EXPERIMENT NO : 2

TITLE : DETERMINATION OF ASH CONTENT

GROUP NO : 10

SESSION : MONDAY ( 2PM-5PM)

GROUP MEMBERS :
1. LOW SU LI 159676
2. NG CHA XIN 157666
3. NURUL SYAMIMI BINTI MOHD ROSIDI 157880
4. NURSYAHIDAH BINTI MD. ARIF 156869

DATE OF LABORATORY PRACTICAL: 26 SEPTEMBER 2011






U N l V E H S l T l P U T H A M A L A Y S l A
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DETERMINATION OF ASH CONTENT

Low Su Li, Ng Cha Xin, Nurul Syamimi binti Mohd Rosidi, and Nursyahidah binti Md. AriI
Department oI Food Technology, Faculty oI Food Science and Technology
University oI Putra Malaysia, 43400 UPM Serdang, Selangor Malaysia

ABSTRACT

Ash content is popular measured properties oI Iood materials. It plays an important role in Iood
research study. In this study, we determine the ash content oI a number oI Ioods. They are milk
powder, Ilour, chillies, green apple, groundnuts, and soya bean. The experimental results Ior ash
content oI milk powder, Ilour, chillies, green apple, groundnuts, and soya bean are 1.0426,
0.42, 0.96, 0.39, 1.751, and 4.46 respectively. The experimental results are diIIerent
Irom the theoretical results. ThereIore, this shows each Iood has its respective ash content.

OB1ECTIVE
In this study, we learn to select suitable ashing procedure based on the limitations. Besides, we
know that there is correlation oI ash content with Iood quality, proximate analysis and nutrient
intake. Many diIIerent types oI Iood sample are being studied enable us to demonstrate sample
preparation Ior diIIerent sample characteristics. Lastly, sequences oI analysis and evaluation can
be carried out Ior the collected experimental data.
INTRODUCTION
Ash is deIined as the inorganic residue remaining aIter a process, burning. Burning will
remove the water and organic matter in the presence oI oxidizing agents. Complete burning will
indicates the ash content by measuring the Iormation oI white ash. Ash content is a measure oI
the total amount oI minerals within a Iood. Minerals distinguish Irom all the other components
within a Iood in some measurable way are the only method oI analytical techniques applied and
give the mineral content inIormation. Nowadays, commonly used methods are based on the Iact
that minerals are not destroyed by heating, and they have a low volatility compared to other Iood
components. Dry ashing, wet ashing and low temperature plasma dry ashing are the three main
types oI analytical procedure used to determine the ash content oI Ioods. DiIIerent condition will
need diIIerent method Ior analysis. ThereIore, the method chosen must consider on the reason Ior
carrying out the analysis, the type oI Iood analyzed and the equipment available. Theoretically,
we should know that ash contents oI Iresh Ioods rarely exceed 5, although some processed
Ioods can have ash contents as high as 12 such as dried beeI. There are 3 main types oI ashing
procedures.
First ashing procedure is dry ashing. It uses a high temperature muIIle Iurnace capable oI
maintaining temperatures oI between 500 and 600
o
C. Normally, in these high temperature, water
and volatile materials will vaporize whereas the organic substances will convert to CO
2
, H
2
O and
N
2
when they are burned in the presence oI the oxygen in air. Although most minerals have Iairly
low volatility at these high temperatures, some are volatile and may be partially lost such as iron,
lead and mercury. It is more advisable to use alternative methods that using lower temperature
when analysis oI determining concentration oI the substances. This advice will prevent the
problems cause by high temperature. There are many advantages oI dry ashing. They are saIe,
Iew reagents are required, many samples can be analyzed.
The next ashing method is wet ashing. Wet ashing is primarily used in the preparation oI
samples Ior subsequent analysis oI speciIic minerals. It breaks down and removes the organic
matrix surrounding the minerals so that they are leIt in an aqueous solution. A dried ground Iood
sample is usually weighed into a Ilask containing strong acids and oxidizing agents 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 oI acids and
oxidizing agents used. Advantage oI wet ashing is little loss oI volatile minerals compared to dry
ashing as lower temperature is used and the process is Iaster. However, it is labor intensive and
require special Iume-cupboard as the method uses acid.
Lastly, low temperature plasma which undergoes oxidation reactions is also one oI the
procedures. Vacuum and an electromagnetic Iield are applied to this procedure. The organic
matter in the sample is rapidly oxidized by the nascent oxygen and the moisture is evaporated
because oI the elevated temperatures. The relatively cool temperatures ( 150
o
C) used in low-
temperature plasma ashing cause less loss oI volatile minerals than other methods is the main
advantage. However, it requires expensive equipment and small sample throughput.
The purpose oI this study is to understand the importance oI minerals content in Iood,
analysis and nutrient requirement.
MATERIALS and APPARATUS and METHODS

