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Setyaningrum Ariviani
 Ash analysis is a measure of the total

amount of minerals present within a food
 Mineral analysis is a measure of the

amount of specific inorganic components
present within a food such as Ca, Na, K
and Cl
 Ash is 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.
 Principle:
› Minerals are not destroyed by heating, and that they
have a low volatility compared to other food
components.
 Ashing may also be used as the first step in preparing
samples for analysis of specific minerals, by atomic
spectroscopy or the various traditional methods.
 The ash content of most fresh foods rarely is greater
than 5%, Fats, oils, and shortenings vary from 0.0 to
4.1% ash, while dairy products vary from 0.5 to 5.1%.
Fruits, fruit juice, and melons contain 0.2–0.6% ash, while
dried fruits are higher (2.4–3.5%). Flours and meals vary
from 0.3 to 1.4% ash. Pure starch contains 0.3% and
wheat germ 4.3%ash.
 Solid food are finely ground and mixed
 Sample with high moisture content are often
dried to prevent spattering during ashing
 Sample with high fat content are usually
defatted
 Mineral from grinders, glassware or crucible
should be prevented to come into contact with
sample.
 The water source used in dilutions also may
contain contaminants of some
microelements==> Deionized water is
recommended to avoid incorrect results.
v Dry ashing
v Wet ashing
Procedures
 AOAC International has several dry ashing
procedures (e.g., AOAC Methods 900.02 A or
B, 920.117,
923.03) for certain individual foodstuffs
1. Weigh a 5–10-g sample into a tared crucible. Predry if the
sample is very moist.
2. Place crucibles in a cool muffle furnace. Use tongs, gloves, and
protective eyewear if the muffle furnace is warm.
3. Ignite 12–18 h (or overnight) at about 550◦C.
4. 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.
5. 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 weighin
% ash (wet basis)=
wt after ashing−tare wt of crucible × 100

original sample wt
% ash (dry basis)=
wt after ashing−tare wt of crucible × 100

original sample wt × dry matter coefficient
where: dry matter coefficient = % solids/100
 Use a high temperature muffle furnace (550-
600°C)
 Water and other volatile materials are vaporized
and organic compounds are burned in the
presence of oxygen to CO2, H2O and N2.
 Most minerals are converted to oxides, sulfates,
phosphates, chlorides or silicates
 The sample is weighed before and after ashing
 Advantages:
› Safe, few reagent are required, many samples can be
analyzed simultaneously, not labor intensive, and ash
can be analyzed for specific mineral content
 Disadvantages:
› Long time required, muffle furnace are quite costly to
run due to electrical costs, lost of volatile minerals at
high temperature eg, Cu, Fe, Pb, Hg, Ni and Zn
 Primarily used in the preparation of samples for
subsequent analysis of specific minerals
 It breaks down and removes the organic matrix
surrounding the minerals so that they are left in an
aqueous solution.
 A dried ground food sample is usually weighed into a
flask containing strong acids and oxidizing agents (e.g.
nitric, sulfuric acid) and then heated.
 Heating is continued until the organic matter is
completely digested, leaving only the mineral oxides
in solution. The temperature and time used depends
on the type of acids and oxidizing agents used.
 Typically, a digestion takes from 10 minutes to a few
hours at temperatures of about 350oC. The resulting
solution can then be analyzed for specific minerals.
 Advantages: little loss of volatile minerals due to
low temperature 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
throughout
1. Soluble and Insoluble Ash in Water (e.g., AOAC Method 900.02)
› An index of fruit content of preserves and jellies
› A lower ash indicates extra fruit is added to fruit and sugar products
› Ash is diluted with distilled water then heated to nearly boiling, and the
resulting solution is filtered. The amount of soluble ash is determined by
drying the filtrate, and the insoluble ash is determined by rinsing, drying and
ashing the filter paper.
2. Ash Insoluble in Acid
› Use to measure surface contamination of fruits and vegetables, wheat and
rice coating=> contaminants are generally silicates and remain insoluble in
acid, except HBr.
3. Alkalinity of Ash(e.g., AOAC Method 900.02, 940.26)
› Ash of fruits and vegetable is alkaline; ash of meats and some cereals is acid.
4. Sulfated ash (AOAC Method 900.02, 950.77)
› Applied to sugars, syrups, and color additives Used as quality index of fruit
and fruit juices
 The conventional dry ashing procedure is simple to
carry out, is not labor intensive, requires no expensive
chemicals and can be used to analyze many samples
simultaneously. Nevertheless, the procedure is time-
consuming and volatile minerals may be lost at the high
temperatures used.
 Wet ashing are more rapid and cause less loss of volatile
minerals because samples are heated to lower
temperatures. Nevertheless, the wet ashing procedure
requires the use of hazardous chemicals and is labor
intensive
1. A grain was found to contain 11.5% moisture. A 5.2146g sample was
placed into a crucible (28.5053g tare). The ashed crucible weighed
28.5939g. Calculate the percentage ash on
(a)an as-received (wet weight) basis
(b)a dry matter basis.
2. The following data were obtained on a sample of
hamburger: sample wt, 2.034g; wt after drying, 1.0781g; wt
after ether extraction, 0.4679g; and wt of ash, 0.0233g. What
is the percentage ash on
(a) a wet weight basis and dry weight basis (b) a fat-free basis?
1. Crucible + ash: 28.5939g, Tared crucible: 28.5053g ==> Ash: 0.0886g
(a) Calculate for ash on a wet weight basis (a):
(0.0886g ash : 5.2146g sample )×100% = 1.70%
(b) Calculate for ash on a dry weight basis (b):

