Determination of Ash and Minerals Determination of Ash and Minerals

Ash
It refers to the inorganic residue remaining after
o The “ash content” is a measure of the total amount either ignition or complete oxidation of organic matter
of minerals present within a food in a foodstuff
 Types of ashing
Two main types of ashing are used
o The “mineral content” is a measure of the amount
1. Dry Ashing
of specific inorganic components present within a
o It refers to the use of a muffle furnace capable of
food, such as Ca, Na, K and Cl 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
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Ash Content in foods

Importance of Ash in Food Analysis
Sr. Food item Ash content
 Ash content represents the total mineral content No. (%)
in the food 01 Most fresh foods 5%
02 Pure oils and fats No ash
 Determining ash content may be important for 03 Dairy products 0.5-5.1%
several reasons
04 Dried fruits 2.4-3.5%
It is a part of the proximate analysis for
nutritional evaluation 05 Flours and meals 0.2-0.6%
Ashing is a first step in the preparation of a 06 Pure starch 0.3%
food sample for specific elemental analysis 07 Wheat germ 4.3%
08 Nuts and nut products 0.8-3.4%
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09 Meat, poultry and seafoods 0.7-1.3
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 1. Dry Ashing
Determination of Ash and Minerals…
Methods of ash determination
Principle
 The most widely used methods are based on the
fact that minerals are not destroyed by heating, and  Dry ashing procedures use a high temperature
that they have a low volatility compared to other muffle furnace capable of maintaining
food components
temperatures of between 500 and 600 ºC
 The methods used for determination of ash content:
1.Dry ashing
2.Wet ashing  Water and other volatile materials are
3.Low temperature plasma dry ashing vaporized and organic substances are burned
4.Instrumental analysis in the presence of the oxygen in air to CO2,
5.Microwave ashing H2O and N2
 There are a number of different types of crucible available for ashing
food samples, including quartz, Pyrex, porcelain, steel and platinum
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1. Dry Ashing… 1. Dry Ashing…

 After ashing most minerals are converted to Advantages and disadvantages of dry ashing
1. Oxides Advantages
2. Sulfates 1. Safe
3. Phosphates 2. Only few reagents are required
4. Chlorides 3. Many samples can be analyzed simultaneously
5. Silicates 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
MASH=Mass of the ashed sample
costs
MDRY=Original mass of the dried sample
MASH=Refer to the original masses of the dried and wet 3. Loss of volatile minerals at high temperatures, e.g., Cu,
samples Fe, Pb, Hg, Ni, Zn
AOAC
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1. Dry Ashing… 2.Wet Ashing

Weighed Dried ground food sample

 Recently, analytical instruments have been
developed to dry ash samples based on
microwave heating HNO3 and HCLO4

 The major disadvantage is that it is not
possible to simultaneously analyze as many
samples as in a muffle furnace
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Heated 350 C 0 for 10 min to few hrs
The resulting solution can then be
analyzed for specific minerals
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2. Wet Ashing… 2. Wet Ashing…

Steps involved in wet ashing Advantages and disadvantages of wet ashing
Advantages
1. A dried ground food sample is usually weighed into  Little loss of volatile minerals occurs because of the
a flask containing strong acids and oxidizing agents lower temperatures used
(e.g., nitric, perchloric and/or sulfuric acids) and then
 More rapid than dry ashing
heated
2. The temperature and time used depends on the
type of acids and oxidizing agents used. Disadvantages
3. Typically, a digestion takes from 10 minutes to a few  Labor intensive
hours at temperatures of about 350ºC  Requires a special fume-cupboard if perchloric acid
4. The resulting solution can then be analyzed for is used because of its hazardous nature
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 Low sample throughput
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3. Low Temperature Plasma Ashing 3. Low Temperature Plasma Ashing…

Principle Advantages and disadvantages

 A sample is placed into a glass chamber which is
evacuated using a vacuum pump.
 Advantages
 Application of an electromagnetic radio frequency
field Less chance of losing trace elements by
The organic matter in the sample is rapidly
volatilization
oxidized at elevated temperatures
 The relatively cool temperatures (< 150ºC) used in  Disadvantages
low-temperature plasma ashing cause less loss of Relatively expensive equipment and small
volatile minerals than other methods sample through put

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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

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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
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Determination of Specific Mineral
Content
1. Gravimetric Analysis
 Knowledge of the concentration and type of
specific minerals present in food products is often
important in the food industry 2. Colorimetric methods
 Many more traditional methods can be found in the
AOAC Official Methods of Analysis
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3. Atomic Absorption Spectroscopy
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
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The Methods of Determination of
Minerals
Sample + reagent (Filtration, Drying & weighed) the
amount of mineral in formula of PPT e.g. Chlorine +
excess silver ion = silver chloride precipitate
 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
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 Atomic Absorption Spectroscopy Atomic Absorption Spectroscopy…
Dissolved in
 Atomic absorption spectroscopy (AAS) is an analytical aqueous solution
method that is based on the absorption of UV-visible Put in instrument
Food sample Ash
and heated
radiation by free atoms in the gaseous state
 The food sample to be analyzed is normally ashed and
then dissolved in an aqueous solution Vaporize
 This solution is placed in the instrument where it is heated
to vaporize and atomize the minerals Atomizer

 A beam of radiation is passed through the atomized

sample, and the absorption of radiation is measured at Beam radiation Atomized mineral
specific wavelengths corresponding to the mineral of interest
Detector
 Information about the type and concentration of minerals
present is obtained by measuring the location and The absorption of radiation is measured at
intensity of the peaks in the absorption spectra specific wavelengths corresponding to the
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