Materials and apparatus
In this study, the materials used is Ilour whereas the apparatus used are muIIle Iurnace at 550C,
crucible, thong, desiccators, and spatula.

Methods
Firstly, the crucibles are place Ior 1 hour in the oven at 105C. Then the crucibles are cooled
down in the desiccator. AIter the crucibles are cooled down, the crucibles are weighed
rapidly and accurately. Sample (Flour) is weighed (35g) in the crucibles. Next, the crucible
is inserted together with the sample into the muIIle Iurnace at 550C. They are burned at
least 2 hours or until no black particle present to obtain permanent weight. Then the crucibles
and ash are cooled down in the desiccator. Finally, the crucible is weighed together with the
ash.
RESULT and DISCUSSION
The experimental ash content Ior Ilour is presented as shown in Table 1.
Sample Weight of
crucible
(g)
Weight of
sample
(g)
Weight of crucible
+
Sample after
incineration (g)
Weight of ash
after
incineration
(g)
Ash
percentage
()
A 57.5443 3.0135 57.5576 0.0133 0.44135
B 53.2614 3.0018 53.2728 0.0114 0.37977
C 60.2461 3.0043 60.2592 0.0131 0.43604

The experimental and theoretical moisture content Ior each Iood sample are presented as shown
in Table 2.

The mean oI ash content Ior Ilour is 0.42 whereas standard deviation oI ash content Ior Ilour is
0.035.

CALCULATION
Formula oI ash content,
ash (weight oI ash weight oI crucibles) (weight oI crucible) X 100
Weight oI sample
Calculation oI the ash content Ior each sample,
Sample Experimental Ash Content () Theoretical Ash Content ()
Milk Powder 1.0426 7.7
Flour 0.42 1.0
Chilies 0.96
Green Apple (1) 0.39 0.2
Green Apple (2) 0.31 0.2
Groundnut 1.751 2.5
Soya Bean 4.46 4.8
Sample A
ash 57.5576 57.5443 X 100
3.0135
0.44
Sample B
ash 53.2728 53.2614 X 100
3.0018
0.38
Sample C
ash 60.2592 60.2461 X 100
3.0043
0.44
Mean oI ash content 0.44 0.38 0.44
3
0.42
Standard deviation oI ash content, o
_
_x -
(_x)
n
n-1