%db = %wb/ (1-ka) = 1.7% :( 1-0.115) = 1.7%/ 0.885 = 1.92%
2. Sample wet wt: 2.034g, Sample dry wt: 1.0781g Wt, after extraction: 0.4679g Wt of
ash: 0.0233g
(a) Calculate for ash on a wet weight basis and dry weight basis
- Ash (% wb) = (0.0233g ash : 2.034g sample)×100% = 1.15%
- moisture= [(2.034g wet sample−1.0781g dry sample) / 2.034 g wet sample ] x 100% =
= 47%
- Ash (% db) = % wb / (1-ka) = 1.15%/ (1-0.47) = 2.17%
(b) calculate for ash on a fat-free basis?
- fat (g ) = 1.078g dry sample - 0.4679g sample after extraction = 0.6102 g fat
- % ash (fat free basis)=
[0.0233g ash / (2.034 g wet sampel - 0.6102 g fat)] x 100% = 1.64%
 The most effective means of determining the
type and concentration of specific minerals in
foods is to use atomic absorption or emission
spectroscopy
 Can quantify to concentrations as low as a few
ppm
 The sample need to be ashed using one of the
method previously described
› Reason: to isolate the minerals from the
organic matrix surrounding them
 Presence of contaminants in the water, reagents
or glassware
› Recommended to use ultrapure water and/or
reagents
› Use the same glassware and reagents for blank
 The element to be analyzed is precipitated from
solution by adding a reagent that reacts with it to
form an insoluble complex with a known chemical
formula
 The precipitate is separated from the solution by
filtration, rinsed, dried and weighed
 The amount of the element present in the sample is
determined from the chemical formula of the
precipitate
 Example: the amount of chloride in a solution can
be determined by adding excess silver ions to form
an insoluble silver chloride precipitate.
› It is known that Cl is 24.74% of AgCl.
 Not suitable to determine trace elements in food
because the balances are not sensitive enough to
accurately weigh small amount of precipitate
formed.
 Rely on a change in color of a reagent when it
reacts with a specific mineral in solution which can
be quantified by measuring the absorbance of the
solution at a specific w/length using a
spectrophotometer
 Example: yellow-orange color forms when vandate-
molybdate is added to phosphorus containing
sample. The phosphorus then can be quantified by
measuring the absorbance of the solution at 420nm
and comparing with a calibration curve.
 EDTA compleximetric titration
› EDTA is a chemical reagent that forms strong
complexes with multivalent metallic ions.
› The complexes formed by metal ions and
EDTA can be represented by the following
equations:
m2+ + H2Y2- → mY2- + 2H+
m3+ + H2Y2- → mY- + 2H+
m4+ + H2Y2- → mY + 2H+
Sample is diluted with water
Made alkaline (pH 12.5 to 13)
Indicator is added
Titrate with EDTA

 EDTA forms complexes with minerals first then
with the indicator – determine the end point of
the reaction
 The calcium content is determined by
comparing the volume of EDTA required to
titrate it to the end point with a calibration
curve prepared for a series of solutions of
known calcium concentration
 When at least one of a titration reaction is
insoluble in precipitate
 Common method: Mohr for chloride analysis
 Silver nitrate is titrated into an aqueous solution
containing sample and a chromate indicator
AgNO3 + NaCl → AgCl (s) + NaNO3
 End point: the first hint of orange color
 Principle:
› Each element has a unique electronic structure
› Consequently, it absorbs or emits radiation at
specific wavelength
› Absorption: electrons in the ground state are
promoted to various excited states
› Emission: electrons in an excited state fall back
to a lower energy level
 Atomic absorption spectroscopy (AAS) is an
analytical method that is based on the
absorption of UV-visible radiation by free atoms
in the gaseous state.
Ashed sample is dissolved in an aqueous solution
Placed in the instrument where it is heated to vaporize

and atomize the minerals
A beam of radiation is passed through the atomized sample
Absorption of radiation at specific w/length

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Setyaningrum Ariviani

 Ash analysis is a measure of the total

 Mineral analysis is a measure of the

wt after ashing−tare wt of crucible × 100

% ash (dry basis)=

wt after ashing−tare wt of crucible × 100

(b) Calculate for ash on a dry weight basis (b):

Made alkaline (pH 12.5 to 13)

Titrate with EDTA

Placed in the instrument where it is heated to vaporize

A beam of radiation is passed through the atomized sample

Absorption of radiation at specific w/length

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