ASH

The students will be able to:

■ Define ash and examples of ash.
■ State various methods for ash
determinations
■ Describe the principles for ash
determinations.
■ Analyse and evaluate the compositions of
food products.
■ To calculate the ash content in food
 Definition

ASH

Inorganic residue remaining after ignition or

complete oxidation of organic matter in a
foodstuff.
Three major types of ashing:

■ Dry ashing – majority samples

■ Wet ashing/oxidation – high fat samples;

preparation step for elemental analysis.

■ Plasma ashing – preparation for volatile

elemental analysis
 Importance of Ash Analysis
■ Indicator of nutritional value for some food/feeds
especially for exporting goods.
Eg: Mineral content for bran 20 times than in endosperm,
indicates thoroughness separation of bran and germ from
wheat kernel.

■ Indicator for adulteration of some juices and beverages.

Eg: Able to distinguishes fruit vinegar from synthetic
vinegar.

■ Index of fruit content for jellies and fruit preserves.

Eg: In fruit jellies and marmalades, ash content used to
estimate fruit content in product.
■ Ash content represents total mineral in
foods.

■ Part of proximate analysis for nutritional

evaluation.

■ Ashing is the first step in sample preparation

for specific elemental analysis.
Minerals composed ash are:
i) Calcium- high concentration in most dairy and dairy
containing products, cereals, nut, egg, fish and
certain vegetables.

ii) Phosphorus- dairy products, grains, nut, meat, fish,

poultry, eggs and legumes.

iii) Iron- grains and grain products, eggs, legumes,

seafood, poultry.
iv) Sodium- poultry, meat, fruits, cereals,
fish, egg and others.

v) magnesium- nut, cereal and legumes.

vi) sulfur- in protein rich foods and

vegetables.
Others are potassium, zinc, copper, cobalt.
 Ash Contents in Foods

Food % Ash
Milk and dairy products 0.5 – 5.1
Meat, poultry and fish 0.8 – 3.0
Fruits and vegetables 0.3 – 2.3
Cereals 0.4 – 1.7
Fats and oils 0.0 – 4.0
Nuts 0.8 – 3.4
 Sample Preparation
i) Most dry samples (eg. whole grain, cereals, dried
vegetables) does not require preparation.

ii) Fresh vegetables need to be dried prior to ashing.

Plant materials pre-dried first then ground. If
moisture <15% prior drying is not required. Fresh
stem and leaf tissue should be dried in 2 stages :
• at low T of 55oC then
• at higher T to prevent artifact lignin.
 continue…
iii) High fat products, syrups and spices require
treatments prior to ashing, where samples need to
be dried on a steam bath and fat extracted before
ashing. This is because high fat and moisture may
cause spattering, swelling or foaming that may
result in sample loss. Therefore cause
underestimation of ash content.

iv) Solid foods must be finely ground but may add

mineral contents from the grinders steel
construction. Not suitable in analysis of specific
mineral analysis.
 Crucible Selection
■ Quartz : resistant to acids and halogens but not alkali
at high temperatures.
■ Vycor brand glass : stable up to 900oC, resistant to
most chemicals and acid except bases.
■ Porcelain : resemble quartz properties. Usual choice,
withstand 1200oC, easy to clean, cheap, susceptible to
alkali, but will crack with rapid T changes. Relatively
inexpensive.
■ Steel : resistant to both acids and alkali, inexpensive,
but possible sources of contamination (composed of
chromium and nickel).
■ Platinum : very inert, the best crucibles but very
expensive for routine use. Recommended procedures
of AOAC, for cereal, dairy, meat and fish products.
 Porcelain Steel Platinum

Opaque quartz Quartz Vycor

 DRY ASHING
■ Principle
■ Incineration at high temperatures (500oC or higher)
■ water and volatile materials are vaporized and organic
substances burned in presence of O2 in air, producing
CO2, H2O and N2.
■ Most minerals converted to oxides, sulfates, phosphate,
chloride and silicates.
■ Crucibles are pre-dried and weighed before ashing and
cooled to room temperature after ashing before
weighing.
■ % Ash (wet basis) = M ash x 100
M wet
 Advantages
■ Safe method.
■ Most common procedure to determine total mineral
content of foods.
■ Requires no reagents.
■ Resultant ash can be used for other analyses e.g.
water-soluble, water-insoluble, and acid-insoluble
ash.
■ Applicable also in determination of most common
metals.
■ Requires little attention and simple.
■ Large numbers of samples can be handled at once.
■ No blank subtraction required.
 Disadvantages

■ Time consuming (12-18hrs or overnight).

