Lab FST306 Moisture

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FOOD ANALYSIS

FST306
EXPERIMENT 1

TITLE DETERMINATION OF MOISTURE


GROUP AS1163B2
PREPARED BY 1. FARIS DANIAL BIN FAIZUL UMRI (2018273768)
2. MOHAMAD BARSYIK MIRZA BIN MOHAMED
ARSHAD (2019241704)
3. KHAIRUL NISAK BINTI MOHAMAD SHARIN
(2019280956)
4. NURUL SAKINAH BINTI CHE RAHI (2019426508)
5. SITI NURAISHAH ATIRAH BINTI MUHAMAD LATEF
(2019410758)
DATE OF EXPERIMENT 22 OCTOBER 2020
DATE OF SUBMISSION 10 DECEMBER 2020
INSTRUCTOR MADAM NUR AISYAH BINTI ISMAIL

1
INTRODUCTION
Food moisture analysis involves the whole coverage of the food items in the world because
foods are comprising a considerable amount of water rather than other ingredients. Moisture
content is derived from the loss of product weight during drying by measuring the change in
mass of a sample while being heated at a controlled rate until no more change in weight is
observed. Moisture content of the food material is important to consider the food is suitable
before the consumption, because moisture content affects the physical, chemical aspects of
food which relates with the freshness and stability for the storage of the food for a long
period of time and the moisture content determine the actual quality of the food before
consumption and to the subsequent processing in the food sector by the food producers.

The simplest method to measure moisture content is based on gravimetric where the loss of
weight due to water evaporations is calculated. This can be accomplish using air oven,
vacuum oven, convection oven or other sophisticated instruments such as infra-red lamp,
halogen radiator and microwave energy. An instrument such as Moisture Analyser used in
this experiment operators on the thermo gravimetric principle. This instrument first measure
the initial weight of sample and then the sample is quickly heated by an integral halogen
dryer unit to vaporize the water. During the drying operation, weight of the sample is
continuously determines until at the completion of drying result is displayed as percent
moisture content.

Other methods for moisture determination include distillation and chemical methods. For
distillation method, moisture is removed from the sample by distillation as an azeotrope with
toluene. The water is collected in a suitable trap and its volume is measured at a known
temperature. This method is applicable to all unmodified starches, most modified starches
and many starch products. For chemical method, the most accurate and specific method for
determining the water content of a substance is Karl Fischer titration. It is based upon the
reaction of iodine with sample water, in presence of alcohol solvent, sulphur dioxide, and a
base. Unfortunately, this method is not suitable for foods of high moisture content. It is
applicable to foods that give erratic result when heated or placed under vacuum for example
dried fruits and vegetables, oils, candies and chocolate.

OBJECTIVES

1. To determine the moisture content of selected food using oven drying method.
2. To determine the moisture content of food selected using moisture analyser.

2
APPARATUS

MATERIALS

METHOD

OVEN DRYING METHOD

Procedur:

1. An aluminium dish was dried with cover for 4 hours in an oven at 105 oc. The dish is
been transferred into the desiccator to let it cool and weighed after it attained room
temperature
2. About 5 g of homogenized sample was weighed approximately into the aluminium
dish
3. The sample was placed uncover, in the oven overnight at 60oc
4. While dish is still in the oven, the lid is been replaced, remove dish from oven. Cool
in desiccator band soon weighed after attaining room temperature. Record the weight
obtained
5. The drying process (step 3 and 4) was repeated until constant weight is achieved
6. The percentage of moisture is been calculated

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DRYING METHOD (MOISTURE ANALYSER)

Procedure
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 and set the drying parameter based on the following:

Drying temperature: 150oc


Profile: standard
Switch OFF Time: 15 minutes
Display set: % moist
Target weight: 1g
Program: Auto switch-off

3. The cover of the instrument was opened and the pan is been cleared
4. An empty sample pan is been placed in the pan handler and the pan handler was
placed 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 plan handler
5. The TARE button is been pressed to sets reading to zero
6. About 1g of sample is been placed, evenly distributed in the sample pan. The cover
was closed
7. Press the START/STOP button to start the drying process
8. At the end of the drying process, the result display for % moist was read and the
reading was recorded in the Data Sheet.
9. The cover is been opened and the pan handler was carefully lifted from the chamber
to remove the sample.

