of filtrate is obtained.
It is dried in an oven at 100C overnight. Using safety tongs, the crucible is
transferred quickly to a dessicator. The crucible is allowed to cool prior to
weighting.
It is weighted and is calculated as percent H2O-insoluble ash.
The soluble ash content is calculated by subtracting insoluble ash weight from
the total ash
Duplicate determinations are made and the average water-soluble and water-
insoluble ash contents are calculated in the sample.
5.0 RESULTS
Calculations:
𝑊1 − 𝑊2
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒(%) = x 100
𝑊1
where,
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒(%) 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒
5.3391 − 3.5240 5.3690 − 3.4563
= 𝑥 100 = 𝑥 100
5.3391 5.3690
= 34.0% = 35.62%
1.2
0.8
0.6
0.4
0.2
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
Reading 1 Reading 2
Graph Average Moisture loss (g) against time
(min)
1.4
1.2
0.8
0.6
0.4
0.2
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30
Time (min)
Reading
Calculation:
1.20𝑚𝑙
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 (%) = 𝑥 100
10.20𝑔
= 11.76%
Calculations:
𝑻𝒐𝒕𝒂𝒍 𝒂𝒔𝒉 (𝒈) = (𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒄𝒓𝒖𝒄𝒊𝒃𝒍𝒆 + 𝒂𝒔𝒉) − (𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒄𝒓𝒖𝒄𝒊𝒃𝒍𝒆)
𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒂𝒔𝒉
𝑻𝒐𝒕𝒂𝒍 𝒂𝒔𝒉 (%) = 𝐗 𝟏𝟎𝟎
𝒘𝒆𝒊𝒈𝒉𝒕 𝒐𝒇 𝒔𝒂𝒎𝒑𝒍𝒆
Plate W1 W2
Weight of crucible with lid (g) 49.49 46.91
Calculations:
Plate W1 W2
Weight of ash (g) 0.30 0.29
Weight of crucible with lid (g) 49.49 46.91
Weight of crucible with water-
49.57 46.97
insoluble ash (g)
Weight of water-insoluble ash
49.57 – 49.49 = 0.08 49.97 – 46.91 = 0.06
(g)
Weight of water-soluble ash (g) 0.30 – 0.08 = 0.22 0.29 – 0.06 = 0.23
0.08 0.06
Total water-insoluble ash (%) 𝑥 100 = 1.58% 𝑥 100 = 1.19%
5.05 5.04
0.22 0.23
Total of water-soluble ash (%) 𝑥 100 = 4.37% 𝑥 100 = 4.56%
5.05 5.04
𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛
𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛
Based on the results, the moisture content of the flour is 12.99% which is
equivalent to 1.30g. It is acceptable for standardization of moisture content flour
sample reported in wheat quality and carbohydrate research by North Dakota State
University. The moisture content of flour is advised to set it less than 14% due to
instability of flour in room temperature. This is because organisms present in flour
will start growing at high moisture, which will cause spoilage and produce odors.
Infra-red method is the best method in determining the moisture content of flour as
compared to oven method because flour is a dried sample. Oven method is simple
method in identifying only free water in food samples. Although flour is mentioned as
“dried sample”, there are still contain water in sample which are water of hydration or
adsorbed water because only free water is completely evaporated. The experiment
was done duplicated to obtain an average of moisture loss to increase the accuracy of
the data in result.
Method 3: Reflux Distillation
Based on the result obtained in the laboratory, the ash content in tea leaves is in
average of 5.85% (± 0.14). The reference value for total ash content in teal leaves is in
the range of 4% to 8%. This shows the average obtained in laboratory is accurate. The
lid of crucible is slipped to one side to allow 80% to 90% of water content in the
sample to evaporate so that water loss during evaporation can be calculated accurately
to obtain value moisture content in sample. Duplicate determination is made to
achieve better accuracy of result. Also, the water-soluble ash in tea leaves is in
average of 4.47% (± 0.13) and water-insoluble ash is 1.39% (± 0.28). Crucible should
be covered during weighting to avoid ash readily lost to the surrounding and affects
the accuracy of the data. The crucible used in the laboratory is made out of porcelain
due to its inert properties which will not readily react with the minerals in ash content
and heat-resistant during drying in oven under high temperature.
7.0 QUESTIONS
2. The aluminium pan liners used in the infra- red method of moisture
determination should be never be handled with your fingers. Tongs should
always be used. Why?
Tongs are used to avoid fingerprint formed on the aluminium pan liners since
infra-red is used to penetrate the aluminium pan liners. It will disturb the
refraction of infra-red, causing inaccuracy in result.
9.0 REFERENCE