_
|0.44)
2
+ (0.38)+ (0.44)] -
(0.44+0.38+0.44)
3
3 - 1

0.035
DISCUSSION
Generally, ash content is a measure oI the total amount oI minerals present within a Iood. The
higher the ash content, the higher the mineral content in the Iood. Ash is the inorganic residue
remaining aIter the water and organic matter have been removed by heating in the presence oI
oxidizing agents, which provides mineral content, a measure oI the total amount oI speciIic
inorganic components within a Iood. The ash content oI each Iood will be diIIerent due to the
diIIerent mineral content in each Iood and the origin oI the Iood. For instance, the sample oI my
group experiment is Ilour. The ash content oI Ilour represents the quantity oI bran which is the
outer layer oI the kernel oI wheat, remains in the Ilour aIter the milling process. Analytical
techniques Ior the total mineral content are based on the minerals that can be distinguished Irom
all the other components within a Iood. According to the theory Ior dry ashing, diIIerent Iood has
diIIerent ash content.
In this study, we know that the theoretical ash content value oI the Ilour is 1.0 whereas the
experimental ash content value (mean) oI the Ilour is 0.42. The standard deviation oI the ash
content is 0.035. Since the standard deviation value is low, it indicates the experimental results
are close to the mean and have higher accuracy. Calculation shows that there is diIIerence
between the theoretical ash content and experimental ash content, which is 0.58. The
diIIerence is a little signiIicance compare to theoretical value. We believe that the diIIerence may
due to several reasons. Firstly, the types oI Ilour sample given are not known. This may
encounter the diIIerence oI ash content compare with the theoretical value. Ash content indicates
milling perIormance by indirectly revealing the amount oI bran contamination in Ilour.
ThereIore, whole wheat Ilour and Ilour with the present oI bran will have diIIerent ash content
value. Next, part oI the minerals may be volatile at certain temperature. ThereIore, this properties
cause the diIIerence between theoretical value and experimental value. Some oI the mineral may
have eliminated during the experiment due to the volatile property and the temperature oI the
analytical equipment.
Generally Irom the sight oI theory, determination oI the ash and minerals content in the Iood
using analytical techniques are important. The data provided are important Ior nutritional
labeling. The concentration and type oI minerals present able to be stipulated on the label oI a
Iood. Next, the quality oI Ioods depends on the concentration and type oI minerals within it. The
quality oI Iood included taste, appearance, texture and stability oI Iood. Then, microbiological
stability can be studied through the data. High mineral contents may be used to retard the growth
oI certain microorganisms or increase the Iermentative activity Ior yeast. Besides, it is Ior
nutrition study oI Iood. Some minerals are essential to a healthy diet such as calcium,
phosphorous, potassium and sodium whereas others can be toxic such as lead, mercury, cadmium
and aluminium. The last importance oI ash and mineral content is Ior processing oI Iood in
industry. It is oIten important to know the mineral content oI Ioods during processing because
this aIIects the physicochemical properties oI Ioods. During the experiment, Ilour is our group
sample material. Our Ilour has lower ash content. This shows that the Ilour has lower mineral
content. Besides, the Ilour will have lower Iermentation activity in dough due to the limited
minerals. The Ilour will also give light (white) color oI dough and light Ilavour oI bread due to
the lower ash content.
Furthermore, minerals oI the Iood are varies because diIIerent Iood are Irom diIIerent raw
material and origin. ThereIore, diIIerent Iood will have diIIerent minerals in it. For instance,
Ilour as a raw material has diIIerent minerals Ior whole wheat Ilour and Ilour with bran
remainder. Besides, diIIerent physicochemical properties oI minerals contribute to diIIerent
value oI minerals content. They are volatility oI minerals, ability oI minerals to react with
speciIic chemical reagents to give measurable changes and unique electromagnetic spectra oI
minerals. For instance, some oI the Iood varies with minerals content due to the minerals
eliminated while the Iood in high temperature. The temperature causes the minerals to gone and
reduce.
Last but not the least, there are diIIerent types oI sample being carried out during the day oI
experiment. They are groundnuts, Ilour, chillies, Ilour, green apple, milk powder and soya bean.
From the experimental value shown, we can see that apple has the lowest ash content value
compare to the other samples. Milk powder has the highest ash content value compare to the
other samples. This shows that diIIerent types oI Iood will have diIIerent ash content. Apple has
the lowest ash content Ior experimental value which is only 0.39. The value is close to the
sample done in our group experiment, Ilour which is 0.42. Apple has low ash content because
it is Iruit which mainly Iiber rather than minerals. Whereas Ilour has low ash content may due to
many reasons as discussed above. Soya bean has the highest ash content which is 4.46. It is
because soya bean is a type oI natural Iood which is very healthy, Iull oI nutrients, and
containing a lot oI minerals.
CONCLUSION
In short, dry ashing method is our choice in the experiment because the method is normally used
Ior all kinds oI Iood except Iood containing trace metal. Our sample in the study is Ilour which
do not contain any trace metal. ThereIore, we choose dry method to analyses our sample, Ilour.
From the study, we know that ash content is a measure oI the total amount oI minerals present
within a Iood. The higher amount oI ash indicates the higher mineral content in the Iood. The ash
content is important Ior proximate analysis such as microbial growth study. Besides, ash content
directly impact to the Iood quality. This is because the quality oI Iood is indicated through the
concentration and type oI minerals present within it. Then it results changes to the taste,
appearance, texture, stability oI Iood and so on. Since ash content has close relationship with the
minerals content, Iood intake with higher ash content will provide more nutrients especially
minerals. Seven diIIerent types oI Iood are being studied. Samples with high moisture content
need to be dry prior to analyses such as green apple. However, our sample, Ilour is not
categorized under high moisture Iood, so it can be prepared without dry prior to analyses. In
order to obtain random sample, we mix the sample well and Ilatter it. AIter that, we will divide it
into quarter and remove two parts Irom the quarter which is diagonally. We should repeat those
step until the suIIiciency amount is leIt Ior the experiment. Other than that, bigger proportion is
required Ior liquid sample whereas dry sample like Ilour need smaller proportion compare to
liquid sample. In the study, we collected the experimental data oI three portion oI sample to
calculate the mean and standard deviation. The experimental ash content is 0.42 which has
6.25 errors Irom the theoretical value, 1 but experimental result still consider acceptable
because the standard deviation, 0.035 is small.