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RESULT

DETERMINATION OF MOISTURE
DATA SHEET
Table 1.1: Determination of Moisture Data using Oven method
Sample Trial Aluminium Initial Aluminium % Moisture
dish + cover (g) sample dish + cover
weight (g) + dried
sample
1 25.6778 5.02 28.9408 35.00
Bread 2 25.7761 5.06 29.0297 35.70
3 25.5998 5.04 28.8556 35.40
Mean±SD 35.47
1 25.6554 5.03 28.8193 37.10
Cheese 2 25.7001 5.00 28.8507 37.00
3 25.5887 5.07 28.7637 37.40
Mean±SD 37.27

Table 1.2: Determination of Moisture Data Using Moisture Analyzer method


Sample Trial % Moisture
1 12.05
Wheat flour 2 12.00
3 12.02
Mean±SD 12.04
1 4.01
Milk powder 2 4.00
3 4.03
Mean±SD 4.02

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DISCUSSION

Oven Drying Method:

In this practical, we have learned how to determine the moisture content of selected food
sample using drying oven method. In this experiment, bread and cheese was used as a
sample. It was dried uncovered in the oven overnight at 60C after it removed from the oven
and cooled down it in desiccator. It was weight after attaining room temperature. The weight
was recorded in Table 1.1 on Data Sheet.

Based on our experiment, we do three trials to the determine the moisture of bread and
cheese. So, for our result shows bread has moisture of 35.47% while cheese has 37.27%. If
we compared both of bread and cheese, cheese has higher moisture than bread. For
theoretical value, moisture content of bread is 37.5%. Meanwhile, moisture content for
cheese is about 30%. Thus, we can see the different between the sample value and theoretical
value.

The error may occur during this experiment is instrumental error. The weighing balance has a
zero error, and it may be due to personal error. Furthermore, the sample itself can cause to the
error. The sample was exposed to air for a long period. To overcome this error, make sure the
entire instrument in a good condition before do the experiment.

Drying Method (Moisture Analyser):

In this practical, we learned how to determine the moisture content of selected food samples
using moisture analyser. In this experiment, wheat flour and milk powder were used as a
sample. It was dried and analysed by using moisture analyser. The weight was recorded in
Table 1.2 on Data Sheet.

Based on our experiment, we also do three trials to determine the moisture of wheat flour and
milk powder. The result shows wheat flour has moisture of 12.04% while milk powder has
4.02%. If we compared both wheat flour and milk powder, wheat flour has higher moisture
than milk powder. For theoretical value, moisture content of wheat powder is 14%.
Meanwhile, moisture content for milk powder is around 3-4%. Thus, we can see the different
between the sample value and theoretical value.

6
CONCLUSION

To sum up, in this practical, we learned how to determine the moisture content of selected
food samples using drying oven method. Bread and cheese was dried uncovered in the oven
overnight at 60C after it was removed from the oven and cooled down. The result shows
bread has moisture of 35.47% while cheese has 37.27%. If we compared both of bread and
cheese, cheese has higher moisture than bread. The error may occur during this experiment is
instrumental error.

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QUESTION

1) Identify five (5) factors that you need to consider when choosing a moisture
analysis method for specific food product.
 the measurement principle
 contact method
 testing techniques
 advantages and disadvantages
 typical applications

2) In the drying oven method, why do you allow the sample to get cool before
weighing?

Because weighing the sample while it is hot will cause inaccurate measurements because as
the sample cools, the weight fluctuates due to convection currents and give an incorrect
measurement.

3) Discuss possible errors involves in using distillation method.

- Formation of emulsions between the water and the solvent because its difficult to
separate.

- Water droplets adhere inside of the glassware.

- Decomposition of thermally labile sample with production of water can occur at the
elevated temperature used.

