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Chem181 Lab Applied Chemistry (03/16/16)

Proximate Analysis of Vitarich Premium Plus Hog Finisher


Cagampan, John S., Dagondon, Vanessa Olga J., Jomocan, Christine Anne D.
University of the Philippines Visayas
Miagao, Iloilo
Abstract
The feed industry is one of the growing industry in the Philippines. It consists primarily
of livestock, poultry, and aquaculture sub-sectors. In livestock, one of the most sought feed is the
hog feeds. Hog industry is one of the main sources of protein in the country. Thus, a quality
assured hog feeds must be manufactured and distributed in agricutural sectors in order to
produce high quality hog meat.
In this study, a proximate analysis is done on a representative hog feed, Vitarich Premium
Plus Hog Finisher Pellets. Nutrients found in the feed such as moisture, curde protein crude fait,
crude fiber, ash/mineral and the Nitrogen free extract were analyzed by standard analytical
methods such as oven drying, kjeldahl method, etc. The analysis yielded the following values for
the said nutrients: for moisture content, 8.123 (0.063) %; for crude protein content, 19.9 (1.0)
%; for crude fat content, 11.8 ( 6.3)%; for crude fiber content, 6.85 ( 0.86)%; for
ash/mineral content, 18.049 (11.0)%; and, for a nitrogen free extract, 43.4%. These obtained
values corresponds to the guaranteed analysis done by Vitarich.
Introduction
Vitarich Hog Grower feeds is one of
the many commercially available feeds for
poultry such as pigs. This grower feeds is
used to help speed up the growth of pigs to
let the owner have a good profit from selling
it. Hog grower feeds is said to have a great
effect on the growth of feeds, thus it is well
known and readily available in the market.
Proximate analysis is a series of
testing, extracting and many other process as
to which we could differentiate and
determine different amount of compounds
that are present in the food or any material
of interest. This series of test often include
ashing, which determines the amount of
insoluble component in our samples,

determination of moisture, crude fat, fiber


and some other test that are used for
different components which we are
interested in. This would help us easily
identify important factors such as the
amount of metal, amount of soluble
compounds, etc.
As one of the easiest method and
somehow cheap, this analysis would readily
help us to determine and identify the
presence and amount of compound in the
sample which is of our interest. With this
proximate analysis help, different companies
and other agencies could help verify whether
labels and content information which are
presented are true. This would also help
determine which part or component of the
sample could be easily used or discard in
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Chem181 Lab Applied Chemistry (03/16/16)

order to improve such products. Thus


proximate analysis would readily help an
individual in creating and improving
different products.
Theory
Moisture
Moisture determination is one of the
most used methods of analysis in the
agricultural sector. Water is one of the six
classes of nutrients present in animal feeds
alongside carbohydrates, proteins, fats,
vitamins and minerals. Therefore, the
determination of the moisture in animal
feeds is critical in its overall nutritional
value and thus is an important factor in
agricultural commerce and management
(Thiex and Richardson, 2003).
Also, the moisture content is
essential to the conversion of the nutrient
contents to a dry matter (DM) basis Dry
matter basis is one bases on which a nutrient
content can be expressed. This is the amount
of nutrient contained in the feedstock in the
dry matter fraction, without water. The DM
basis of nutritional contents can be estimated
in terms of percentage by subtracting 100 by
the moisture content. The determination of
the DM basis is important in ensuring that
the feeds are giving the proper nutrients to
the animals through their prescribed diet and
feeding program (Jurgens and Bregendahl,
1972;Thiex and Van Erem, 1999; Nenninch
and Chase, 2012).
The moisture content of a feed can
be calculated as the weight loss of a feed
sample after the application of heat. The
most common procedure in determining the

weight loss of the sample after drying is the


oven-drying method. This method incudes
oven drying approximately 2 grams of the
sample feed at 135 degree Celsius for two
hours (AOAC, 1990; method 930.15). This
method is widely used because of its
simplicity.
Crude Protein
Proteins are polymers of amino
acids. Amino acids are a class of nitrogencontaining compounds. There are twenty
different amino acids occurring naturally in
proteins. This variation gives proteins
different molecular structures, nutritional
attributes and physiochemical properties.
Crude protein content in feedstuffs is one of
the most essential parameters from a
nutritional and from a quality perspective.
Sufficient protein must be provided to the
livestock to ensure energy supply required
by the animal for maintenance, growth,
pregnancy and lactation.
The percentage crude protein in a
feedstuff can be determined by first
determining its nitrogen content by Kjeldahl
method. The Kjeldahl method of the
determination of nitrogen was first
introduced by Johan Kjeldahl in 1883. Over
the past 100 years, Kjeldahl method has
been altered and refinde but its basic
principles still remain today. Kjeldahl
analysis has three major steps: (1) digestion,
(2) distillation, and (3) titration.
In the digestion process, the nitrogen
is decomposed decomposes in the presence
of a concentrated acid solution. This is done
by heating the sample to boiling in a
concentrated sulfuric acid to yield a solution
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Chem181 Lab Applied Chemistry (03/16/16)

