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(STKM 2311)


MATRIX NO: A155560




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 determination of moisture content is one of most vital and fundamental

analytical procedures in food analysis. The approximate water content of a food can
affect the choice of method analysis. There are many methods can be used in
determine the moisture content depending on:
a) the form in which water is present
b) nature of product analyzed
c) rapidity of determination
d) accuracy desired
e) availability and cost of equipment required

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 110.6C, 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.


Ash is inorganic residue remaining after ignition or complete oxidation of

organic matter in foodstuff. Ash is an important part of proximate analysis for
nutritional information. Ferum, magnesium, zinc, calcium, sodium, potassium and
phosphorus are some of the minerals present in ash from food. By ashing, the mineral
contaminants in food can be measured, such as sand in dried fruits and vegetables.
Ashing is the first step in the preparation of a food sample for elemental analysis.

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 600C. 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.


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.


Method 1: Oven Method
Analytical balance, desiccator with some moisture absorbent (silica gel, calcium
chloride, concentrated sulphuric acid etc.), nickel dish with lid (filled with
predried sand and a glass rod), oven (set at 105C), tongs

Method 2: Infra-red Metnod

Desiccator with some moisture absorbent (silica gel, calcium chloride,
concentrated sulphuric acid etc.), disposable aluminum pan liner, infra-red balance

Method 3: Reflux Distillation

Aluminum foil, analytical balance, distillation apparatus with Bidwell-Sterling
moisture trap, distillation flask 300mL, graduated cylinder 250mL


Determination of total ash in tea leaves
Analytical balance, crucibles and lids 15-20mL, desiccator with some moisture
absorbent (silica gel, calcium chloride, concentrated sulphuric acid etc.), electic
heating mantle placed in a fume hood, muffle furnace with tempertature display,
thick gloves, tongs

Water-soluble and water- insoluble ash

Analytical balance, ashless filter paper, 100mL beaker, 100mL conical flask,
desiccator with some moisture absorbent (silica gel, calcium chloride,
concentrated sulphuric acid etc.), electric heating mantle, funnel, 25 mL graduated
cylinder, muffle furnace with tempertature display, hot distilled water, ash from
Part A


Method 1: Oven Method

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 105C.

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 100C overnight and left to cool in

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).

Method 3: Reflux Distillation

10g sample is weighted approximately onto a piece of aluminum foil and well

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 450-550C overnight in a
muffle furnace, cooled in a desiccators and weighted after reaching room

5g of tea leaves is weighted approximately in a crucible with its lid. It is done in

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 450-550C.

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
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

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 100C overnight. Using safety tongs, the crucible is
transferred quickly to a dessicator. The crucible is allowed to cool prior to

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.


Method 1: Oven Method (Minced meat)

1st reading (g) 2nd reading (g)

Dish with glass rod and lid 25.0600 59.8700
Meat sample (before drying) (W1) 5.3391 5.3690
Dish with glass rod, lid, meat (before
30.3845 65.2390
drying )
Dish with glass rod, lid, meat (after
26.8605 61.7827
drying ) (W2)
Meat sample (after drying) (W2) 30.3845 – 26.8605 = 65.2390 – 61.7827
3.5240 = 3.4563


𝑊1 − 𝑊2
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒(%) = x 100


W1 = weight (g) of sample before drying

W2 = weight (g) of sample after drying

1st reading 2nd reading

𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒(%) 𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒
5.3391 − 3.5240 5.3690 − 3.4563
= 𝑥 100 = 𝑥 100
5.3391 5.3690
= 34.0% = 35.62%

𝑨𝒗𝒆𝒓𝒂𝒈𝒆 𝒎𝒐𝒊𝒔𝒕𝒖𝒓𝒆 𝒄𝒐𝒏𝒕𝒆𝒏𝒕 𝒐𝒇 𝒎𝒆𝒂𝒕

34.0 + 35.62
= 34.81%
Method 2: Infra-red Method (Flour)

Moisture loss percent (%)