4) Does the pigment in the toluene from analysis of turmeric powder represent
moisture? Explain.

No, because the pigment in the toluene is oil which is lipid. Toluene was dissolving other
substances easily because toluene is known as a good solvent than water and also toluene
evaporates quickly into the air.

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5) What are the advantages and disadvantages that you observed from the method
conducted in this practical?

OVEN DRYING METHOD

ADVANTAGES DISADVANTAGES

 Several sample can be determined at   requires extended heating periods


the same time and cooling phases, it means this
 produces high accuracy result method takes a few hours for the
result.
 This method procedures are
involving many manual steps.
Therefore, the potential for error is
high

DRYING METHOD (MOISTURE ANALYSER)

ADVANTAGES DISADVANTAGES

 Fast measurement less than an hour  Sample material may decompose or


 Simple handling evaporate
 Only one measurement can be
performed at one time

9
REFERENCES
1. FNH teaching lab (8 August 2016) Moisture Determination
https://www.youtube.com/watch?v=Y11mFljmrAE

2. DR.Liji Thomas, MD (28 August 2018) Moisture analysis Techniques


https://www.news-medical.net/life-sciences/Moisture-Analysis-
Techniques.aspx#:~:text=Chemical%20Methods%20for%20Moisture
%20Analysis&text=The%20most%20accurate%20and%20specific,sulfur%20dioxide
%2C%20and%20a%20base.

3. MicroChem’s Experiments (5 July 2020) Determination of Moisture Content


https://www.youtube.com/watch?v=DtSH8n1jbyM

4. https://en.wikipedia.org/wiki/Food_moisture_analysis

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FOOD ANALYSIS
FST306
EXPERIMENT 2

TITLE DETERMINATION OF FAT


GROUP AS1163B2
PREPARED BY 6. FARIS DANIAL BIN FAIZUL UMRI (2018273768)
7. MOHAMAD BARSYIK MIRZA BIN MOHAMED
ARSHAD (2019241704)
8. KHAIRUL NISAK BINTI MOHAMAD SHARIN
(2019280956)
9. NURUL SAKINAH BINTI CHE RAHI (2019426508)
10. SITI NURAISHAH ATIRAH BINTI MUHAMAD LATEF
(2019410758)
DATE OF EXPERIMENT 26 NOVEMBER 2020
DATE OF SUBMISSION 10 DECEMBER 2020
INSTRUCTOR MADAM NUR AISYAH BINTI ISMAIL

11
INTRODUCTION
Lipids are one of the major constituents of foods, and are important in our diet as a major
source of energy and providing essential fatty acids. It also plays a major role in determining
the overall physical characteristics of foods, such as flavour, texture, mouth feel and
appearance. Lipids are usually defined as those components that are soluble in organic
solvents such as ether, hexane or chloroform, but are insoluble in water.

The fat content of foods for some purposes can be determined by solvent extraction methods,
non-solvent extraction methods, and instrumental methods that rely on physical and chemical
properties of lipids. Solvent extraction techniques are one of the most used methods to isolate
lipids from foods and determine the total lipid content in foods. The Soxhlet method is often
the method of choice as a routine test. Crude fat content is determined by extracting the fat
from the sample using a solvent, the determining the weight of the fat recovered.

OBJECTIVE
1. To determine the fat content of selected food samples using Soxhlet method.

APPARATUS

MATERIALS

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METHOD
1. 2g of dried sample is weighed accurately into an extraction thimble or a piece of filter
paper.
2. The opening of the thimble loosely is plug with cotton or the filter is fold and plug
with cotton.
3. The thimble or paper and content is placed into a Soxhlet extractor.
4. A dried round bottom flask is weighed and 150ml of petroleum ether is added.
5. The apparatus is connected to the condenser, the water is turned on and extract for a
minimum of 8 hours on an electrothermal extraction unit.
6. The flask containing the petroleum ether extract is removed after the extraction
complete.
7. The petroleum ether is evaporated off on a boiling water bath.
8. The flask is transfer into an oven at 105℃ for one hour to dry the extract.
9. The flask is transferred immediately into a desiccator to cool and weighed.

