ASH ANALYSIS

Introduction

Ash:
Refer to inorganic residue remaining after either
ignition or complete oxidation of organic matter in
foodstuff
Estimate the total mineral content in foods
minerals are not destroyed by heating, and they
have a low volatility
Ash content of most fresh foods rarely > 5%, but
processed food (e.g.: dried beef = 12%)
Pure oils & fats contain no ash / little

Importance of Ash

Nutritional labeling concentration and type of

mineral normally stipulated on the label
Quality depends on the concentration and type of
mineral esp. appearance, texture, taste or stability
Microbiological stability- high mineral content may
retard the growth of certain microorganisms
Nutrition essential to healthy diets (Ca, K, P, Na)
but some toxic (lead, aluminum, mercury)
Processing- will effect the physicochemical
properties of food

3 major types of ashing method:

Dry ashing
muffle furnace, 500 600oC/24 h
Wet ashing
as a preparation for the analysis of certain
minerals.
Low-temperature plasma dry ashing
by nascent oxygen in a partial vacuum

Sample Preparation For

Ashing
Particle size reduction (milling, grinding),
representative
Avoid micro-elemental contamination (water,
glass, metal)
- use acid wash, deionized water
Pre-treatment to prevent sample loss:

Drying or fat extraction

- For liquids (high in moisture), high fat or sugar
content samples

Dry Ashing

Principle: incineration of sample at high temp. (500

600oC)/ 24 h, in a muffle furnace
Water & volatiles are vaporized
Organic substances are burned in the presence of
O2 in air to CO2, H2O of N2 (gas )
Most mineral are converted to oxides, sulfates,
phosphates, chlorides, and silicates
Cu, Fe, Se, Pb, Hg, Ni, Zn may partially volatilize
with this procedure need to use lower temperature
ashing method

Dry Ashing Cont. Crucible

Selection

Selection of crucible highly depends on sample and

furnace temperature
Quartz : resistant to acids & halogen, but not alkali at high
temperature
Porcelain: crack with rapid temperature changes,
inexpensive
- usually the crucible of choice
Steel: resistant to acids & alkalis, inexpensive, but may be
a source of contaminants (Ni & Cr)
Platinum: very inert, too expensive for routine use for large
number of sample
All crucibles should be labeled for identification

Type of crucible for dry

ashing

Advantages of Dry Ashing

Safe method, no added reagents or blank
subtraction
Little attention is needed once ignition
begins
Can handle a large number of crucibles at
one time
Resultant ash can be used for:

Analysis of individual elements

Acid insoluble ash
Water-soluble & insoluble ash

Disadvantages of Dry Ashing

Time consuming (12 18 hr, overnight)
Expensive equipment electrical cost
Lost of volatile elements: As, B, Cd, Cr, Cu,
Fe, Pb, Hg, Ni, P, V and Zn
May have interaction between crucibles and
elements

Procedure
5 10 g sample (pre-dry if very moist)
Place in muffle furnace
Ignite 12 18 hr (or overnight), 550oC
Open door carefully
to avoid ash that
may be fluffy

Turn off, wait until temp drop to <250oC

Quickly transfer crucibles to desiccator

Ash content calculated as,

% ash (dry basis)

= wt after ashing(g) - wt of empty crucible (g) x 100

dry matter (g)

Special Application

Completely oxidized sample: white in colour

If C persists, add several drops of H2O or HNO3, then re-ash

If C still present such as in high sugar sample;

1) suspend the ash in water

2) filter through ashless filter paper
3) dry the filtrate
4) place paper & dried filtrate in muffle

High fat sample: extract or burn off the fat

Prevent spattering (jam/jellies): mixed sample with cotton
wool
Glycerin, alcohol & hydrogen accelerate ashing
Cereals: a solution of magnesium acetate as can accelerate
ashing, use a blank

Question:
A grain was found to contain 11.5%
moisture. A 5.2146 g sample was placed into
a crucible (28.5053 g tare). The ashed
crucible weighed 28.5939 g. Calculate the
percentage ash on:
a) an as-received basis (wet basis)
b) a dry-matter basis

Wet Ashing
Sometimes called wet oxidation or wet digestion
Principle: oxidizing organic substances by using
strong and oxidizing agents acids (nitric, perchloric,
sulfuric acid) or their combinations, then heating.
Use to prepare for specific mineral analysis
Advantages:

Mineral stay in aqueous solution, little or no loss from

volatilization because of the lower temp. (350C)
Time used is shorter than dry ashing (10 min to few
hours)

Wet Ashing

Disadvantages:
Need constant operator attention
Use corrosive reagent (HNO3, HClO4 & H2SO4)
A special perchloric acid hood is required
Only small numbers of samples at a time
Single acid does not give complete & rapid
oxidation, need to combine with H2SO4 or HClO4
diff. combination for diff .samples
Very hazardous
Do not determine the total ash content

Procedure
1 g sample
+ 10 ml HNO3, (overnight for high fat content)
+ 3 ml 60% HClO4, heat to 350oC
Sample turn from black to clear when complete digest. Let cool.
+ 10 ml 50% HCl
Make-up to 50 ml with deionized water

Low-Temperature Plasma
Ashing- The principle
Dry ashing in a partial vacuum with nascent
oxygen
Ashing temperature is much lower than
furnace (150oC)
Glass ashing system consist of chambers,
glass boat for holding samples & vacuum
pump
Once a vacuum is satisfactory, a small flow
of oxygen or air is introduced by
electromagnetic field generator (<14MHz)

Low-Temp Plasma Ashing

Advantages:
Prevent loss of volatile or trace elements
Low temp allows the microscopic & crystalline
structure to remain unaltered

Disadvantages:
Small sample capacity
Expensive equipment
May be the equipment of choice under certain
circumstances, especially for volatile salts

Microwave Ashing
A system for dry & wet ashing
Working with open or closed vessels for ashing
a variety of samples
Advantages : reduce time of ashing greatly, 40
min = 4 h time ashing with a conventional muffle
furnace
Wet ashing in a closed system is rapid & safe
Disadvantages : Not possible to analyze as
many sample as in a muffle furnace

Other Ash Measurements

Soluble & Insoluble Ash in Water

As an index of the fruit content of preserves &
jellies
A lower ash in the water-soluble fraction is an
indicator that extra fruit is added
Weigh the total ash add 10 ml DI water
cover & heat to boiling filter & rinse with hot
DI water dry & re-ash filter paper at least 30
min weigh & calculate as % water insoluble
ash.

Other Ash Measurement..

Ash Insoluble in Acid

Determination of the surface contamination
(silicates) of fruits & vegetables, wheat & rice
coatings
Silicates remain insoluble in acid
Weigh total ash add 25 ml 10% HCl cover
& boil filter with hot distilled water dry & reash weigh & calculate as %

Other Ash Measurements..

Alkalinity of ash
Alkaline ash: Ca, Mg, K, Na (fruits & veg.)
Acid ash: P, S, Cl (meat, some cereals)
The alkalinity of ash has been used as a quality
index of fruit & fruit juices
Total ash add 0.1 N HCl add boiling water
if necessary & warm on a water bath cool
titrate the excess HCl with 0.1N NaOH (methyl
orange as indicator) express as ml of 1N
acid / 100 g sample.