Average of moisture loss
Time (min) 1st reading 2nd reading
(%) (g) (%) (g) (%) (g)
1 1.09 0.11 1.79 0.18 1.44 0.15
2 2.16 0.22 2.71 0.27 2.44 0.25
3 3.26 0.33 3.63 0.36 3.45 0.35
4 4.34 0.43 4.48 0.45 4.41 0.44
5 5.23 0.52 5.29 0.53 5.26 0.53
6 6.08 0.61 6.04 0.60 6.06 0.61
7 6.85 0.69 6.73 0.67 6.79 0.68
8 7.54 0.75 7.37 0.74 7.46 0.75
9 8.16 0.82 7.94 0.79 8.05 0.81
10 8.72 0.87 8.49 0.85 8.61 0.86
11 9.22 0.92 8.97 0.90 9.10 0.91
12 9.67 0.97 9.41 0.94 9.54 0.96
13 10.07 1.01 9.82 0.98 9.95 1.00
14 10.43 1.04 10.19 1.02 10.31 1.03
15 10.76 1.08 10.53 1.05 10.65 1.07
16 11.05 1.11 10.83 1.08 10.94 1.10
17 11.31 1.13 11.10 1.11 11.21 1.12
18 11.54 1.15 11.35 1.14 11.45 1.15
19 11.75 1.18 11.56 1.16 11.66 1.17
20 11.94 1.19 11.75 1.18 11.85 1.19
21 12.11 1.21 11.95 1.20 12.03 1.20
22 12.26 1.23 12.10 1.21 12.18 1.22
23 12.39 1.24 12.25 1.23 12.32 1.23
24 12.51 1.25 12.38 1.24 12.46 1.25
25 12.63 1.26 12.49 1.25 12.56 1.26
26 12.73 1.27 12.59 1.26 12.66 1.27
27 12.81 1.28 12.68 1.27 12.75 1.28
28 12.89 1.29 12.76 1.28 12.83 1.28
29 12.96 1.30 12.83 1.28 12.90 1.30
30 13.02 1.30 12.95 1.30 12.99 1.30

𝑴𝒐𝒊𝒔𝒕𝒖𝒓𝒆 𝒄𝒐𝒏𝒕𝒆𝒏𝒕 𝒐𝒇 𝒇𝒍𝒐𝒖𝒓 = 𝟏. 𝟑𝒈

Graph moisture loss (g) against time (min)






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






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)

Average of moisture loss in reading 1 and 2 (g)

Method 3: Reflux Distillation (Margarine)


Sample weight (g) 10.20

Volume of water collected (ml) 1.20


𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 𝑐𝑜𝑙𝑙𝑒𝑐𝑡𝑒𝑑

𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 (%) = x 100
𝑆𝑎𝑚𝑝𝑙𝑒 𝑤𝑒𝑖𝑔ℎ𝑡

𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 (%) = 𝑥 100
= 11.76%

Moisture content of margarine = 11.76%

1) Determination of total ash in tea leaves

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

Weight of tea leaves (g) 5.05 5.04

Weight of crucible with tea leaves
54.54 51.95
and lid (g)
Weight of crucible with ash and
49.79 47.20
lid (g) (after drying)
Weight of ash (g) 49.79 – 49.49 = 0.30 47.20 – 46.91 = 0.29
0.30 0.29
Total ash (%) 𝑥 100 = 5.94% 𝑥 100 = 5.75%
5.05 5.04

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑡𝑜𝑡𝑎𝑙 𝑎𝑠ℎ (𝑔) 𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

0.30𝑔 + 0.29𝑔
= (0.30 − 0.2950)2 + (0.29 − 0.2950)2
2 = √
= 0.2950𝑔 2−1
= 0.01

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑡𝑜𝑡𝑎𝑙 𝑎𝑠ℎ (%) 𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

5.94% + 5.75%
= (5.94 − 5.85)2 + (5.75 − 5.85)2
2 = √
= 5.85% = 0.14

Average total ash = 5.85 ± 0.14

2) Water-soluble and water-insoluble ash


Water – insoluble ash (g) = [(weight of crucible + water – insoluble ash) –

(Weight of crucible)
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟 − 𝑖𝑛𝑠𝑜𝑢𝑏𝑙𝑒 𝑎𝑠ℎ
𝑾𝒂𝒕𝒆𝒓 − 𝒊𝒏𝒔𝒐𝒍𝒖𝒃𝒆 𝒂𝒔𝒉 (%) = X 100
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
𝑾𝒂𝒕𝒆𝒓 − 𝒔𝒐𝒍𝒖𝒃𝒍𝒆 𝒂𝒔𝒉 (%) = (% 𝑇𝑜𝑡𝑎𝑙 𝑎𝑠ℎ) − (% 𝑊𝑎𝑡𝑒𝑟 − 𝑖𝑛𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ)