of ammonium sulfate. Boiling chips and a


digestion catalyst is added to the solution to
aid boiling. Equation 1 illustrates the
reaction that takes place in digestion.
NH
( 4 )s SO 4 + H 2 O+CO2 +other sample
Organic N + H 2 SO 4
eq. 1
In distillation, an excess base is
added to the digested mixture to convert
ammonium ion into ammonia gas. The
ammonia gas is then boiled and condensed
(distilled) and is trapped into a flask
containing a standardized acid or boric acid
to be titrated in the next step. Equation 2
shows the reaction when s relatively strong
solution of NaOH is added to the digested
mixture containing the ammonium sulfate.
Consecutively, equation 3 shows the
reaction between boric acid and the
ammonia liberated in equation 2.

complex is titrated against a standardized


acid with BCG-MS as an indicator. The
resulting chemical reaction for the titration
against HCl is as follows:
2 NH 4 H 2 BO 3 + HCl NH 4 Cl + H 3 BO 3
eq. 3
The addition of HCl neutralizes the
ammonium borate complex and the original
color of the solution restored prior to the
addition of boric acid (green to pale red).
Using basic titrimetric and analytical
calculations, the concentration of nitrogen
expressed as % w/w is determined.
After determining the %N, the crude
protein can be calculated by multiplying the
%N with a conversion factor. The
conversion factor is usually 6.25 for a lot of
products. However, this is only an average
and different conversion factor depends on
the amino acid composition of the product.

NH
( 4 )s SO 4 +2 NaOH NH 3 + Na2 SO 4 +2 Crude
H 2 O Fat

The term fat is a general term that


is
also
referred to as lipid in scientific
eq. 2
terms. Fats or lipids are a diverse group of
organic chemicals but they similarly
3+ H 3 BO 3
dissolve in nonpolar solvents and are not
4 + : H 2 BO
soluble in polar solvents such as water.
NH 3 + H 2 BO 3 NH
There are two methods for the
analysis of fat in certain samples, namely,
eq. 3
crude methods and total fat test. Crude
methods involve extracting fat by dissolving
At this stage, the solution is of green
the samples fat in an organic solvent
color due to the presence of the ammoniumusually ether or hexane and eventually
borate complex. The last step is titration.
evaporating the solvent.
Titration is done to determine the amount of
Crude fat is the term used to refer to
ammonia trapped in the resulting solution in
the crude mixture of fat-soluble material that
equation 3. The solution containing the
is present in a sample. Crude fat also known
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Chem181 Lab Applied Chemistry (03/16/16)

as the ether extract or the free lipid content,


is a measure of fat in food products.
The lipid materials present in crude
fat may include triglycerides, diglycerides,
monoglycerides, phospholipids, steroids,
free fatty acids, fat soluble vitamins,
carotene pigments, chlorophylls, etc.
Total crude fat determination can be
based on the solubility of lipids in non-polar
organic solvents such as hexanes and
petroleum ether. The two methods used
commonly to determine crude fat are wet
extraction and dry extraction. Wet extraction
is performed on water-containing samples.
(Rosenthal and Trowbridge, 1915)
The method used in this analysis is
dry extraction where the samples are made
moisture-free. A common dry extraction
method is Soxhlet extraction method. This is
performed with anhydrous ether. It is
common crude fat determination method in
many food and other products. This
technique extracts the crude fat into ether
which is finally evaporated. Dry extraction
is preferred when it is inconvenient to
remove most of the water from a sample.
After extraction the solvent used is
evaporated, then the residue is weighed and
is reported as percent crude fat.
Three factors that can affect crude fat
analysis are moisture content, sample
preparation, and extraction methodologies.
The Soxhlet allows one to extract
chemicals from a solid sample into a liquid,
leaving behind insoluble impurities, as it
consists of a glass reservoir which sits
between a lower flask at the bottom and a
condenser at the top. It uses a small volume
of solvent over and over again. Inside the
reservoir sits a thimble-shaped filter in
which one's sample is placed at the start of
the procedure. The solvent is heated up from
its starting position in the lower flask. As the

