Introduction
y Ash: total mineral content; inorganic residue remaining
Total ash analysis
Assoc. Prof. PHAM VAN HUNG, PhD
Ash Contents in Foods
Wheat flour, whole grain
Macaroni, dry, enriched
Milk, whole, fluid
Butter, with salt
Apple, raw with skin
Banana, raw
Egg, whole, raw
Hamburger, regular, plain
after ignition or complete oxidation of organic matter
y Minerals:
{ Macro minerals (>100 mg/day)
Ù C P
Ca, P, Na
N ,K,
K MMg, Cl,
Cl S
{ Trace minerals (mg/day)
Ù Fe, I, Zn, Cu, Cr, Mn, Mo, F, Se, Si
{ Ultra trace minerals
Ù Va, Tn, Ni, Sn, B
{ Toxic mineral
Ù lead, mercury, cadmium, aluminum
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Importance of ash analysis
y Nutritional labeling. The concentration and type of minerals
1.6% present must often be stipulated on the label of a food.
0.7% y Quality. The quality of many foods depends on the concentration and
type of minerals they contain, including their taste, appearance, texture
0.7% and stability.
2.1% y Microbiological stability. High mineral contents are sometimes
used to retard the growth of certain microorganisms.
0.3%
y Nutrition. Some minerals are essential to a healthy diet (e.g., calcium,
0.8% phosphorous, potassium and sodium) whereas others can be toxic (e.g.,
lead, mercury, cadmium and aluminum).
0.9%
y Processing. It is often important to know the mineral content of foods
1.7% during processing because this affects the physicochemical properties of
foods.
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 Methods for Determining Ash Dry Ashing

{ Dry ashing y Principles

Ùhigh temperature { Separation of minerals from organic compounds of
food products using a muffle furnace capable of
{ Wet ashing maintaining high temperature (>525°C).
(>525 C).
Ùoxidizing agent and/or acid Ù Water and volatiles are vaporized.

{ Microwave ashing Ù Organic substances are burned in the presence of oxygen in

air to CO2 and oxides of N2.
ÙAvailable for both dry and wet ashing Ù The remaining is ash. Most minerals are converted to oxides,
sulfates, phosphates, chlorides, and silicates.

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Dry Ashing General Procedure for Dry Ashing

y Weigh a 5–10 g sample into a tared crucible. Predry if the

y Instrumentation sample is very moist.
{ Muffle furnace y Place crucibles in a cool muffle furnace. Use tongs, gloves,
{ Crucible
and protective eyewear if the muffle furnace is warm.
y Ignite 12
12–18
18 h (or overnight) at about 550
550◦C
C.
Ù porcelain
y Turn off muffle furnace and wait to open it until the
temperature has dropped to at least 250◦C, preferably
lower. Open door carefully to avoid losing ash that may be
fluffy.
y Using safety tongs, quickly transfer crucibles to a desiccator
with a porcelain plate and desiccant. Cover crucibles, close
desiccator, and allow crucibles to cool prior to weighing.
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2
 General Procedure for Dry Ashing Dry Ashing

The ash content is calculated as follows
wt after ashing - crucible wt
% ash (db) =
S l wtt × solid%/100
Sample lid%/100
y Advantages
{ safe and easy
{ no chemical
× 100 { manyy samples
p handled at one time
{ resultant ash for further mineral analysis

wt after ashing - crucible wt y Disadvantages

% ash (wb) = × 100 { loss of volatiles
Sample wt
{ interaction
{ long time and expensive equipment

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Wet Ashing Wet Ashing

y a procedure for oxidizing organic substances by
using acids and oxidizing agents or their
combinations.
y Minerals are solubilized without volatilization.
y Its primary use is preparation for specific mineral
analysis and metallic poisons.
y Analytical testing laboratories use only wet ashing in
preparing samples for certain mineral analyses (e.g.,
Fe, Cu, Zn, P), because losses would occur by
volatilization during dry ashing.
1. Evaporate moist samples (25–50 ml) in an appropriate
dish at 100◦C overnight or in a microwave drying oven
until dry.
2. Heat on a hot plate until smoking ceases.
3. Ash in a 525◦C furnace for 3–8 h.
4. Remove dish from furnace and allow to cool. Ash
should be grayish white to white and free from carbon.
5. Cool and wet with deionized distilled water plus 0.5–
3.0 ml of HNO3.

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3
 Wet Ashing
6. Dry on a hot plate or steam bath and then return to a
525◦C furnace for 1–2 h.
7. Repeat steps 5 and 6 if carbon persists.
8 Dissolve the ash in 5 ml of 1M HNO3 by warming on a
8.
hot plate for 2–3 min to aid solution. Transfer to an
appropriate size volumetric flask (i.e., 50 ml), then
repeat with two additional portions of 1M HNO3.
9. The specific type of mineral being analyzed using AAS
or ICP-MS.
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The end!
Wet Ashing
Advantages
- Minerals will usually stay in solution.
- Little or no loss from volatilization because of the
lower temperature.
- The oxidation time is short and requires a hood,
hood hot
plate, and long tongs, plus safety equipment.
Disadvantages
- It takes virtually constant operator attention,
corrosive reagents are necessary.
- Only small numbers of samples can be handled at
any one time.