Lampiran 1. Kromatogram Hasil Analisis Komponen Senyawa PFAD dengan alat GC
Lampiran 2. Kromatogram Analisis Fraksi yang Tidak Tersabunkan dengan Pelarut Dietil eter Menggunakan Alat GC.
Lampiran 3. Kromatogram Hasil Analisis Fraksi yang Tidak Tersabunkan dengan Pelarut Petroleum Benzena Menggunakan Alat GC
b. Sampel 2
Lampiran 4. Kromatogram Hasil Analisis Fraksi yang Tidak Tersabunkan dengan Pelarut n-heksana Menggunakan Alat GC.
a. Sampel 1
Lampir g Tidak Ter
T akan Alat H
Lampiran 7. Penentuan Panjang gelombang maksimum Vitamin E dengan alat Spektrofotometer Uv-Vis
panjang gelombang maksimum Vitamin E
Lampiran 8. Adsorbsi Tokoperol dengan Galaktomanan + Tween 20
2 Standard Tokoperol A 3.4280 3.3955 3.4122 3.4119
Lamiran 9. Adsorbsi Tokoperol dengan Galaktomanan tanpa tween 20
Standard Tocoperol 80 %
2 Standard Tokoperol A 3.4280 3.3955 3.4122 3.4119
- 0.15 gr Galaktomanan = .
.
0.12% = 0.1145%
- 0.05 gr Galaktomanan =
.
.
0.12% = 0.1194%
No Sampel Konsentrasi Tocoperol % Adsorbsi
Lampiran 10. Hasil uji stabilitas oksidasi sampel A dengan alat Rancimat
Lampiran 11. Hasil uji stabilitas oksidasi sampel B dengan alat Rancimat
Lampiran 12. Hasil uji stabilitas oksidasi sampel C dengan alat Rancimat
2
TGL : 02-2-2014
Lampirran 14. Has
Den
sil analisis
ngan vitam
galaktoma
min E mengg
anan kolang
gunakan al
g-kaling ya
lat FT-IR
Lampir
Hasil uji S
Hasil uji S vitamin E
aran 1000 k
sil Analisis
ngan alat SE
Perbesaran 1500 kali
Lampiran 16. Prosedur Analisis TG menggunakan Alat Kromatografi Gas (AOCS Ce5-86)
1. Definition
The content of a group of triglycerides having the same carbon number is a quantity
expressed as a percentage relative to the total triglycerides content of the sample, separated according to the present procedure.
2. Principle
Separation of the triglyceride groups having the same carbon number by direct Gas Liquid Chromatography (GLC) of a fat or oil solution under temperature programmed conditions. Identification by reference to a standard triglycerides solution. Content determination by peak areas ratio.
3. Scope
Applicable to vegetable oils, especially for palm oils, palm kernel oils, coconut oils and derivatives.
4. Reagents
4.1. n-Hexane, analytical chromatography grade quality, purity 98% min. 4.2. Gases:
a. Carrier gas - hydrogen, ultra high purity grade, minimum purity 99.95% mol, dried and containing max of 10 mg O2/kg.
b . Make up gas1 - nitrogen, ultra high purity grade.
c. Detector gases - hydrogen, ultra high purity grade, and compress air, ultra high purity,
hydrocarbon free, less than 2 ppm hydrocarbon equivalent to CH4.
5. Apparatus
5.1 Gas Chromatograph with facilities:
a. Column Oven, capable of temperature programming up to at least 360oC. b. Sample Inlet System, capable on capillary split injection using Pneumatic Split/ Splitless (PSS) Injection.
c. Flame Ionization Detector (FID), capable to be maintained at least 25oC above maximum column temperature.
5.2 Capillary column, type Quadrex 007-65HT.
5.3 Autosampler equipped with syringe (maximum 10μL), graduated in 0.1μL. 5.4 Transferpette® (capacity 5 – 50μL).
5.5 Sample vials 2mL.
6. Procedure
6.2 Chr b. Pipette 5 c. Shake th d. Inject fro romatograph Set up the g ll changes in ies of the sa
ression of R a. Determin each peak usin b. Determin correction factors d
Table 1 Pro qua
he samples a 5μl - 7μl2 sa e vials for 1 om those via hic specifica gas chromat n the progra amples bein
Results nation of the
ng the graph ne the corre
determined b
oposed optim antification
To ensure th specify Prod When a spec Gas-liquid ch
plit/splitless Sample vials -hexane (Li
as necessary ample into a 1 minute to
hic edit func ected peak a
by interpola
mum GLC c of specified
he accuracy duct analysi ify time per hromatograp
s injection a s 2 mL (cap
chrosolv gr
y so that it i a vial. Dilut make sure a
chromatog
th the tempe required du .
des group co
ction. areas of each
ation obtain
conditions f d sample pr
of the gas c is.
riod is elaps ph with faci and FID (Fl pacity 5 - 50
rade).
s completel te with 1.5m
all the samp raphy.
erature and ue to the con
omposition
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ed from the
for triglycer roduct.
chromatogra
sed and ever ilities for ca lame Ioniza 0μL) Refere
ly liquefied. ml n-hexane
ple is dissolv
column as d ndition of th
is carried o
triglycerides
e standard tr
rides identif
aphy instrum
ry change c apillary colu he column a
out by ident
s using the
riglycerides
fication and
ment is with
column. umn, PSS
or) Transfer ard) sample
Lampiran 17. Prosedur analisis vitamin E menggunakan alat HPLC (AOCS Ce8-89)
1. Objective
To determine the content of tocopherols and tocotrienols.
2. Scope
Applicable to palm oil phytonutrients / vitamin e sample.
3. Reagents
3.1. Acetic Acid Glassial
3.2. HPLC mobile phase – n-Hexane:Isopropanol:Acetic Acid (1000:5:1, v/v). 3.3. n-Hexane for Liquid Chromatography
3.4. Methanol for Liquid Chromatography
4. Apparatus
4.1. Analytical Balance.
4.2. Interchangeable Hypodermic Syringe 4.3. PTFE Membrane Filter 0.2μm
4.4. Volumetric Flask 100 mL
5. Method’s Parameters
5.1. Weigh accurately the sample and standard sample (Adjust sample weight based on vitamin E
concentration.
See Notes 8.1) into a 100 mL volumetric flask. Add a quantity of n-Hexane (Reagents 4.3),
make up to volume and swirling to dissolve the sample.
5.2. Inject 10 μL of the test solution and standard solution onto the column HPLC by mobile phase : n- Hexane:Isopropanol:Acetic Acid (1000:5:1, v/v ). and identify the tocopherols (and tocotrienols) present by reference to the chromatograms obtained from standards. 5.3. Carry out two determinations (each consisting of duplicate injections of the prepared test. solutions) in rapid succession, using a fresh test portion for each determination.
6. Calculation
7. Expr
ress of resu s the result i
es
ways filterin hase, with 0.
ways test sta
nstant and v ult
in 2 decima
ng every rea .2μm PTFE andard sam
valid.
al points.
agent that w Filter mple minimu
we use as a s
um once a w
solvent or a
week to mak
s a mixture
ke sure the r
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results of ou
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