Food Analysis

Efendi Oulan Gustav Hakim Nata Buana, S.TP. M.Eng.

Aprilia Fitriani, S.TP., M.Sc.
 Course Contract
• 80% minimum attendance. Fail to do so
Component Percentage (%) without prior notification, you’ll get D.

Quiz 10 • Assignment could be either paper work or

presentation.
Assignment 20
•Your participations during class are
Middle Term 30 highly encouraged

Final Term 30 Grade Score Grade Score

A 86 C 56
Activity 10
AB 78,5 CD 48,5
Total 100 B 71 D 41
BC 63,5 E 0
 Course Content
Schedule Chapter Lecturer

1 3 April 2018 Sampling Technique EOG

2 10 April 2018 Moisture & Total Solids APF

analysis
3 17 April 2018 Carbohydrate Analysis APF
4 24 April 2018 Protein Analysis EOG
5 1 Mei 2018 Lipid Analysis APF
6 8 Mei 2018 Mineral & Ash Analysis EOG
7 15 Mei 2018 Vitamin Analysis APF
UTS
 Course Content
Time Chapter Lecturer

8 29 Mei 2018 Mass Spectometry APF

9 5 Juni 2018 Chromatography APF
10 12 Juni 2018 Pigment Analysis EOG
11 19 Juni 2018 Antioxidant Analysis APF
12 26 Juni 2018 Physical Properties Analysis EOG
13 3 Juli 2018 Toxin and Food Analysis EOG
14 10 Juli 2018 Electrophoresis and Immunological
EOG
Based Analysis
UAS
Moisture and Total Solid
Analysis

Aprilia Fitriani
 Why Moisture Content is
Important?
Food Quality
• Jams and jellies to prevent sugar crystallization
• Sugar syrups
• Prepared cereals
Food Preservation
• Dehydrated food
• Dried milk
• Spices and herbs
Convenience in packaging or shipping
• Concentrated milk
• Concentrated fruit juices

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 Why Moisture Content is
Important?

Calculate the other content of the food (dry weight basis)

• Carbohydrate content
• Ash content
• Protein and fat content
Compositional standart
• Cheddar cheese must be ≤ 39% moisture
• Enriched flour must be ≤ 15% moisture
• Pineaple juice must have soluble solids of ≥ 10,5° brix

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 Forms of Water in Foods
Free water

• This water retains its physical properties

• Acts as the dispersing agent for colloids and the solvent for salts

Adsorbed water

• This water is held tightly

• Is occluded in cell walls or protoplasm and is held tightly to protein

Water of hydration

• This water is bound chemically, example: some salts such as

Na2SO4.10H2O

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Zone of Moisture in A Typical Isotherm

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Zone of Moisture in A Typical Isotherm

Zone 1
• Tightly bound water.
• Requires lowering the aw to very low levels to remove it from direct
proximity to binding sites
Zone 2
• Intermediately bound water
• Loosely bound water perhaps in the secondarily binding sites on food
molecules
Zone 3
• Unbound water driven off by only a slight drop in aw

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Moisture
Content of
Selected
Foods

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Moisture
Content of
Selected
Foods

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 Moisture Analysis
Oven Drying Methods
• Oven drying; vacuum oven; forced draft oven; microwave
analyzer; Infrared drying; rapid moisture analyzer
Distillation Procedures
• Reflux distillation with immiscible solvent

Chemical Method: Karl Fischer Titration

Physical Method
• Dielectric Methods; Hydrometry; Refractometry; Infrared
analysis; Freezing Point

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 Oven Drying Methods

Principle
• Evaporate food moisture based on drying process till
we get the constant weight
Condition factors
• Room temperature and humidity
• Oven temperature
• Sample size and structure

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 Oven Drying Methods

Adventages
• Simple method
• Can be used for sample in bulk
Disadventages
• Volatile components that are not heat resistant will
be evaporated and counted as water loss
• Food components decomposition

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Oven Drying Instruments

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 Analysis procedures
Dry the empty dish and lid in the oven at 105°C for 3 H and transfer to
desicator to cool. Weigh the empty dish and lid

Weigh about 3 g of sample to the dish. Spread the sample with spatula

Place the dish with sample in the oven. Dry for 3 H at 105°C

After drying, transfer the dish with partially covered lid to the desicator to
cool. Reweigh the dish and its dried sample.

