CHAPTER 3

CHEMICAL ANALYSIS
1. Proximate analysis:
a. Moisture and total solid
b. Ash and mineral
c. Crude fat analysis
d. Protein
e. Carbohydrate
f. Fiber
2. Individual analysis
a. Vitamin analysis
b. Salt
c. pH and titratable acidity
3.1 MOISTURE
 The importance of water
content
A.Quality factor in the preservation of some
products and affects stability in:
i. Dehydrated vegetables and fruits
ii. Dried milks
iii.Powdered eggs
iv.Dehydrated potatoes
v. Spices and herbs
B. For convenience in packaging or shipping
of:
i. Concentrated milks
ii. Liquid cane sugar (67% solids) and
liquid corn sweetener (80% solids)
iii.Dehydrated products (these are
difficult to package if too high in
moisture)
iv.Concentrated fruit juices
 FORM OF WATER IN FOODS
1) Free water – This water retains its physical properties
and thus as the dispersing agent for colloids and the
solvent for salts
2) Adsorbed water – This water is held tightly or is
occluded in cell walls or protoplasm and is held tightly
to proteins
3) Water of hydration – This water is bound chemically,
• For example, lactose monohydrate
• Some salts such Na2SO410H2O.
 Sample preparation
When determining the moisture content of a food, it is
important to prevent any loss or gain of water.
For this reason, exposure of a sample to the
atmosphere, and excessive temperature fluctuations
should be minimized.
When samples are stored in containers, it is common
practice to fill the container to the top to prevent a large
headspace, because this reduces changes in the sample
due to equilibration with its environment.
 Evaporation methods
•Determined by measuring the mass of a food before and after the water is
removed by evaporation:
•The total solids content is a measure of the amount of material remaining
after all the water has been evaporated:

•% Total solids = (100 - % Moisture)

 Drying ovens

Convection oven
Forced draft oven
- Weighed samples are placed in an oven for specified
time and temperature (e.g. 3 hours at 100◦C) and
their dried mass is determined, or they are dried until
they reach constant mass.
Vacuum oven
 Convection oven
The thermal energy used to evaporate the
water is applied directly to the sample via
the shelf and air that surround it.
Temperature variations.
This is because hot air slowly circulates
without the aid of a fan.
 Forced draft oven

Air is circulated by a fan that forces air

movement throughout the oven cavity.
To achieve a more uniform temperature
distribution within the oven.
 Vacuum oven

Weighed samples are placed under reduced pressure

(typically 25-100 mm Hg) in a vacuum oven for a specified
time and temperature and their dried mass is determined.
The boiling point of water is reduced when it is placed
under vacuum.
If the sample is heated at the same temperature, drying
can be carried out much quicker.
Alternatively, lower temperatures can be used to removed
the moisture (e.g. 70◦C instead of 100◦C), and so problems
associated with degradation of heat labile substances can
be reduced.
 Infrared moisture analyzer
•The sample to be analyzed is placed under an
infrared lamp and its mass is recorded as a
function of time. The water molecules in the food
evaporate because they absorb infrared energy,
which causes them to become thermally excited.
Factors influencing the rate and
efficiency of moisture removal
1)Sample dimensions
2)Clumping and surface crust formation
3)Water type
4)Decomposition of other food component
 1. Sample dimensions
•The rate and extent of moisture removal
depends on the size and shape of the sample,
and how finely it is ground. The greater the
surface area of material exposed to the
environment, the faster the rate of moisture
removal.
 2. Clumping and surface crust
formation
•Some samples tend to clump together or form a
semi-permeable surface crust during the drying
procedure. This can lead to erroneous and
irreproducible results because the loss of moisture
is restricted by the clumps or crust
 3. Water type
•The ease of water to remove depends on
its interaction with other component
present.
•Free water is most easily removed from
foods by evaporation.
 4. Decomposition of other
component
•Drying temperature high or drying process too
long, decomposition of carbohydrate to water
occur – it will cause hydrolysis of sucrose to
glucose + fructose; water absorption, therefore
lead to ???
Moisture content (MC) of
foods
3.2 ASH
Ash refers to the inorganic residue remaining
after either ignition or complete oxidation of
organic matter in a foodstuff.
Types of ashing
a) Dry ashing
b) Wet ashing
Importance of Ash analysis
Indicator of nutritional value for some food/ feed
-For exporting goods. E.g: mineral content for bran is 20 times
than in endosperm
Indicator for adulteration of some juices and beverages.
-e.g: distinguishes from fruit vinegar and synthetic vinegar
Index of fruit content jellies and fruit preserves.
- e.g: fruit jellies and marmalade= to estimate fruit content in
product. Lower ash in water soluble fraction indicates extra
fruit added. High ash= low fruit.
Importance of Ash analysis