REFERENCES
1. http://people.umass.edu/~mcclemen/581Ash&Minerals.html
2. http://www.progressivebaker.com/resources/tipsunderstandingashcount.shtm
3. http://www.wheatIlourbook.org/Main.aspx?p27
4. http://www.Iarine-mc.com/2009/09/Ilour-ash-content.html
5. http://www.scribd.com/doc/25575913/Determination-oI-Ash
6. Book : Fennema, Owen. R., 1996.Food chemistry, 3rd Ed, Marcel Dekker, Inc. New York.

QUESTIONS
is te burning of sample need to be continued wen black particles of carbon are still
present?
Black particles oI carbon indicate the present oI organic compounds in the sample and
incomplete burning. Continuous burning will result to the Iormation oI white ash which
indicates complete burning and no organic compound present.

at is te purpose of placing te crucible in te oven at C? Give oter alternative tat
ave te same purpose
Ensure the crucible to dry completely is the main purpose oI placing the crucible in the oven
at 105C. This temperature will ensure the results oI moisture content are not aIIected by the
moisture in the crucible when it is weight by the analytical balance. Alternatively, silica gel
is added in the desiccators to achieve the same purpose. Silica gel will absorb all the moisture
in the desiccators and crucible to ensure the moisture content oI the crucible is correct.

ow food industries meet te mineral requirement for te food tat te produced?
Food industries meet the mineral requirement Ior the Iood that they produced by carry out
burning oI the Iood and analyses the ash Iorm. White ash indicates the complete burning is
carried out. The ash Iormed can then be a measure oI the total amount oI minerals within the
Iood. There are three main types oI analytical techniques use to determine the ash content oI
Ioods. They are dry ashing, wet ashing and low temperature plasma dry ashing. This type oI
analytical techniques are commonly use in Iood industries in order to meet the mineral
requirement Ior the Iood produced. DiIIerent types oI Iood, purpose oI analysis and
equipments availability will need diIIerent methods to carry out the analysis.

4. at tpe of desiccant used in tis analsis? ow ou andle our desiccant to give good
performance?
The type oI desiccant used in this analysis is silica gel. It is a Iorm oI silica dioxide (SiO
2
), a
naturally occurring mineral. This silica gel is used to absorb all the moisture being absorbed by
the crucible while taking out Irom the oven and transIer to the desiccator. ThereIore, desiccator
should near to the oven to reduce the exposure probability oI crucible to the moisture
atmosphere. Besides, the opening hole to transIer crucible to desiccators should as small as
possible to reduce moisture air enter.