■ Loss of volatile minerals at high
temperatures (e.g. Cu, Fe, Pb, Hg, Ni, Zn,
As, Cd, Cr).
■ Interaction between mineral components
and crucibles.
 II. Wet Ashing / Oxidation
■ Use for samples with high fat content (meats and
meat products), for determining trace elements and
metallic poisons.
■ Procedure involves oxidizing organic substances
using acids and oxidizing agents (eg nitric acid with
either perchloric and/or sulfuric acids) and heated
to about 350oC.
■ Minerals are solubilized without volatilization.
■ Rapid decomposition of many organic compounds
that difficult to oxidize.
■ Adding salt (e.g. potassium sulfate) raises the
boiling point of the acid and accelerates
decomposition.
 Principle
■ Oxidation of organic substances by strong acid,
nitric acid (HNO3) and oxidizing agents perchloric
acid (HCIO4).
■ Heat slowly up to 350oC until organic matter
completely digested and HNO3 evaporated.
■ Boiling continues until sample becomes colourless
or light in colour.
■ Cool, add HCl then dilute with distilled deionized
water. Pre-dry sample then incinerate at 525oC for
1-2hrs.
 Advantages

■ Use low temperature therefore little

or no loss from volatilization.
■ Short oxidation time.
 Disadvantages
■ Very hazardous. Requires a hood, hot plate, long tongs,
and safety equipment.
■ Require large amounts of corrosive reagents and correction
for reagents.
■ Small numbers of samples can be handled at one time.
■ Need constant operator's attention.
■ Single acid does not give complete and rapid oxidation of
organic compounds. Nitric acid with sulfuric or perchloric
acids and potassium chlorate or sulfate are used in varying
combination.
■ Special perchloric acid hood required (with wash-down
capabilities to protect from explosion).
 III. Plasma Ashing

■ Use for preparation of samples when volatile

elemental analyses are determined.
■ Plasma process is accomplished through the
use of low pressure and radio frequency to
induced gaseous discharge.
 Principle
■ A sample is placed into a glass chamber which is
evacuated using a vacuum pump
■ A small amount of oxygen is pumped into the
chamber and broken down to nascent oxygen by
application of an electromagnetic radio frequency
field
■ The organic matter in the sample is rapidly
oxidized by the nascent oxygen and the moisture is
evaporated because of the elevated temperatures
 Advantages & Disadvantages

■ Minimal chances of trace ■ Small sample capacity.

elements volatilization ■ High expense of the
compared to classical dry
equipment
ashing
■ Equipment of choice for
volatile salts analysis.
■ Low temperatures used
(<150oC) allows
microscopic and crystalline
structures to remain
unaltered.
■ No toxic chemicals
employed.
 IV. Soluble & Insoluble Ash in
Water

■ These measurements are an index of the

fruit content of preserves and jellies. A lower
ash in the water-soluble fraction is an
indication that extra fruit is added to fruit and
sugar products.
 Procedure

Weigh total ash obtained and add the water

Heat near to boiling, filter on ashless filter paper

Rinse with hot water several times.

Dry and re-ash filter paper for 30mins.

Weigh and calculate as % H2O-insoluble ash.

Calculate soluble ash by subtracting insoluble ash from total

ash or dry the filtrate, re-ash and weigh
 V. Ash Insoluble in Acid
■ Measure surface contamination of fruits and
vegetables, wheat and rice coatings such as dirt or
sand. E.g. surface contamination of fruits and
vegetables, wheat washing prior to milling and rice
coatings. These contaminants are silicates that
remain insoluble in acid.
Procedure:
■ Add HCl 10% to total ash or H2O-insoluble ash.

■ Boil for 5mins then filter on ashless filter paper

and wash several times with hot water

■ Re-ash filter paper and residue for 30mins.

■ Weigh and calculate as a percentage (%).

 Alkalinity of Ash
■ Useful measurement to determine the
acid-base balance of foods and quality index
of fruits and fruit juices.

■ Ash from fruits and vegetables is alkaline

(Ca, Mg, K, Na).

■ Ash from meat and some cereals is acid (P,

S, Cl).
 Procedures:
■ Place ash (total or H2O-insoluble ash) in
platinum dish.

■ Add 0.1N HCl and warm on a steam bath.

■ Cool and transfer to Erlenmeyer flask.

■ Titrate the excess HCl with 0.1N NaOH

using methyl orange as indicator.
 Summary
■ Ashing conducted by any one of 3 methodologies - dry
ashing, wet ashing/oxidation and plasma ashing.
■ Dry ashing based on incineration at high temperature in
muffle furnace.
■ Wet ashing uses corrosive reagents that require constants
operator's attention.
■ Dry ashing result in lost of volatile elements. Wet ashing
and plasma ashing cause minimal volatilization.
■ Wet ashing and low temperature plasma ashing are
expensive; require operator time and limited to small
number of samples.
■ 3 post-ashing procedures (soluble and insoluble ash in
water, ash insoluble in acid and ash alkalinity) are special
measurements for certain foods.