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RESULT
DETERMINATION OF FAT

DATA SHEET
Table 2.1: Determination of Fat Data using Soxhlet method
Sample Trial Weight of Weight of Weight of % Fat
Sample (g) round round
bottom bottom
flask (g) flask + fat
(g)
1 2.01 93.9 95.6 84.58
2 2.05 94.0 95.3 63.41
Milk Powder
3 2.02 93.9 94.8 44.55
Mean 64.18
1 2.1 94.2 95.6 66.67
2 2.05 93.9 94.9 48.78
Cheese
3 2.03 94.1 95.3 59.11
Mean 58.19

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DISCUSSION
In this experiment, Soxhlet method apparatus was found to be about 95% effective. The fat
contents obtained may be a little below the actual fat content of the product. The fat was
extracted by using Soxhlet apparatus which functions by drippong pure ether through a fat
containing substance. The fat content can be determined by weight of fat sample and weight
of sample taken. For this experiment, we used milk powder and cheese. The first trial of milk
powder is, the fat content is 84.58%, second trial is 63.41% and last trial is 44.55%. the first
trial has the highest fat content compared with second and last trial. So, in order to get
accurate result, the experiment was repeated at least three time. The average fat content in
milk powder is 64.18%.

In cheese sample, the same procedur was repeated. For the first trial of cheese sample, we get
66.67%, second trial is 48.78% and the last trial is 59.11%. It is the same with milk powder,
cheese also repeated three times to obtain an exact results. The average of fat content in
cheese sample is 58.19%. So we can conclude that milk powder has more fat content than
cheese. However the higher fat content compared to milk powder is expected to be cheese,
since the Soxhlet method is not appropriate for cheese. So, after all Soxhlet method is not
suittable for cheese because of the bound nature of the fat. Cheese has low fat content
compared to milk powder. It is because the bound fat is not included in the reading of fat
content.

The errors that will occur in this experiment are that the extraction takes too much time than
the actual time indicated. This is because the preparation of the sample is very much affected
by the dissolving process.

15
CONCLUSION

To sum up, milk powder sample has more fat content than cheese sample. The average of
milk powder is 64.18% while cheese is 58.19%. However the higher fat content compared to
milk powder is expected to be cheese, since the Soxhlet method is not appropriate for cheese.
It is because the bound fat is not included in the reading of fat content. So, the objective was
achieved.

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QUESTION

1. Draw and label main components of Soxhlet apparatus

2. Which is the best extraction procedure

This Soxhlet method is better with several extraction with smaller volume but same
volume than one extraction with larger volume. It is because maybe in the first extraction,
they still left fat content in the sample, so if just do one extraction it will get an error in fat
content and several extractions is better that can make result more accurate.

17
REFERENCES
a. Kellen Xu, (2 July 2017) Fat Analysis using Soxhlet Method
https://www.youtube.com/watch?v=f-psdtCdq64

b. Meat Techmology-information sheet, (1998) Crude Fat Determination-Soxhlet


Method
https://meatupdate.csiro.au/infosheets/Crude%20Fat%20Determination%20-
%20Soxhlet%20Method%20-%201998.pdf

c. SHAFIKANOR3661, (31 January 2014) Lab Food Analysis-fat


https://www.scribd.com/doc/203587765/Lab-Food-Analaysis-fat

d. Wanizalil, (8 November 2015) Fat Determination Soxhlet


https://www.scribd.com/document/288947382/Fat-Determination-Soxhlet

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FOOD ANALYSIS
FST306
EXPERIMENT 3

TITLE DETERMINATION OF SUGAR BY REFRAVTOMETRIC AND


VOLUMETRIC METHODS
GROUP AS1163B2
PREPARED BY 11. FARIS DANIAL BIN FAIZUL UMRI (2018273768)
12. MOHAMAD BARSYIK MIRZA BIN MOHAMED
ARSHAD (2019241704)
13. KHAIRUL NISAK BINTI MOHAMAD SHARIN
(2019280956)
14. NURUL SAKINAH BINTI CHE RAHI (2019426508)
15. SITI NURAISHAH ATIRAH BINTI MUHAMAD LATEF
(2019410758)
DATE OF EXPERIMENT 5 NOVEMBER 2020
DATE OF SUBMISSION 10 DECEMBER 2020
INSTRUCTOR MADAM NUR AISYAH BINTI ISMAIL