boils, the condenser returns it to drip


steadily into the thimble. This allows the
soluble components of the sample to be
extracted (Sella, 2007).
Crude Fiber
Crude fiber is a measure of the
quantity of indigestible cellulose, lignin, and
other components of this type in present
foods.
It is the residue of plant materials
remaining after solvent extraction followed
by digestion with dilute acid and alkali.
These components have little food value but
provide the bulk necessary for proper
peristaltic action in the intestinal tract in
humans as well in most animals.
The crude fiber method was
developed in the 1850s to estimate
indigestible carbohydrate in animal feeds.
Since an easy alternative was not available,
fiber in human foods was measured as crude
fiber until the early 1970s. Crude fiber
method is one of the gravimetric method
that measures the organic food residue
remaining after sequential digestion with
sufficient concentration of sulfuric acid and
of sodium hydroxide solutions. This can be
followed by oven-drying at 104C overnight
and ignition in muffle furnace at 600C for 3
hours. The compounds removed are
predominantly protein, sugar, starch, lipids
and portions of both the structural
carbohydrates and lignin. Crude fiber
method measures variable amounts of the
cellulose and lignin in the sample, but
hemicelluloses, pectins, and added gums or
hydrocolloids are solubilised and removed.
Therefore, crude fiber measurement
drastically underestimates dietary fibre in
foods since it measures only cellulose and
lignin. This is why this method is only used
in determining the crude fiber amount is
animal feeds.
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Chem181 Lab Applied Chemistry (03/16/16)

Ash/Mineral
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.

After cooling, each was weighed in an


analytical balance (SHIMADZU). The
crucibles were again oven dried for an hour,
cooled for half an hour and were again
weighed. This repetitive process is done
until a constant weight was achieved.
However, due to time constraints and
instrumental errors, it was done until five
trials only.
The weight reading in the fifth trial
was used to calculate for the moisture
content of the three samples. Moisture
content of the sample was expressed in
percentage with its corresponding standard
deviation.

NFE

Crude Protein

Nitrogen-Free Extract is a section in


which we estimate the highly digestible
carbohydrates such as starch, free sugars and
hemicelluloses. It accounts for all the
previous fraction that are reduced from its
original amount. Thus, its numerical values
are affected by the errors done in every
analysis which results to the biggest error in
approximation.

The percentage crude protein of the


resulting samples in the determination of
moisture content was analyzed. The samples
analyzed were in triplicates. Prior to the
analysis, the reagents needed were prepared.
40% NaOH, 0.100N of HCl and the
digestion catalyst were prepared by the
designated groups in the class. Other
reagents such as the concentrated sulfuric
acid, 4% boric acid, Na2CO3 standard and
the mixed indicator BCG-MR were readily
given in stock at the laboratory.

Methodology
Moisture
A hog feeds of known brand
(Vitarich Premium Plus Finisher Pellets)
was obtained. Around 20 grams of the feeds
were powderized and homogenized using a
mortar and pestle. Approximately 5 grams of
the powderized feeds were placed in a preweighed crucible. This was done in
triplicates. The crucibles containing the
feeds were oven dried at around 110 degree
Celsius for an hour. The crucibles were let to
cool down in a desiccator for 30 minutes.

SemiKjeldahl
method
was
incorporated in order to determine the
percentage nitrogen and thereby calculating
the percentage crude protein in each sample.
The procedure for the determination of
percentage nitrogen composes of three
major steps. The first one step is the
standardization of the 0.100 N HCl, next is
the digestion and lastly the distillation which
includes the titration process.
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Chem181 Lab Applied Chemistry (03/16/16)

The standardization of the 0.100N


HCl was done by a designated group in the
class. The prepared HCl was standardized
against a standard Na2CO3 with the mixed
indicator BCG-MR as the indicator. The
standardization was done in triplicates. The
used volume of HCl was recorded and the
average normality of HCl was computed.
The sample taken from the pre-dried
samples from the moisture content analysis
was weighed accordingly to the approximate
protein content of the sample feed given in
its label. The approximate protein content of
the sample feed is 16% which corresponds
to a sample size of 300 mg. Only 100 mg of
the sample was weighed in all replicates.
The sample was transferred in the Kjeldahl
flask along with the boiling chips and
approximately two grams of the digestion
catalyst which was made from mixing
CuSO4*5H2O
and
K2SO4.
10
ml
concentrated H2SO4 was added to the flask
and was boiled until a clear solution was
obtained. It took around 8 hours of boiling
before the clear solution was achieved. The
last step in the procedure is the distillation.
The digest was transferred from the Kjeldahl
flask to the round bottom flask attached to
the distilling unit. In a 125 ml Erlenmeyer
flask, 10 ml of the 4% Boric acid and 3-4
drops of BCG-MR were added. This
Erlenmeyer flask was connected to the tip of
the condenser. Approximately 30-40 ml of
40% NaOH was added to the round bottom
flask until solution is dark. It was then
distilled until solution turned green.
Afterwards the distillate collected in the
Erlenmeyer flask was titrated with the
standardized HCl until the color changes
from green to light pink. The used volume

