Lec-5 Ash

Determination of Ash and Minerals
o The “ash content” is a measure of the total amount

of minerals present within a food
o The “mineral content” is a measure of the amount

of specific inorganic components present within a
food, such as Ca, Na, K and Cl
Determination of Ash and Minerals
Ash
It refers to the inorganic residue remaining after
either ignition or complete oxidation of organic matter
in a foodstuff
 Types of ashing
Two main types of ashing are used
1. Dry Ashing
o It refers to the use of a muffle furnace capable of
maintaining temperatures of 500-600 oC
o Primarily used for proximate composition and some types of
specific mineral analysis
2. Wet Ashing
o It is a procedure for oxidizing organic substances by using
acids and oxidizing agents or their combinations minerals
are solubilized without vlatilization
Importance of Ash in Food Analysis
 Ash content represents the total mineral content
in the food
 Determining ash content may be important for

several reasons
It is a part of the proximate analysis for
nutritional evaluation
Ashing is a first step in the preparation of a
food sample for specific elemental analysis
Ash Content in foods
Sr. Food item Ash content
No. (%)
01 Most fresh foods 5%
02 Pure oils and fats No ash
03 Dairy products 0.5-5.1%
04 Dried fruits 2.4-3.5%
05 Flours and meals 0.2-0.6%
06 Pure starch 0.3%
07 Wheat germ 4.3%
08 Nuts and nut products 0.8-3.4%
09 Meat, poultry and seafoods 0.7-1.3
Determination of Ash and Minerals…
Methods of ash determination
 The most widely used methods are based on the
fact that minerals are not destroyed by heating, and
that they have a low volatility compared to other
food components
 The methods used for determination of ash content:
1.Dry ashing
2.Wet ashing
3.Low temperature plasma dry ashing
4.Instrumental analysis
5.Microwave ashing
1. Dry Ashing
Principle
 Dry ashing procedures use a high temperature

muffle furnace capable of maintaining
temperatures of between 500 and 600 ºC
 Water and other volatile materials are

vaporized and organic substances are burned
in the presence of the oxygen in air to CO 2, H2O
and N2
 There are a number of different types of crucible available for ashing food
samples, including quartz, Pyrex, porcelain, steel and platinum
1. Dry Ashing…
 After ashing most minerals are converted to
1. Oxides
2. Sulfates
3. Phosphates
4. Chlorides
5. Silicates
MASH=Mass of the ashed sample

MDRY=Original mass of the dried sample
MASH=Refer to the original masses of the dried and wet
samples
AOAC Official Methods of
Analysis
1. Dry Ashing…
Advantages and disadvantages of dry ashing
Advantages
1. Safe
2. Only few reagents are required
3. Many samples can be analyzed simultaneously
4. Not labor intensive
5. Ash can be analyzed for specific mineral content
Disadvantages
1. Long time required (12-24 hours)
2. Muffle furnaces are quite costly to run due to electrical
costs
3. Loss of volatile minerals at high temperatures, e.g., Cu,
Fe, Pb, Hg, Ni, Zn
1. Dry Ashing…
 Recently, analytical instruments have been

developed to dry ash samples based on
microwave heating
 The major disadvantage is that it is not

possible to simultaneously analyze as many
samples as in a muffle furnace
2.Wet Ashing
Weighed Dried ground food sample
HNO3 and HCLO4
Heated 350 C 0 for 10 min to few hrs
The resulting solution can then be

analyzed for specific minerals
2. Wet Ashing…
Steps involved in wet ashing
1. 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
2. The temperature and time used depends on the
type of acids and oxidizing agents used.
3. Typically, a digestion takes from 10 minutes to a few
hours at temperatures of about 350ºC
4. The resulting solution can then be analyzed for
specific minerals
2. Wet Ashing…
Advantages and disadvantages of wet ashing

