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Analysis of
Ash & Minerals
Dry Matter
1. Organic compounds:
– Carbohydrates
– Lipids
– Proteins
– Nucleic acids
– Vitamins
– Organic acids
2. Inorganic Compounds:
- Minerals
• “Ash content” - total amount of minerals
present within a food.
• “Mineral content” - amount of specific
inorganic components present within a food,
such as Ca, Na, K and Cl.
Determination of Ash Content
• Ash - inorganic residue remaining after water and
organic matter removed by heating in the presence
of oxidizing agents.
• Principle: Minerals are not destroyed by heating,
and they have low volatility compared to other
food components.
• Main types Ashing: dry ashing, wet ashing,
plasma ashing
• Method chosen depends on the reason for
carrying out analysis, type of food analyzed
and equipment available
Sample Preparation
• Representative sample.
Typically, samples of 1-10g are used.
Solid foods are finely ground and carefully mixed
(representative sample).
• Before ash analysis, samples high in moisture are
dried to prevent spattering.
• High fat samples are defatted by solvent extraction
(facilitates release of moisture and prevents
spattering).
• Avoid contamination of samples by minerals in
grinders, glassware or crucibles etc.
Dry Ashing
• Use a high temperature muffle furnace (To between 500
and 600oC).
• Water and other volatile materials are vaporized and
organic substances are burned in the presence of O2 in
air to CO2, H2O and N2.
• Most minerals are converted to oxides, sulfates,
phosphates, chlorides or silicates.
• Some minerals are volatile and may be
partially lost, e.g., iron, lead and mercury.
• For such minerals - use an alternative ashing
method that uses lower temperatures.
• Food sample is weighed before and after ashing to
determine the concentration of ash present.
• The ash content can be expressed on either a dry or
wet basis:
• The following data was obtained on a sample of hamburger:
sample wt, 2.034 g ; wt after drying, 1.0781 g; and wt of ash,
0.0233 g.
What is the percentage ash on a) a wet weight basis and b)
dry-weight basis?
Wet Basis Ash % = (0.0233 / 2.034) *100
= 1.15 %
Dry Basis Ash % = (0.0233 / 1.0781) * 100
= 2.16 %
• Different types of crucible - quartz, Pyrex,
porcelain, steel and platinum.
• Selection depends on sample being analyzed and
furnace temperature used.
• Most widely used - porcelain (relatively
inexpensive, resistant to high temperatures
(< 1200oC) and easy to clean).
Platinum
Pyrex
Porcelain
Quartz
• Advantages: Safe, few reagents are required, many
samples can be analyzed simultaneously, not labor
intensive, and ash can be analyzed for specific
mineral content.
• Disadvantages: Long time required (12-24 hours),
muffle furnaces are quite costly to run due to
electrical costs, loss of volatile minerals at high
temperatures, e.g., Cu, Fe, Pb, Hg, Ni, Zn.
Wet Ashing
• Primarily used in preparation of samples for specific
minerals analysis.
• It breaks down and removes organic matrix
surrounding minerals and left them in an aqueous
solution.
• A dried ground food sample weighed into a flask
containing strong acids and oxidizing agents (e.g., nitric,
perchloric and/or sulfuric acids) heated.
• Heating is continued until organic matter is
completely digested, leaving only mineral oxides in
solution.
• Temperature and time - depends on type of acids
and oxidizing agents used.
• Typically, a digestion takes from 10 minutes to a
few hours at about 350oC.
• Resulting solution can be analyzed for specific
minerals.
• Advantages: Little loss of volatile minerals
occurs because of the lower temperatures used,
more rapid than dry ashing.
• Disadvantages: Labor intensive, requires a
special fume-cupboard if perchloric acid is used
because of its hazardous nature, low sample
throughput.

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Ash FT.pptx

  • 1. Analysis of Ash & Minerals
  • 2. Dry Matter 1. Organic compounds: – Carbohydrates – Lipids – Proteins – Nucleic acids – Vitamins – Organic acids 2. Inorganic Compounds: - Minerals
  • 3. • “Ash content” - total amount of minerals present within a food. • “Mineral content” - amount of specific inorganic components present within a food, such as Ca, Na, K and Cl.
  • 4. Determination of Ash Content • Ash - inorganic residue remaining after water and organic matter removed by heating in the presence of oxidizing agents. • Principle: Minerals are not destroyed by heating, and they have low volatility compared to other food components.
  • 5. • Main types Ashing: dry ashing, wet ashing, plasma ashing • Method chosen depends on the reason for carrying out analysis, type of food analyzed and equipment available
  • 6. Sample Preparation • Representative sample. Typically, samples of 1-10g are used. Solid foods are finely ground and carefully mixed (representative sample).
  • 7. • Before ash analysis, samples high in moisture are dried to prevent spattering. • High fat samples are defatted by solvent extraction (facilitates release of moisture and prevents spattering). • Avoid contamination of samples by minerals in grinders, glassware or crucibles etc.
  • 8. Dry Ashing • Use a high temperature muffle furnace (To between 500 and 600oC). • Water and other volatile materials are vaporized and organic substances are burned in the presence of O2 in air to CO2, H2O and N2. • Most minerals are converted to oxides, sulfates, phosphates, chlorides or silicates.
  • 9. • Some minerals are volatile and may be partially lost, e.g., iron, lead and mercury. • For such minerals - use an alternative ashing method that uses lower temperatures.
  • 10. • Food sample is weighed before and after ashing to determine the concentration of ash present. • The ash content can be expressed on either a dry or wet basis:
  • 11. • The following data was obtained on a sample of hamburger: sample wt, 2.034 g ; wt after drying, 1.0781 g; and wt of ash, 0.0233 g. What is the percentage ash on a) a wet weight basis and b) dry-weight basis? Wet Basis Ash % = (0.0233 / 2.034) *100 = 1.15 % Dry Basis Ash % = (0.0233 / 1.0781) * 100 = 2.16 %
  • 12. • Different types of crucible - quartz, Pyrex, porcelain, steel and platinum. • Selection depends on sample being analyzed and furnace temperature used. • Most widely used - porcelain (relatively inexpensive, resistant to high temperatures (< 1200oC) and easy to clean).
  • 14. • Advantages: Safe, few reagents are required, many samples can be analyzed simultaneously, not labor intensive, and ash can be analyzed for specific mineral content. • Disadvantages: Long time required (12-24 hours), muffle furnaces are quite costly to run due to electrical costs, loss of volatile minerals at high temperatures, e.g., Cu, Fe, Pb, Hg, Ni, Zn.
  • 15. Wet Ashing • Primarily used in preparation of samples for specific minerals analysis. • It breaks down and removes organic matrix surrounding minerals and left them in an aqueous solution. • A dried ground food sample weighed into a flask containing strong acids and oxidizing agents (e.g., nitric, perchloric and/or sulfuric acids) heated.
  • 16.
  • 17. • Heating is continued until organic matter is completely digested, leaving only mineral oxides in solution. • Temperature and time - depends on type of acids and oxidizing agents used. • Typically, a digestion takes from 10 minutes to a few hours at about 350oC. • Resulting solution can be analyzed for specific minerals.
  • 18. • Advantages: Little loss of volatile minerals occurs because of the lower temperatures used, more rapid than dry ashing. • Disadvantages: Labor intensive, requires a special fume-cupboard if perchloric acid is used because of its hazardous nature, low sample throughput.