19
INTRODUCTION

Carbohydrates are one of the most important components in many foods. Carbohydrates
maybe present as isolated molecules or they may be physically associated or chemically
bound to other molecules. Individual molecules can be classified according to the number of
monomers that they contain as monosaccharides, oligosaccharides or polysaccharides.
Molecules in which the carbohydrates are covalently attached to proteins are known as
glycoproteins, whereas those in which the carbohydrates are covalently attached to lipids are
known as glycolipids. Some carbohydrates are digestible by humans and therefore provide an
important source of energy, whereas others are indigestible and therefore do not provide
energy. Indigestible carbohydrates form part of a group of substances known as dietary fiber,
which also includes lignin. As well as being an important source of energy and dietary fiber,
carbohydrates also contribute to the sweetness, appearance and textural characteristics of
many foods.

A number of chemical methods used to determine monosaccharides and oligosaccharides are


based on the fact that many of these substances are reducing agents that can react with other
components to yield precipitates or colored complexes which can be quantified. The
concentration of carbohydrate can be determined gravimetrically, spectrophotometrically or
by titration. Many different chemical methods are available for quantifying carbohydrates.
Most of these can be divided into three categories: titration (Lane-Eynon Method),
gravimetric (Munson-Walker Method) and colorimetric (Somogyi-Nelson Method). For
different physical methods have been used to determine the carbohydrate concentration of
foods. These methods rely on their being a change in some physicochemical characteristic of
a food as its carbohydrate concentration varies. Commonly used methods include
polarimetry, refractometry, IR, and density.

OBJECTIVE

1. To determine the total soluble solids of selected food samples using refractometric
method.

20
APPARATUS
Burette 50mL, Erlenmeyer flask 300mL, hot plate, retort stand, dropper

MATERIALS
Fehling’s solution no 1 and 2, methylene blue

METHOD
Refractometric

1. The secondary prism is opened and 2-3 drops of specimen are dropped onto the centre of
the main prism. The secondary prism is closed gently.
2. While looking through the eyepiece, the measurement knob is turned slowly until the
boundary line appears in the refraction field of vision.
3. The Refractive Index and the Brix is read.

Lane-Eynon’s Titration:

Preparation of chemical reagents

1. Fehling’s solution A: 69.28 g CuSO4.5H2O and 1.0 ml of 1 M H2SO4 are dissolved in water
and make up to 1.0 litre water.
2. Fehling’s solution B: 346 g KNaC4H4O6.4H2O and 100 g NaOH is dissolved in water and
make up 1.0 litre water.
3. Mixed Fehling’s solution: Equal volumes of Fehling’s solution A is mixed and B by pipetting
4. Methylene blue: 1 % aqueous solution

Preliminary titration

The solution, inverted if necessary, should normally be cleared first with zinc ferrocyanide and the
concentration should be adjusted to give a titre between 15 and 50ml (0.1-0.3 g of sugar per 100 mL
for 10 mL of Fehling’s solution, 1.25-0.8 g of sugar per 100 mL for 25 mL of Fehling’s solution)

1. The burette is filled with sugar solution.


2. 10 ml (or 25 ml) of mixed Fehling’s solution is pipetted into a conical flask and 10-15 ml of
sugar solution is added from the burette.

