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NH
( 4 )s SO 4 +2 NaOH NH 3 + Na2 SO 4 +2 Crude
H 2 O Fat
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.
NFE
Crude Protein
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.
Page 5 of 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
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
Page 7 of 16
Page 8 of 16
Page 10 of 16
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
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
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
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
Moisture
%Moisture=
Trial 1
%Moisture=
%Mois ture=
Trial 3
Moisture=
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=
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
Trial 1
N HCl =
1L
0 .1162 N 14 100
1000 mL
=3 . 0418
0 .1016 g
Page 13 of 16
Crude Fat =
Weight Fat
x 100
Weight Dry Sample
s=
( xmean x)2
N1
2
s=6 . 283987254
RSD=
s
6 . 283987254
=
=0 .5344571858
mean x
11 . 7577
% 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
s
n
6 . 283987254
=4 . 44345
2
% Crude Fat =
0. 4061 g
x 100=16 . 2012
2. 5066 g
Crude Fiber
Crude Fiber =
Crude Fiber =
( 1 .1331 g )0 .9334 g
x 100
2 . 5033 g
= 7.9775 %
For Sample No. 2,
Page 14 of 16
Crude Fiber =
( 1 .1687 g )1 .0252 g
x 10 0
2 .5066 g
= 5.7249 %
%Ash=0.6161/2.0043 x 100=30.74%
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
(4.32353.7156)2 +(3.10773.7156)2
s=
21
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
s
n
Average %Ash=15.2357
Std Dev.
Ashing (Dry Basis)
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
=74.34%
=74.33%
%NFE (Dry Basis) = 100 (% Crude Protein + %
Crude Fat + % Crude Fiber + % Ash)
Page 16 of 16