of HCl during the titration of the triplicates


was recorded. This was used to compute for
the percentage nitrogen. From the
percentage nitrogen, the percentage crude
protein was calculated by multiplying it with
a factor (6.25). The average of the triplicates
was reported alongside its uncertainty.
Crude Fat
Approximately 2.5 g of ground
sample was weighed and was placed on a
filter paper. Three replicate samples were
prepared but only two were used for the
extraction using the Soxhlet apparatus
because of shortage of materials for the setup. After placing the sample on the filter
paper, the filter paper was folded twice,
wrapping and protecting the sample.
The
Soxhlet
apparatus
was
assembled and each of the samples was
placed on its designated Soxhlet flask. One
blank was run for two groups of samples by
using the same size of filter paper.
Approximately 175 mL of petroleum
ether was poured into the each of the flask,
soaking the sample with the solvent. The
extraction lasted for 8 hours, from 11 am to
7 pm. A cotton was plugged in the hollow
tube on the top of the condenser to avoid
leaks.
After the extraction using the
Soxhlet apparatus, the filter paper with the
sample was removed from each of the flask
and was allowed to be air-dried to remove
excess ether. The petroleum ether with the
crude fat in the round bottom flask was
attached to the rotary evaporator to
evaporate the solvent slowly and to isolate
the crude fat. The solvent was recovered and
the isolated fat was then placed in a
preweighed vial for each trial. The vials with
the crude fat were weighed in an analytical
balance.
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Chem181 Lab Applied Chemistry (03/16/16)

Crude Fiber
The defatted sample from part C was
transferred into 600-mL beaker. Two
hundred mL of 0.64 N sulfuric acid and the
sample was boiled for 10 minutes with
constant stirring. After boiling for 10
minutes, the mixture was filtered using a
dress linen. The residue was washed in hot
distilled water (50 mL per washing) for
several times until the washings were no
longer acidic when added by the indicator
methyl red. Acidity is signaled by having red
to yellow color change. When the washing
were no longer acidic, the residue was
quantitatively transferred to another beaker
by using 100 mL hot water. Two hundred
mL of 1.56N NaOH was added to the
transferred residue and was boiled to 10
minutes like in the acid mixture. After
boiling for ten minutes, the residue was
again filtered using a dry dress linen and
was washed several times with hot distilled
water as in the acid mixture. This time,
washings were made until the filtrate was no
longer alkaline as signaled by adding a
phenolphthalein indicator, with clear to light
pink change in color of the liquid.
When the filtrate was no longer
alkaline, the residue was transferred to a preweighed filter paper. The mass of the residue
was obtained by weighing by difference.
The whole process was done in the two
replicate defatted samples.
Ash/Mineral
Three marked clean porcelain crucible were
heaated in the muffle furnace for about an
hour. Each of the crucibles were then cooled
in a desiccator and were weighed after 30
minutes. Approximately 2.00 grams sample
were weighed into a weighed porcelain in
triplicates. It was pre-ashed under the hood
until fumes were all consumed. It was then
transfer to a muffle furnace, and was ignited
at 550 degrees C for about 6 hours or until

residue is uniformly grayish to white color.


The temperature was lowered at 105 degrees
C and was maintained for about 20 minutes.
It was cooled in a desiccator and weighed
after 30 minutes.
NFE
Arithmetic Difference of all the results of
previous analysis were applied to get the
percent NFE value.
Discussion
Table 1 shows the summary of the
results of the proximate analysis of the
Vitarich Premium Plus Hog Finisher from
the moisture content to the NFE content all
having stated their standard deviations.
Crude protein, crude fat, crude fiber,
ash/mineral and NFE content are all dry
basis.
Consequently, Table 2 shows the
result of the guaranteed analysis of Vitarich
for their product. These values ill serve as
comparison with the obtained values in the
analysis.
Parameter
Moisture
Crude Protein
Crude Fat

Value (meanSD)
8.123 (0.063) %
19.9 (1.0) %
11.8 ( 6.3)%.

Crude Fiber

6.85 ( 0.86)%

Ash/Mineral
18.049 (11.0)%
NFE
43.4%
Table 1. Summary of the Proximate Analysis
of Vitarich Premium Plus Hog Finisher.
Parameter
Value
Moisture
NMT 12.00%
Crude Protein
NLT 15.00%
Crude Fat
NLT 4.00%
Crude Fiber
NMT 7.00%
Table 2. Vitarich Premium Plus Hog
Finisher Guaranteed Proximate Analysis.
*NMT means not more than
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Chem181 Lab Applied Chemistry (03/16/16)

**NLT means not less than


Statistics were employed in the
interpretation of data in each section of the
proximate analysis. The summary of the
results of the statistics of each section are
found in the Appedix I: Tables and Figures.
The percent moisture in the three
samples of hog feeds was averaged to be
8.123 (0.063) %. The coefficient of
variance between the samples was
calculated to be only 0.77%. This minimal
magnitude indicates a precise measurement
of moisture in each sample thereby random
errors were minimized throughout the
course of the analysis. When compared with
the given value of percent moisture in the
guaranteed analysis of the product, a
percentage difference of 32.31% was
calculated. Take note that the guaranteed
analysis is just an approximate and better
yet, only is a range of the true value. That is,
the percent moisture from the guaranteed
analysis is given to be not more than 15%.
The result of this analysis gives a value less
than 15% which parallels to the claim of the
guaranteed analysis.
However, the result of this analysis
was highly susceptible to errors. Aside from
random errors, personal and method errors
are prone to be committed in this type of
analysis. The method incorporated in
determining the moisture content of the
samples includes constant weighing.
Weighing itself is vulnerable to personal
errors such as misreading the analogue read
out meter and acquiring extra moisture along
the course of weighing carelessly. One of the
major problems encountered in the analysis
is the constant weighing of the crucible