Place the dish with sample in the oven, again. Replicate the drying process till
get the constant weight.

Stop the drying process when obtained by the weight difference reaches
0.0002 g or 0.2 mg

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 Calculation
Moisture (wb%) = (W1 – W2) x 100% Moisture (db%) = (W1 – W2) x 100%
W1 W2

Where:
W1 = Weight (g) of sample before
Total solid (%) = W2 x 100%
drying
W1
W2 = Weight (g) of sample after drying

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 Problem Solving

You have the following drying method. The

results show that the weight of dried the dish
and the lid is 3.7641 g. Weight of the dish set
and tomato is 6.7662 g. Weight of the dish set
and dried tomato is 4.2761 g. Calculated the
moisture content of the sample and how much
the % solid content?

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 Problem Solving

• The weight of dried the dish and the lid is 3.7641 g.

• The weight of the dish set and tomato is 6.7662 g.
• The weight of the dish set and dried tomato is 4.2761 g.
Calculated the moisture content of the sample and how much the
% solid content?
• W1 = 6.7662 g – 3.7641 g = 3.0021 g
• W2 = 4.2761 g – 3.7641 g = 0.5120 g
• The moisture content:
% moisture content = (W1 – W2) x 100%
W1
= 82.9452 %
Solid content = W2 x 100% = 17.0547%
W1

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 Distillation Methods

Principle
• Separate the moisture in a food sample with a high boiling
point solvent that is immiscible in water. Collecting the
mixture that distills off, and then measuring the volume of
water.

Condition factors
• Immiscible solvent of higher boiling point than water.
• Liquid solvent with a flash point well above the boiling point
for water.

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 Distillation Methods

Adventages
• Rapid method
• Good accuracy
• Less thermal decomposition of some foods
Disadventages
• Using a solvent with a lower boiling point will
increase distillation time.
• Be careful reading the volume of water

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Analysis procedures Reflux Distillation
Place sample in distillation flask and cover completely with solvent.

Fill the receiving tube (e.g., Bidwell-Sterling Trap) with solvent, by pouring it through
the top of the condenser.

Bring to a boil and distill slowly at first then at increased rate.

After the distillation has proceeded for approximately 1 hr, use an adapted buret brush
to dislodge moisture droplets from the condenser and top part of the Bidwell-Sterling
trap.

Slide the brush up the condenser to a point above the vapor condensing area.

Rinse the brush and wire with a small amount of toluene to dislodge adhering water
drops.

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Analysis procedures Reflux Distillation
If water has adhered to the walls of the calibrated tube, invert the brush and use the
straight wire to dislodge this water so it collects in the bottom of the tube.

Return the wire to a point above the condensation point, and rinse with another small
amount of toluene.

After no more water has distilled from the sample, repeat the brush and wire routine to
dislodge adhering water droplets.

Rinse the brush and wire with toluene before removing from the condenser.

Allow the apparatus to cool to ambient temperatures before measuring the volume of
water in the trap.

Volume of water x 2 (for a 50 g sample) = % moisture

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Illustration aparatus

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Illustration aparatus

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 Illustration
aparatus

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 Distillation Methods
Direct/simple Distillation
• in direct distillation with
immiscible solvents of higher
boiling point than water, the
sample is heated in mineral oil
or liquid with a flash point
well above the boiling point
for water. Other immiscible
liquids with boiling point only
slightly above water can be
used (e.g., toluene, xylene, and
benzene)
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Reflux distillation
• Reflux distillation uses
either a solvent less dense
than water (e.g., toluene,
with a boiling point of
110.6◦C; or xylene, with a
boiling range of 137–140◦C)
or a solvent more dense than
water (e.g.,
tetrachlorethylene, with a
boiling point of 121◦C)
28
 Calculation
Moisture (%) = Volume of water (ml) x 100%
weight of initial sample (g)

Moisture (%) = volume of water x 2 (for a 50 g sample)

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 Problem Solving

1. You have the following destillation method.

The results show that the volume of water is
15 ml. Weight of the initial sample is 20 g.
Calculated the moisture content of the
sample!
2. I have 50 g initial sample for moisture
analysis. It has 10% moisture content. How
much volume of the water which i have using
destillation method?