Advantages
 Little loss of volatile minerals occurs because of the
lower temperatures used
 More rapid than dry ashing
Disadvantages
 Labor intensive
 Requires a special fume-cupboard if perchloric acid
is used because of its hazardous nature
 Low sample throughput
3. Low Temperature Plasma Ashing
Principle
 A sample is placed into a glass chamber which is
evacuated using a vacuum pump.
 Application of an electromagnetic radio frequency
field
The organic matter in the sample is rapidly
oxidized at elevated temperatures
 The relatively cool temperatures (< 150ºC) used in
low-temperature plasma ashing cause less loss of
volatile minerals than other methods
3. Low Temperature Plasma Ashing…
Advantages and disadvantages
 Advantages
Less chance of losing trace elements by
volatilization
 Disadvantages
Relatively expensive equipment and small
sample through put
4. Microwave Ashing
 Both wet and dry ashing can be done using

microwave instrumentation, rather than the
conventional dry ashing in a muffle furnace and wet
ashing in a flask or beaker on a hot plate
 It will reduce the sample time
 Wide spread use of microwave ashing
4. Microwave Ashing…
a. Microwave Wet Ashing
 May be performed safely in either an open or

closed vessel microwave system
 Choice of system depends on amount of sample
and temperature required to digest it
 Close vessel microwave digestion system can
process up to 14 samples at a time
 Digestion normally takes less than 30 min
4. Microwave Ashing…
b. Microwave Dry Ashing
 Microwave muffle furnace can ash sample in

minutes, decreasing analysis time by as much as
97%
 Temperature may reach up to 1200 oC
 It will also equipped with exhaust system that
circulate the air in the cavity to help decrease ashing
time
 Microwave furnace do not require fume hood space
Other Ash Measurements
1. Soluble and insoluble ash
(e.g., AOAC Method 900.02)-applied for fruits
2. Ash insoluble in acid
A measure of the surface contamination of a fruits and
vegetables and wheat and rice coatings; contaminants
are generally silicates and remain insoluble in acid
3. Sulfate ash
 The sulfated ash test utilizes a procedure to measure the amount of residual substance
not volatilized from a sample when the sample is ignited in the presence of sulfuric acid.
The test is usually used for determining the content of inorganic impurities in an organic
substance. -applied to sugars, oils, syrups, and color additives
4. Alkalinity of Ash
(e.g., AOAC Method 900.02, 940.26)-Ash of fruits and vegetables
is alkaline; ash of meats and some cereals is acid
Determination of Specific Mineral
Content
 Knowledge of the concentration and type of

specific minerals present in food products is often
important in the food industry
 Many more traditional methods can be found in the

AOAC Official Methods of Analysis
The Methods of Determination of
Minerals
1. Gravimetric Analysis
Sample + reagent (Filtration, Drying & weighed) the
amount of mineral in formula of PPT e.g. Chlorine +
excess silver ion = silver chloride precipitate
2. Colorimetric methods
 Sample + colored reagent give change in color reagent
when react with mineral and determined it by
spectrophotometer
 For example Phosphorous by vandate-molybdate
reagent give yellow-orange at 420 nm and comparing
with standard curve
3. Atomic Absorption Spectroscopy
Atomic Absorption Spectroscopy
 Atomic absorption spectroscopy (AAS) is an analytical
method that is based on the absorption of UV-visible
radiation by free atoms in the gaseous state
 The food sample to be analyzed is normally ashed and
then dissolved in an aqueous solution
 This solution is placed in the instrument where it is heated
to vaporize and atomize the minerals
 A beam of radiation is passed through the atomized
sample, and the absorption of radiation is measured at
specific wavelengths corresponding to the mineral of interest
 Information about the type and concentration of minerals
present is obtained by measuring the location and
intensity of the peaks in the absorption spectra
Atomic Absorption Spectroscopy…
Dissolved in
aqueous solution
Put in instrument
Food sample Ash
and heated
Vaporize
Atomizer
Beam radiation Atomized mineral
Detector
The absorption of radiation is measured at

specific wavelengths corresponding to the
mineral of interest.

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Determination of Ash and Minerals

o The “ash content” is a measure of the total amount

o The “mineral content” is a measure of the amount

 Determining ash content may be important for

 Dry ashing procedures use a high temperature

 Water and other volatile materials are

MASH=Mass of the ashed sample

 Recently, analytical instruments have been

 The major disadvantage is that it is not

Weighed Dried ground food sample

HNO3 and HCLO4

Heated 350 C 0 for 10 min to few hrs

The resulting solution can then be

1. A dried ground food sample is usually weighed into

Advantages and disadvantages of wet ashing

Advantages and disadvantages

 Both wet and dry ashing can be done using

a. Microwave Wet Ashing

 May be performed safely in either an open or

 Microwave muffle furnace can ash sample in

 Knowledge of the concentration and type of

 Many more traditional methods can be found in the

Beam radiation Atomized mineral

The absorption of radiation is measured at

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