containing the oven dried sample. A constant


weigh wasnt achieved in the analysis (i.e.
0.0008 difference between the weighing
trials). Due to time constraints, only four
weighing trials were done for each crucible.
Another weighing trial is performed the day
after. There was an increase in weight in the
fifth weigh (see Table 2 on Appendix A)
which means that the overnight storage of
the samples, even inside the desiccator,
resulted to an acquisition of moisture. The
fifth weigh, being the latest of all data, were
used to compute for the moisture content.
This may introduce a systematic error in the
result of the analysis which can be reflected
in the accuracy of the results. Another major
contributor of errors is the method used in
the analysis.
According to a latter study by Mo
and Tjornhom (1978), the method of oven
drying in determining the moisture content
overestimates the moisture in the samples.
During oven drying, other volatile
substances are lost aside from water and side
chemical reactions may occur during the
heating process. Other sources of errors
include the sample preparation in which it
may not be fine enough and therefore affects
the portion side, room humidity, stability of
the oven and the analytical balance, the
desiccant and drying time and temperature
(Thiex and Richardson 2003).
The moisture content of a feedstuff is
important information in livestock industry
because it affects the weight of the feed but
does not provide nutrients to the animal.
Therefore, there is a need to determine the
dry basis of the nutrients in the feed.

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Chem181 Lab Applied Chemistry (03/16/16)

The average percent crude protein


determined in the analysis of hog feeds is
19.9 (1.0) %. The average percent nitrogen
content in the same hog feeds is 3.19 (0.16)
%. The standard deviation of the replicate
samples must range 0.10 for samples with
10% CP to 0.20 for samples with 20% CP
(AOAC, 1990). The magnitude of the
standard deviation exceeds that of the
standard and therefore the precision of the
replicates is poor. The coefficient of
variation of the percent crude protein is
5.12%. This variation indicates random
errors that might have had occurred in the
analysis. The guaranteed analysis of the feed
product claimed a crude protein content of
not less than 16% which parallels to the
result of the analysis. A percentage
difference between the result of the analysis
and the given value in guaranteed analysis
yields 32.67%. Although the results
indicated the precision of the results, the
definite accuracy of the result cannot be
determined since the only theoretical value
given is a range where the true value lie.
Variation in the data is caused by
errors acquired either of method or of
personal means. Systematic errors are
introduced in the analysis when the sample
size was approximated to be only 100 mg
instead of 300 mg. The Kjeldahl method
itself introduced errors in the analysis. In the
sample preparation, it must be first ensured
that the sample was grinded thoroughly to
ensure a homogenous mixture and thus, the
feedstock is well represented in the analysis.
Another flaw in the Kjeldahl method is that
not all nitrogen is accounted in the analysis.
The nitrate and nitrite cannot be determined
in the Kjeldahl analysis. Sample treatment

can be done to counter this limitation.


Usually the nitrate and nitriles are reduced
to ammonia to be collected in the receiving
flask (Olsen, 1929). A blank wasnt
incorporated in the procedure due to time
constraints. This may be another source of
error in the analysis.
In the determination of crude protein,
the percent nitrogen is multiplied by a factor.
This factor is just an approximate of protein
present in nitrogen. Being an approximate, it
is not exactly the real value but a value close
to it. This factor may also be a source of a
systematic error. Although, the Kjeldahl
method of determining the percent crude
protein has its on limitations and it may be
time consuming, it is one of the simplest
methods still employed in the analysis of
hog feeds.
The average of the percentage of
crude fat was calculated to be 11.8 (
6.3)%. The coefficient of variance was
obtained to be 53.45% between the samples.
This value signifies that random errors were
occurrent throughout this part of the
analysis. The guaranteed value was not less
than 4.00% as given by the Vitarich feeds.
The percentage of crude fat value calculated
parallels and fits the guaranteed value.
The values of standard deviation and
of the standard error of the mean present that
the results obtained are not that satisfactory
in terms of precision. The possible errors
that may have caused to the imprecision of
the results are the small sample number of
trials made, the vulnerability of the cotton
plugged in the apparatus that may have
caused leaks, the random errors that may
have occurred during weighing process
throughout
the
experiment,
not
quantitatively transferring the crude fat to
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Chem181 Lab Applied Chemistry (03/16/16)