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 Problem Solving

1. Destillation method.
volume of water = 150 mL
weight of the initial sample = 2 g
% moisture content = Volume of water (ml) x 100
weight of the initial sample (g)
= 15 x 100 %
20
= 75%
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 Problem Solving

2. Destillation method.
Weight of the initial sample = 50 g
% moisture content = 10%
Volume of water?
% moisture content = Volume of water (ml) x 100 %
weight of the initial sample (g)
10 % = V x 100 %
50
= 5 mL
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 Karl Fischer Titration
Principle
• Titration method for measuring water content which uses
sulphur dioxide and iodine.
Condition factors
• If the moisture in the sample is accessible,the reagent is
added directly as the titrant
• If moisture in a solid sample is inaccessible to the reagent,
the moisture is extracted from the food with an appropriate
solvent (e.g. methanol).
• Particle size affects efficiency of extraction directly.

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 Karl Fischer Titration
Adventages
• For determination of water in many low moisture foods
or any low moisture food high in sugar or protein.
• Quite rapid
• Accurate
• Uses no heat
Disadventages
• Solid sample must be extracted from the food with an
appropriate solvent.
• Long time preparation

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 Manual Karl
Fischer

Nielsen, S.S., 2010

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 Automatic
Karl Fischer

Nielsen, S.S., 2010

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 Karl Fischer Titration

• Coulometric titration is ideal for products with very low levels of

moisture, from 0.03% down. Volumetric titration procedure is
appropriate for samples with moisture content greater than ~0.03%
(100 ppm water to very high concentration).
• Karl Fischer Reagent (KFR) is added directly as the titrant if the
moisture in the sample is accessible. However, if moisture in a solid
sample is inaccessible to the reagent, the moisture is extracted from
the food with an appropriate solvent (e.g., methanol).

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 Sources of Error in The Karl Fischer
Titration

• Incomplete moisture extraction. Fineness of grind is important in

preparation of cereal grains and some foods.
• Atmospheric moisture. External air must not
be allowed to infiltrate the reaction chamber.
•Moisture adhering to walls of unit. All glassware and utensils must
be carefully dried.

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 Sources of Error in The Karl Fischer
Titration

•Interferences from certain food constituents. Ascorbic acid is

oxidized by KFR to dehydroascorbic acid to overestimate moisture
content; carbonyl compounds react with methanol to form acetals
and release water to overestimate moisture content (this reaction also
may result in fading endpoints); unsaturated fatty acids will react
with iodine, so moisture content will be overestimated.

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 Calculation

• A KFR water (moisture) equivalence (KFReq) must be

determined, before the amount of water found in a food sample.
•The KFReq value represents the equivalent amount of moisture
that reacts with 1 ml of KFR.
• Standardization must be checked before each use because the
KFReq will change with time.

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 Calculation

Pure water

Water-in-methanol
Established the KFReq
standart

Sodium tartrate dihydrate

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Calculation

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Calculation

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 Problem Solving

You have the following titration method to

titrate 10 g sample. You use 8 g sodium
tartrate dihydrate as a standart. The results
show that the volume of KFR for titration of
standart is 10 ml and 23 ml to titrate the
sample. Calculated the moisture content of
the sample!

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 Problem Solving

KFReq = 36 x 8 x 1000
230.08 x 10
= 125.1738
%H2O = 125.1738 x 23 x 100
10000
= 28,789 %

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It is Time to Cookiez (Cook the
Quiez)
1. Kedelai sebanyak 500 ton dikeringkan hingga memiliki kadar air
15%. Tentukan : 1) Berat air yang hilang selama proses pengeringan ?
2) Metode apa yang cocok untuk mengeringkan kedelai? Alasan? 3)
Berat kedelai setelah proses pengeringan ?

2. Mengapa kadar air selalu dinyatakan dalam berat basah? Dan

mengapa komponen padatan selalu dinyatakan dalam berat kering?

3. Jelaskan perbedaan direct distillation dan reflux distillation!

4. Sebutkan dan jelaskan faktor eror pada metode titrasi karl fischer!

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