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
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

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑤𝑎𝑡𝑒𝑟 − 𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ(𝑔) 𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

0.08𝑔 + 0.06𝑔 (0.8 − 0.07)2 + (0.06 − 0.07)2
= √
2 =
= 0.07𝑔
= 0.01

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑤𝑎𝑡𝑒𝑟 − 𝑖𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ (%)

(1.58 − 1.39)2 + (1.19 − 1.39)2
1.58% + 1.19% =√
= 2−1
= 1.39% = 0.28

𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

Average water – insoluble ash (%) = 1.39% ± 0.28

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑤𝑎𝑡𝑒𝑟 − 𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ (𝑔)
(0.22 − 0.2250)2 + (0.23 − 0.2250)2
0.22𝑔 + 0.23𝑔 =√
= 2−1
= 0.2250𝑔 = 0.01

𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝑑𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑤𝑎𝑡𝑒𝑟 − 𝑠𝑜𝑙𝑢𝑏𝑙𝑒 𝑎𝑠ℎ (%) 𝑆𝑡𝑎𝑛𝑑𝑎𝑟𝑑 𝐷𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛

4.37% + 4.56%
= (4.37 − 4.47)2 + (4.56 − 4.47)2
2 =√
= 4.47%
= 0.13

Average water-soluble ash (%) = 4.47% ± 0.13



Method 1: Oven Method
Based on the results obtained from the laboratory, the moisture content in
minced meat is 34.81% as compared to 64% fresh meat reported in food safety
information in the US Department of Agriculture Food Safety and Inspection Service.
Minced meat is defined as meat that has passed through the mincing machine as
compared to fresh meat which is chopped down from the domestic animal. The
difference moisture content in minced meat and fresh meat maybe due to during the
mincing process some water content in the meat has been squeezed out and hence
reduces the moisture content. There might be errors occurred during laboratory. Long
duration during spreading the meat sample on the dish using glass rod causing water
content in the meat sample evaporates to the atmosphere. This might lead to errors in
moisture content determination. So, exposure of meat to the environment should be
minimized to avoid moisture in the air adsorbed by the meat. The purpose of adding
sand is to enhance heat absorption and distributed evenly in the meat sample.

Method 2: Infra-red Method

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 moisture content of

margarine is 11.76% which is in the range less than 18% according to article on
margarine by Due to emulsifying process, small drops of moisture will
be added into fats in processing margarine. According to the law, margarine can have
a maximum moisture content of 18% and this proves the data obtained from this
laboratory can be acceptable. However, based on USDA Nutrient Database, moisture
content of margarine is 15.77%. The small differences might due to several errors
during carry out the distillation in laboratory. One of the errors is formation of
emulsion that will not break. So, the apparatus should be allowed to cool after
distillation is completed and before reading the amount of moisture in the trap.
Toluene is used in this laboratory instead of hexane because hexane has lower boiling
point than water, while toluene has slightly higher boiling point than water.


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.

1. What role does moisture determination play in food analysis?

It helps to determine the amount of water or moisture content in food which will
influence the structure, appearance, flavor of food and food spoilage process.

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.

3. What is the importance of ash determination in foods? What does unusually

high ash content in a sample indicate?
Ash determination can measure the mineral contaminants in food as it serves as an
indicator for quality of food products from the aspect of purity. High ash content
indicates high contamination in a sample.

4. What do you do if there are black specks remaining after ashing?

It indicates that organic matter undergoes combustion that is incomplete.
Continuous heating required until the light- grey residue is observed.

The moisture content of minced meat is 34.81% by oven method, flour is

12.99% by infra-red method and margarine is 11.76%. Furthermore, the ash content in
tea leaves is 5.85% (± 0.14) in which content 1.39% (± 0.28) water-insoluble ash and
4.47% (± 0.13) water soluble ash.


1) Peter S. Murano. 2003. Understanding Food Science and Technology. Thomson

Wadsworth, USA.
2) S. Suzanne Nielsen, 2010. Food Analysis. Fourth Edition. Chapter 6, pp 106.
Springer New York Dordrecht Heidelberg London.