the vial from the flask used in the rotavapor


extractor and etc. Since the method used is
gravimetry, any interferences in weight like
moisture acquired in humid air can greatly
affect the results.
The average of the percentage of
crude fat was calculated to be 6.85 (
0.86)%. The coefficient of variance was
obtained to be 23.14% between the samples.
This value signifies that random errors were
minimized in course of the analysis. The
guaranteed value was not more than 7.00%
as given by the Vitarich feeds. The
percentage of crude fiber value calculated
parallels and fits the guaranteed value.
The values of standard deviation and
of the standard error of the mean present that
the results obtained are quite satisfactory in
terms of precision. The possible errors that
may have caused to the imprecision of the
results are the small sample number of trials
made, the possible loss of sample while
doing the washings, the random errors that
may have occurred during weighing process
throughout
the
experiment,
not
quantitatively transferring the sample from
one flask to another and etc. Since the
method used is gravimetry, any interferences
in weight can greatly affect the results.
Dry-ashing was used to generally
destroy the organic matrix present in the
sample. The weight loss of the sample
corresponds to the amount of inorganic
compounds present in it. The average
percentage ash/mineral in the dry basis is
18.049 (11.0)%. The large magnitude of
standard deviation corresponds to the
scaattering of results in each. Since the
method used in this section is gravimetric,
errors are indeed expected especially since
the ashed sample wasnt constant weighed.
There is still traces of moisture and
inorganic materials present in the samples.
The sample used in this method wasnt pre-

dried and therefore the ash/mineral content


in the sample is of wet basis. The dry basis
was calculated.
Some minerals might help improve
the constitution and the growth of the swine,
however too much insoluble minerals might
cause problems with the kidney and the
urinary track of the animal resulting to some
infections. Thus affects the health and
decreases the growth of the swine.
The soluble carbohydrates present in
our sample is calculated to be 43.4%. This
represents the values that are said to be
soluble if taken. However, since this is done
involving all analytical experimentation this
calculation would accumulate the greatest
amount of error.
Conclusion
The proximate analysis of the
Vitarich Premium Plus Hog Finisher feed
resulted to a moisture content of 8.123
(0.063) %; a crude protein content of 19.9
(1.0) %; a crude fat content of 11.8 (
6.3)%; a crude fiber content of 6.85 (
0.86)%; an ash/mineral content of 18.049
(11.0)%; and, a nitrogen free extract of
43.4%.
These
obtained
results
were
susceptible to personal, random errors and
also, errors due to the method employed in
each analysis. These errors are reflected in
the large magnitude of standard deviation of
the results. However, the results parallels
with that of the guaranteed analysis of the
Vitarich and thus, the proximate analysis
done in the Vitarich Premium Plus Hog
Finisher feeds is a success.
References

Page 10 of 16

Chem181 Lab Applied Chemistry (03/16/16)

AOAC. 1990. Official Methods of Analysis.


15th edn. Association of Official Analytical
Chemists. Arlington, V A, USA.
Thiex, N. 2009. Evaluation of analytical
methods for the determination of moisture,
crude protein, crude fat, and crude fiber in
distillers dried grains with solubles. J.
AOAC Int. 92:61-73.
Thiex, N. and C. R. Richardson. 2003.
Challenges in measuring moisture content
of feeds. J. Anim. Sci. 81:3255-3266.
Thiex, N. and T. Van Erem. 1999.
Comparisons of Karl Fischer method with
oven methods for determination of water
in forages and animal feeds. J. AOAC Int.
82:799-808
Nennich, T. and Chase, Larry. 2012. Dry
Matter
Determination.
[online]
Articles.extension.org.
Available
at:
http://articles.extension.org/pages/11315/dry
-matter-determination [Accessed 12 Mar.
2016].

Thiex, N. J. and Manson, H. 2002.


Determination of Crude Protein in Animal
Feed, Forage, Grain, and Oilseeds by Using
Block Digestion with a Copper Catalyst and
Steam Distillation into Boric Acid:
Collaborative Study. Journal of AOAC
International. 85: 309-317.
Amin, M. and Flowers, T. H. 2004.
Evaluation of Kjeldahl Digestion Method.
Journal for Research (Science). 15: 159-179.
Van Soest, P.J.; Nutritional Ecology of the
Ruminant
Second
Edition;
Cornell
University Press; Ithaca and London, 1994
pp. 104
Suzanne Nielsen. S. Food Analysis Third
Edition; KLUWAR ACADEMIC/PLENUM
PUBLISHER 2003 pp. 105
Appendices
Appendix I: Tables and Figures (Raw Data)
Moisture
Trial

Jergens, M. H. and Bregendahl K. 1972..


Animal Feeding and Nutrition 10th edn.
Kendall/Hunt Publishing: USA. pp 100-105.
Labonco. n.d. A Guide to Kjeldahl Nitrogen
Determination Methods and Apparatus.
ExpothecUSA: Houstan, Texas.pp 03-10.
Miller, L and Houghton, J. A. 1945. The
Micro-Kjeldahl Determination of the
Nitrogen Content of amino Acids and
Protein. J. Biol. Chem. 159: 373-383.
Williams, P. C. 1974. Errors in protein
testing and their consequences. Cereal Sci.
Today 19:280-282, 286.