21
3. The flask is heated on hotplate (or plain wire gauze supported on by tripod stand) and let the
liquid boils briskly.
4. 4 drops of 1% methylene blue are added further additions of sugar solution is made at a rate
of 1 ml per second. The liquid is kept boiled throughout, continue added until the blue
colour is discharged (titre=A ml)

Accurate titration

1. 10 ml of mixed Fehling’s solution is pipetted into a conical flask and (A-2) ml of sugar
solution is added from the burette.
2. The flask round is swirl, heated it on the hotplate and the liquid is boiled moderately for 1 ½
- 2 min; 4 drops of methylene blue solution is added.
3. The sugar solution is added about 2-3 drops per second and the titration is completed within
3 min from the time boiling commences.
4. The dextrose table is used to calculate the concentration of sugar in the solution.

22
RESULT

23
DISCUSSION

24
CONCLUSION

25
QUESTION

1. What are reducing sugar?


- A reducing sugar is any sugar that is capable of acting as a reducing agent because
it has a free aldehyde group or a free ketone group.

2. What is refractive index?


- Refractive Index (Index of Refraction) is a value calculated from the ratio of the
speed of light in a vacuum to that in a second medium of greater density.

3. Write the principle reaction (chemical reaction) that occurs in the Lane-Eynon’s
determination of reducing sugar.
- Reducing sugar + Cu 2+ + Base Oxidized sugar + Cu2O (precipitate) Principle are
based on the reaction of reducing sugar with a solution of copper sulphate
followed by reaction with alkaline titrate. Then, the mixture will be boiled for a
specific time with the addition methylene blue.

4. Why is the sample boiled during titration?


- To ensure that the highest reducing power of the sugar was achieve.

26
REFERENCES

1. Ahnaf Irfan (2020) Determination of Sugar by Refractometric and Volumetric Methods


https://www.studocu.com/my/document/universiti-teknologi-mara/food-
analysis/practical/experiment-4-determination-of-sugar-by-reftractometric-and-volumetric-
methods/10043863/view

2. SHAFIKANOR3661 (24 January 2014) Determination of sugar


https://www.scribd.com/doc/201857037/Determination-of-sugar

3. Shashi 12 (2020) PRACTICAL 4 food ana determination of sugar


https://www.coursehero.com/file/25570844/PRACTICAL-4-food-ana-determination-of-
sugardocx/

27
FOOD ANALYSIS
FST306
EXPERIMENT 4

TITLE DETERMINATION OF STANDARD ERYTHROSINE


CONCENTRATION USING UV-VISIBLE
SPECTROPHOTOMETER
GROUP AS1163B2
PREPARED BY 16. FARIS DANIAL BIN FAIZUL UMRI (2018273768)
17. MOHAMAD BARSYIK MIRZA BIN MOHAMED
ARSHAD (2019241704)
18. KHAIRUL NISAK BINTI MOHAMAD SHARIN
(2019280956)
19. NURUL SAKINAH BINTI CHE RAHI (2019426508)
20. SITI NURAISHAH ATIRAH BINTI MUHAMAD LATEF
(2019410758)
DATE OF EXPERIMENT 12 NOVEMBER 2020
DATE OF SUBMISSION 10 DECEMBER 2020
INSTRUCTOR MADAM NUR AISYAH BINTI ISMAIL

28
INTRODUCTION

Spectrophotometer is an instrument that measures the amount of photons (the intensity of


light) absorbed after it passes through sample solution. With the spectrophotometer, the
amount of a known chemical substance (concentrations) can also be determined by measuring
the intensity of light detected. It is based on a simple design of passing light of a known
wavelength through a sample and measuring of the amount of light energy that is transmitted.
Wavelength range for uv-light which is colourless to human eyes id 190 – 350 nm and visible
light (violet – red) is 350 – 700 nm.

OBJECTIVES

1. To obtain the absorption spectrum wavelength for the dye solution


2. To determine the wavelength of maximum absorbance from the spectrum
3. To produce a standard calibration curve from the series of standard solutions
4. To use the standard curve to determine the concentration of an uknown solution
5. To compare between single beam and double beam spectrophotometer

APPARATUS
Double beam UV-Visible spectrophotometers, waste beaker, a pair of cuvettes, volumetric
flask

MATERIAL
Distilled water, blank solution, dye solution

29
METHOD

30
RESULT

31
DISCUSSION

32
CONCLUSION

33
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