Ash content represents total mineral in food. Specific

mineral analysis represent specific mineral value.
Part of proximate analysis for nutritional evaluation.
Ashing is the first step in sample preparation for specific
element analysis.
Ash contents in foods
 1. Dry ashing

Refers to the use of a muffle furnace capable of

maintaining temperatures of 500-600◦C
Water and volatiles are vaporized and organic substances
are burned in the presence of oxygen in air to CO2, and
oxides of N2.
Most minerals are converted to oxides, sulfates,
phosphates, chlorides or silicates.
Where Mash refers to the mass of the ashed sample, and
Mdry and Mwet refer to the original masses of the dried
and wet samples.
 Dry ashing continue…
Advantages :
i. Safe. Few reagents are required
ii. Many samples can be analyzed simultaneously
iii. Not labor intensive
iv. Can be analyzed for specific mineral content
 Disadvantages:
i. Long time required (12-24 hours)
ii. Muffle furnaces are quite costly to run due to electrical costs
iii. Loss of volatile mineral at high temperatures, e.g., Cu, Fe, Pb,
Hg, Ni, Zn.
 Crucibles selection
Porcelain
relatively inexpensive to purchase
Can stand to high temperature (<1200◦C)
Easy to clean
Resistant to acids but can be corroded by alkaline
samples
Prone to cracking if they experience rapid
temperature changes
 2. wet/oxidation ashing
Wet ashing is primarily used in the preparation of samples for subsequent
analysis of specific minerals
It breaks down and removes the organic matrix surrounding the minerals so
that they are left in an aqueous solution
A dried ground food sample is usually weighed into a flask containing strong
acids and oxidizing agents(e.g., nitric,perchloric and/or sulfuric acids) and then
heated. Heating is continued until the organic matter is completely digested,
leaving only the mineral oxides in solution
Typically, a digestion takes from 10 minutes to a few hours at temperatures of
about 350◦C. the resulting solution can then be analyzed for specific minerals
 Wet/oxidation ashing
Advantages :
•Little loss of volatile minerals occurs because of the lower
temperatures used
•More rapid than dry ashing
Disadvantages:
•Labor intensive
•Require a special fume-cupboard if perchloric acid is used
because of its hazardous nature
•Low sample throughput
 3. Plasma ashing

Use for preparation of samples when volatile

elemental analysis are determined.
Plasma process is accomplished through the use
of low pressure and radio frequency to induced
gaseous discharge.
Advantages:
i. Minimal chances of trace elements volatilization
compared to classical dry ashing
ii. Equipment of choice for volatile salts analysis
iii. Low temperatures used (<150◦C) allows
microscopic and crystalline structure to remain
unaltered
iv. No toxic chemical employed

 Disadvantages:
i. Small sample capacity
ii. High expense of equipment
 Determination of water
soluble and insoluble ash
It is sometimes useful to determine the ratio of water soluble to

water-insoluble ash as this gives a useful indication of the quality of

certain foods, such as the fruit content of preserves and jellies.
Ash is diluted with distilled water then heated to nearly boiling, and
the resulting solution is filtered.
The amount of soluble ash is determined by drying the filtrate, and
the insoluble ash is determined by rinsing, drying and ashing the filter
paper.
 Insoluble ash in acid
Refer to insoluble mineral contaminant in food
Useful index of soil minerals contaminants such as dirt
and sand. E.g: surface contaminant of fruit and vegetable,
wheat washing prior to milling and rice coating
Contaminants generally silicates that remain insoluble in
acid
High insoluble ash in acid indicates high contaminants
 Alkalinity of ash
•To determine acid-base balance of food
•To detect adulteration of food with minerals and also as
index of fruit and fruit juices.
•Ash from fruits and vegetables (Ca, Mg, K, Na)
•Ash from meat and some cereals is acid (P, S, Cl)
SUMMARY