Wt. of crucible
in g
22.2382
21.9796
23.5857

1
2
3

Wt. of sample
in g
5.0312
5.0245
5.0131

Table 1.Weight of sample and its corresponding


crucible prior to oven drying
Trial

Weighing
Trial

Wt. of
crucible +
sample in g

Wt. of
Recovered
Sample in g

1
2
3
4
5
1
2
3
4

26.8663
26.8431
26.8384
26.8461
26.8571
26.6075
26.5853
26.5813
26.5833

4.6281
4.6049
4.6002
4.6079
4.6189
4.6279
4.6057
4.6017
4.6037

Page 11 of 16

Chem181 Lab Applied Chemistry (03/16/16)


5
26.5972
4.6176
1
28.2048
4.6191
2
28.1831
4.5974
3
28.1786
4.5929
4
26.1781
4.5924
5
28.1939
4.6082
Table 2. Data for constant weighing of crucible.
3

Trial
1
2
3
Average
Table 3.Percentage Moisture

%Moisture
8.1949
8.0983
8.0768
8.1233

Parameter
Magnitude
Standard Deviation
0.0629
Standard Deviation of
0.0363
the mean
Relative Standard
0.0077
Deviation
Coefficient of Variance
0.7739
Standard Deviation
0.0629
Table 4.Statistical Data For Moisture Content
Crude Protein
Trial
1
2
3
Wt.
Na2CO3 in 53.4000
56.4000
53.7000
g
Final
Volume in 9.31
18.20
26.60
mL
Initial
Volume in 0.00
9.31
18.20
mL
Volume
HCl used 9.31
8.89
8.40
in mL
NHCl
0.1082
0.1197
0.1206
Average
0.1162
NHCl
Table 5.Data for the standardization of HCl
Wt.
of
Trial
digestion
catalyst in g
1
0.1029
2.0129
2
0.1015
2.0020
3
0.1016
2.0120
Table 6.Weight of sample and added digestion
catalyst
Wt. of sample
in g

Initial
Volume in
mL
12.4
14.4

Trial
1
2

Final
Volume in
mL
14.4
16.5

Used
Volume in
mL
2.0
2.1

3
16.5
18.4
1.9
Table 7.Titration of distillate against standard HCl
solution data
%Crude
Protein
1
3.1614
19.7587
2
3.3653
21.0328
3
3.0418
19.0110
Average
3.1895
19.9342
Table 8.Percentage Nitrogen and Crude Protein
Trial

%Nitrogen

Parameter
%N
%CP
Mean
3.1895
19.9342
Standard
0.1636
1.0223
deviation
Standard error
0.0944
0.5572
of the mean
RSD
0.0513
0.0513
CV
5.1282
5.1282
Table 9.Statistical Data for %N and %CP
Crude Fat
Sample/Crucible No.
Weight in grams
1
2.5033
2
2.5066
3
2.5009
Table 10.Weight of Sample on Filter Paper
Sample/Crucible No.
Weight in grams
1
28.7194
2
27.9471
3
29.9761
Table 11. Weight of Sample after Rotavapor
Extraction
Crude Fiber
Sample/Trial
Weight in grams
1
28.4768
2
27.4815
3
29.9166
Table 12.Weight of Filter Paper Used
Ash/Mineral
Trial

Wt. of Empty
Crucible w/o

Wt. of Sample
(g)

Page 12 of 16

Chem181 Lab Applied Chemistry (03/16/16)


cap (g)
1
22.2199
2.0043
2
21.9812
2.0010
3
23.5879
2.0041
Table 13. Wt. of empty crucible and sample prior to
pre-ashing
Trial

Wt. of ash and


Wt. of Ash
crucible (g)
1
22.836
0.6161
2
22.1969
0.2157
3
23.7529
0.165
Table 14. Wt. of empty crucible and sample prior to
pre-ashing

