Determination of Ash

B.K.K.K.Jinadasa

(GS/M.Sc./FOOD/3608/08)
 Determination of Ash 2

Introduction

Ash is the inorganic residue remaining after the water and organic matter have been removed by
heating in the presence of oxidizing agents, which provides a measure of the total amount of
minerals within a food. Analytical techniques for providing information about the total mineral
content are based on the fact that the minerals (the “analyte”) can be distinguished from all the
other components (the “matrix”) within a food in some measurable way. 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. Ash contents of fresh foods rarely exceed 5%,
although some processed foods can have ash contents as high as 12%, e.g., dried beef.

There are 3 main types of ashing procedures:

Dry ashing

– Use of a muffle furnace capable of maintaining 500-600°C.

– Water and volatiles are vaporized and organic compounds are oxidized via O2 in
air into CO2, CO, and N-oxides.
– Most minerals are converted to oxide, sulfates, phosphates, chlorides and silicates.
– Some minerals are volatile (Fe, Se, Pb, Hg) and dry ashing would not be used as
sample pretreatment for analysis of these elements.

Wet ashing

– Use acids alone or in combination with other oxidizing agents.

– Nitric, hydrochloric, or perchloric acid is used.
– Perchloric acid requires use of a special hood

Low – temp – plasma (oxidation reactions, not very common)

– Use of a special device for ashing that uses a vacuum and an electromagnetic
field.
– The oxygen from the air oxidizes sample heated in the electromagnetic field.
– Since the temperature is lower than a muffle furnace, volatilization is much lower.

What are the really in ashes?

• Calcium (most all foods except sugar, starch or oil)

• Phosphorus (dairy, grains, nuts, meats, poultry products)
• Iron (enriched foods, grains, nuts; meats, eggs, legumes)
• Sodium (primarily from added salt)
• Potassium (dairy products, F&V, cereals, nuts, meats)
• Magnesium (nuts, cereals, legumes)
 Determination of Ash 3

• Manganese (cereals, F&V, meats)

• Copper (sea foods, liver, cereals, vegetables)
• Zinc (sea foods)

Acid insoluble ash:

Refers to ash that is insoluble in acids. This is usually silicates primarily from soil, and generally
not tested for in foods.

Sample preparation is extremely important because of the small (2-3g) sample sizes used
(error rates higher).

It is important to use very pure water if further analysis is expected (specific elemental analysis).

High lipid samples should be pretreated (usually by drying) due to spattering or foaming.

Use furnace capable of maintaining 500-600 °C

Careful crucible selection (composition)

Careful crucible handling

Several types of crucibles are used for determine Ash.

QUARTZ crucibles are resistant to acids and halogens at high temperatures but not alkali.

Vycor (brand name) are stable to 900 °C.

Pyrex (brand name) is stable to 500 °C.

Porcelain crucibles are heat stable but readily crack, however, since they are cheap they are
commonly used.

Steel crucibles are resistant and stable but are a possible source of contamination of iron,
chromium, and possibly other metals.

Platinum crucibles are very inert but so expensive ($500-3,000 each).

 Determination of Ash 4

When analyzing ash, should be consider several factors.

ü High fat samples can be solvent extracted to remove fat

ü High moisture samples can be pre-dried first
ü Alcohol, magnesium acetate, and glycerol may speed ashing
ü Spattering can be controlled with lids on the crucibles
ü Wet ashing is often used as prep for mineral analysis
ü Minerals stay in solution, temps are lower, lower volatilization
ü Hot nitric acid mixed with peroxide is a good combination
ü Perchloric acid is a difficult acid to work with, requires special hoods that have no
metal, plastic, or glycerol caulking (can explode when perchloric derivatives are
formed)
ü Hood wash downs are conducted often, to prevent corrosion
 Determination of Ash 5

Materials

Muffle furnace

Platinum or silica dishes

Weighing balance

Desiccator

Tongs

Glows (thermal)

Procedure

5g of sample (black tea) was weighed into a clean dry pre weighed silica dish.

Then the sample was ignited slowly over a Bunsen flame in a fume cupboard until no more
fumes are evolved.

Then the dish was transferred to muffle furnace and incinerated until it was free of black carbon
particles and turn into white in colour. (About three hours)

Dish was removed carefully and cooled in a desiccator. Weight was taken after cooling. Process
of ashing, cooling and weighing was repeated till no further loss in weight was indicated.

This process was done to three samples of black tea (5g each)

To get the dry weight of the sample another sample (2 g each) were weighed into pre weighed
stainless steel dish and kept in oven at 105°C for three hours. Then the samples were cooled and
weighed. Process of drying was repeated until a constant weight was obtained.
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Results and calculation

Petri dish Sample Weight of Sample weight Moisture

weight weight sample + dish after drying Content
40.6857 2.0387 42.7244 42.5829 6.9407
46.3192 2.0134 48.3326 48.1885 7.1570
39.0021 2.1797 41.1818 41.0263 7.1340

Average Moisture Content = 7.0773 %

Wt of Wt of Dry wt. of Wt of crucible + Wt of ash Ash%

crucible (g) sample (g) sample (g) sample after after
incineration (g) incineration(g)
40.6857 5.0968 4.7430 41.0644 0.3787 7.9844
46.3192 5.0335 4.6732 46.6587 0.3395 7.2648
39.0021 5.4493 5.0636 39.3819 0.3798 7.4996

Average ash content = 7.5829 %

 Determination of Ash 7

5.2 Determination of Acid Insoluble Ash

This is the HCl acid insoluble fraction of ash expressed as a percentage of the total ash.

Materials

Steam bath

Dil. HCL acid (10M and 2M)

Litmus paper

Desiccator

Muffle furnace

Ash less filter paper

Procedure

Ash content which was obtained from the above practical was taken in separately and 25mL of
10% HCL was added to it separately. Then it was heated 5 min on a steam bath and heated for 10
minutes.

Sample was filtered through an ash less filter paper and washed with hot water and cold water
until the washings are free from acid.

The filter paper containing the ash was carefully folded and placed in the porcelain dish and
ignited in the muffle furnace, cooled and weighed until a constant weight is obtained.

Results and Calculation

 Determination of Ash 8

Weight of dish + Acid Weight of dish (g) Weight of Ash (g) % of Acid
Insoluble Ash (g)------------- Insoluble Ash
--------(1) ----------(2) ---------------(2-1)
40.7215 40.6857 0.0358 0.7548
46.3550 46.3192 0.0358 0.7661
39.0425 39.0021 0.0404 0.7979

Average amount of acid Insoluble Ash = 0.7548 + 0.7661 + 0.7979

03

= 0.7729 g

Discussion

In the determination of Acid Insoluble Ash, care must be taken to prevent splitting of the content
when boiling the residues with solvent and during filtering.

Platinum dishes are used because they are stable at high temperature and can be cleaned easily
with dilute HCl acid.

Ashing over an open flame requires constant attention. So the initial stage of ashing must be
done by open flame.

A prolonged ashing fails to give carbon free ash the residue should be moistened, dried and
reheated until a white gray ash remains.

Dry ashing is the most satisfactory method if no loss occurs at temperatures up to about 500Co.
 Determination of Ash 9

References:

Fennema, Owen. R., 1996.Food chemistry, 3rd Ed, Marcel Dekker, Inc. New York.

http://www.css.cornell.edu/compost/calc/moisture_content.html