Determination Total FAME by Agilent

Determination of Total FAME and
Linolenic Acid Methyl Esters in

Biodiesel According to EN-14103
Application Note
Energy and Fuels
Author
Introduction
Coen Duvekot
For biodiesel to be used as a motor fuel or blended with petroleum diesel, it

must conform to standard specifications (ASTM D 6751 or EN-14214). There
are standard GC methods in to determine if biodiesel conforms to the standard
specifications, one of which is EN-14103, used to determine the ester and linoleic
acid methyl ester content. Other methods include EN-14105 / ASTM D 6584 (free
and total glycerine and mono, di, and triglyceride content), and EN-14110 (residual
methanol). Agilent has designed GC solutions for each of these standard methods.
Agilent Technologies, Inc.
EN-14103 is used to verify that the ester content of fatty acid methyl esters
(FAMEs) is greater than 90% (m/m) and that the linolenic acid content is between
1% (m/m) and 15% (m/m) consistent with the EN-14214 specifications.
This method is suitable for FAME that contains methyl esters between C14 and C24.
The ester content (C), expressed as a mass fraction in

percent, is calculated using Equation 1.
Materials and Methods

To prepare the sample, accurately weigh approximately
250 mg of sample in a 10 mL vial, then add 5 mL of methyl
heptadecanoate solution (10 mg/mL) using a pipette.
(SA) AEI
C=
CEI VEI
AEI
Conditions
100 %
m
where:
Column
Agilent Select Biodiesel for FAME,

0.32 mm 30 m, 0.25 m (p/n CP9080)
SA = total peak area from the FAME C14:0 to C24:1
Instrument
Agilent GC
CEI = concentration, in mg/mL, of the methylheptadecanoate solution
Software
Agilent Chromatography Data Station
VEI = volume, in mL, of the methylheptadecanoate solution
Injection volume
1 L
m = mass, in mg, of the sample
Injector
Split/splitless 1177, full EFC control, 250 C,

split 100 mL /min
Equation 1.
Carrier gas
Helium, 12 psi (83 kPa)
Oven
210 C isothermal
Detector
250 C, FID, full EFC control
AEI = peak area of methylheptadecanoate
The linolenic acid methyl ester content (L), expressed as a

mass fraction in percent, is calculated using Equation 2.
AL
Results and Discussion
L=
Figure 1 shows a separation of biodiesel, using the conditions

outlined above.
where:
100 %
(SA) - AEI
SA = total peak area from the FAME C14:0 to C24:1

AEI = peak area of methylheptadecanoate
AL = peak area of linolenic acid methyl ester
Equation 2.
Peak identification
C18:1
C16:0
C16:1
C17:0
C18:0
C18:1
C18:2
C18:3
C20:0
C20:1
C22:0
C22:1
C24:0
C24:1
C18:2
C18:0
C18:3
C17:0
C16:0
C20:1
Palmitic acid
Palmitoleic acid
Heptadecanoic acid (IS)
Stearic acid
Oleic acid
Linoleic acid
Linolenic acid
Arachidic acid
Gadoleic acid
Behenic acid
Erucic acid
Lignoceric acid
Nervonic acid
C20:0
C14:0
C22:0
C22:1
Figure 1.
10
C24 isomers
15
Min
20
Separation of biodiesel by gas chromatography using an Agilent Select Biodiesel for FAME column.
25
30
The results of the biodiesel assay are shown in Table 1.

Table 1.
In the method, the absolute difference between two test

results must be FAME > 1.6% (m/m) and linolenic acid
> 0.1% (m/m). All results obtained are within the limits
specified in the method.
Analysis Results of Biodiesel

Area (V.min)
Quantity(mass %)
FAME content
103139
96.6
Linolenic acid
7599.2
7.1
Conclusion
The data clearly show the applicability of the Agilent GC system
with Select Biodiesel for FAME column for the analysis of biodiesel according to the EN-14103 standard method, with good
repeatability. The biodiesel sample fulfilled the requirements
stated in EN-14214.
The biodiesel sample was in accordance with the requirements stated in EN-14214, that is. FAME content > 96.5 %
(m/m) and linolenic acid content < 12 % (m/m). To verify the
integrity of the system, repeatability was determined. One
sample was analyzed 15 times (Table 2 and Figure 2).
Table 2.
References
1. EN-14103. Fat and oil derivatives Fatty Acid Methyl Esters
(FAME) determination of ester and linolenic acid methyl
ester contents.
Repeatability Results
Parameter
FAME (mass %)
Linolenic acid (mass %)
Average
96.4
7.1
Standard deviation
0.20
0.015
RSD (%)
0.21
0.21
2. EN-14214:2003. Automotive fuels Fatty Acid Methyl

Esters (FAME) for diesel engines requirements and test
methods.
For More Information

These data represent typical results. For more information on
our products and services, visit our Web site at
www.agilent.com/chem.
A relative standard deviation of 0.21 % was achieved.

Figure 2 shows the mass % results of the subsequent injections and the absolute difference obtained, compared to the
specification limits.
10.0
100.0
ASTM window of
repeatability
FAME
mass%
9.0
8.0
95.0
Linolenic
Acid
mass%
7.0
6.0
90.0
1
Figure 2.
7
9
Injection number
11
13
15
Repeatability data obtained during the analysis of biodiesel using

an Agilent Select Biodiesel for FAME column. Red lines indicate
the maximum and minimum variation limits specified in the
method.
www.agilent.com/chem
Agilent shall not be liable for errors contained herein or for incidental or consequential
damages in connection with the furnishing, performance, or use of this material.
Information, descriptions, and specifications in this publication are subject to change
without notice.
Agilent Technologies, Inc., 2011
Printed in the USA
September 6, 2011
5990-8983EN

Determination Total FAME by Agilent

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Determination Total FAME by Agilent

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Determination of Total FAME and

Linolenic Acid Methyl Esters in

For biodiesel to be used as a motor fuel or blended with petroleum diesel, it

Agilent Technologies, Inc.

The ester content (C), expressed as a mass fraction in

Materials and Methods

Agilent Select Biodiesel for FAME,

SA = total peak area from the FAME C14:0 to C24:1

CEI = concentration, in mg/mL, of the methylheptadecanoate solution

Agilent Chromatography Data Station

VEI = volume, in mL, of the methylheptadecanoate solution

m = mass, in mg, of the sample

Split/splitless 1177, full EFC control, 250 C,

Helium, 12 psi (83 kPa)

250 C, FID, full EFC control

AEI = peak area of methylheptadecanoate

The linolenic acid methyl ester content (L), expressed as a

Results and Discussion

Figure 1 shows a separation of biodiesel, using the conditions

SA = total peak area from the FAME C14:0 to C24:1

The results of the biodiesel assay are shown in Table 1.

In the method, the absolute difference between two test

Analysis Results of Biodiesel

Linolenic acid (mass %)

2. EN-14214:2003. Automotive fuels Fatty Acid Methyl

For More Information

A relative standard deviation of 0.21 % was achieved.

Repeatability data obtained during the analysis of biodiesel using

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