N HCl =

56 . 4000 g
=0. 1197 N
106
8 . 89 mL
2

Trial 3

N HCl =

53. 7000 g
=0 .1206 N
106
8 . 40 mL
2

N=

APPENDIX II : CALCULATIONS

CP= N Conversion Factor

Moisture

%Moisture=
Trial 1

%Moisture=

%Mois ture=
Trial 3

Moisture=

weight original sampleweight dried sample


100
weight originalConversion
sample Factor: 6.25

5.0312 g4.6189 g
100=8.194 9
5.0312 g

Trial 2

5 . 0245 g4 . 6176 g
100=8 . 0983
5 . 0245 g

5. 0131 g4 . 6082 g
100=8 .0768
5 .0131 g

Crude Protein

Weight of Na2 CO 3
N HCl =
106
Vol HCl
2

Sample 1

2 . 0 mL
N=

CP=3 . 1614 6 .25=19 .7587

Sample 2

2 . 1mL
N=

53 . 4000 g
=0 . 1082 N
106
9 . 31 mL
2

1L
0 . 1162 N 14 100
1000 mL
=3. 3653
0 .1015 g

Sample 3

1 . 9 mL
N=

Trial 2

1L
0 .1162 N 14 100
1000 mL
=3 .1619
0 . 1029 g

CP=3 . 3653 6 . 25=21. 0328

Trial 1

N HCl =

Vol HCl Normality HCl 14 100


Weight of Sample

1L
0 .1162 N 14 100
1000 mL
=3 . 0418
0 .1016 g

Page 13 of 16

Chem181 Lab Applied Chemistry (03/16/16)

CP=3 . 0418 6 .25=19 . 9434


s=
Crude fat

Crude Fat =

Weight Fat
x 100
Weight Dry Sample

Weight Fat = Weight of sample after Rotavap


Extraction Weight of vials used

s=

( xmean x)2
N1
2

(7 . 314311 . 7577) +(16 . 201211 . 7577)


21

s=6 . 283987254

For the blank,


Blank = 29.9761 g 29.9166 g = 0.0595 g
For Sample No. 1,

RSD=

s
6 . 283987254
=
=0 .5344571858
mean x
11 . 7577

Weight Fat = 28.7194 g 28.4768 g


= 0.2426 g
0.2426 g blank = 0.2426 0.0595 g = 0.1831 g

% Crude Fat =

0. 1831 g
x 100=7 .3143
2. 5033 g

CV =

s
6 . 283987254
x 100 =
x 100 =53 . 4457
mean x
11 .7577

Standard error of the mean =

s
n

For Sample No. 2,


Weight Fat = 27.9471 g 27.4815 g
= 0.4656 g

Standard error of the mean =

6 . 283987254
=4 . 44345
2

0.4656 g blank = 0.4656 g 0.0595 g = 0.4061 g

% Crude Fat =

0. 4061 g
x 100=16 . 2012
2. 5066 g

Crude Fiber

Crude Fiber =

( weight of ppt + filter paper )weight offilter


weight of the dry defatted sample

Average % Crude Fat =


For Sample No. 1,

7 . 3143 + 16.2 012


=11 .7577
2

Crude Fiber =

( 1 .1331 g )0 .9334 g
x 100
2 . 5033 g

= 7.9775 %
For Sample No. 2,

Page 14 of 16

Chem181 Lab Applied Chemistry (03/16/16)

Crude Fiber =

( 1 .1687 g )1 .0252 g
x 10 0
2 .5066 g

%Ash=(Weight of residue)/(Weight of Dry Sample)x


100
Trial 1:

= 5.7249 %

%Ash=0.6161/2.0043 x 100=30.74%

Average % Crude Fiber =

7.9775 +5.7249
=6.8512
2

Trial 2:
%Ash=0.2157/2.0010x 100=10.78%
Trial 3:
%Ash=0.165/2.0041x 100=8.23%

s=

(xmean x)

Average%Ash=(30.74%+10.78%+8,23%)/3

N1

Average%Ash (wet basis)= 16.5833%

(4.32353.7156)2 +(3.10773.7156)2
s=
21

Dry Basis Calculation:


Crucible 1.
%Ash=(30.74%x(100))/(100-8.1233%)

s=0.8597004246

%Ash=28.2429
Crucible 2
%Ash=(10.78%x(100))/(100-8.1233%)

RSD=

s
0.8597004246
=
=0.231376
mean x
3.7176

%Ash=9.9043
Crucible 3
%Ash=(8.23%x(100))/(100-8.1233%)

CV =

%Ash=7.56%
s
0.8597004246
x 100 =
x 100 =23.1376
mean x
3.7176
Average %Ash=(28.2429+9.9043+7.56)/3

Standard error of the mean =

s
n

Average %Ash=15.2357
Std Dev.
Ashing (Dry Basis)

Standard error of the mean =

0.8597004246
=0.6079
2

(Wet Basis)
=(((x_i-x)^2)/(n-1))
=(((x_i-x)^2)/(n-1))

Ash/Mineral
Dry Basis Calculation:

=12.32615241
=11.32535757

Page 15 of 16

Chem181 Lab Applied Chemistry (03/16/16)


=12.3261
=11.3254
RSD.

=74.34%
=74.33%
%NFE (Dry Basis) = 100 (% Crude Protein + %
Crude Fat + % Crude Fiber + % Ash)

Ashing (Dry Basis)


(Wet Basis)
=s/x x100%
=s/x x100%
= 74.3431
=74.3344

%NFE (Dry Basis) = 100 (18.8179


+14.1331+3.7156+15.2357)
%NFE (Dry Basis) = 100 53.2499
%NFE (Dry Basis) = 48.0977

Page 16 of 16