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Kerzers, 22. September 2011
Sample Test Report of a B100 according to DIN E 51835-1:2011-01
To whom it may concern
Please find below our sample test report about the oxidation stability testing of a B100 (100% FAME) sample
applying Chemiluminescence in accordance to DIN E 51835-1:2011-01.
We performed the following work:
-
determination of the Oxidation Induction Times (OIT) at different isothermal temperature profiles in
synthetic air
-
data analysis and calculation of the activation energies
Please contact ACL Instruments AG if you have questions about the given test report.
Best regards
Fabian Käser
Managing Director
Direct deposits to ACL Instruments AG:
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Clearing No.: 235 Bank: UBS AG Bern
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110922_ONLINE_SampleReport_DIN E 51835-1_B100
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City: Bern
VAT No.: 703 080
Sample test report No. 1108-1002-a01:
service-No.
sample report
vour reference:
our reference:
Fabian Käser
incoming samples
a) Stability tests according to DIN E 51835-1:2011-01
The oxidation stability of a B100 sample (100% FAME, esterified vegetable oil) was tested with the Chemiluminescence (CL) method according the DIN E 51835-1:2011-01 Norm in synthetic air at different isothermal temperature profiles; we analysed the Oxidation Induction Time OIT as a function of the applied temperature profiles.
b) Notation of the sample
The sample tested is
-
B100, without specification
c) Sample masses and sample preparation/handling
20uL of the sample were pipetted into one-way crucibles, the resulting sample masses were in the
range from 21,17 to 22,84mg.
Then the crucibles were moved in the centre of the CL instrument’s oven compartment. All the experiments were performed without the use of heat conductive additives (e.g. heat conductive paste) to prevent on the one hand the contamination of the oven compartment and on the other hand the crosscontamination with the sample to be tested.
d) Type and size of the crucibles
Saucer-shaped crucibles supplied from ACL Instruments AG were used:
-
glass crucibles: diameter 22mm, borosilicate glass
e) Testing conditions and temperature profiles
The following testing conditions were applied:
method name
OIT
type of method
isothermal, static
duration
variable
temperature profile
iso 70..160°C, ðT = 5K
temperatur tolerance
± 0.02K
heating rate ß*
0K/min
sampling interval
1’000 ms, 3/3
gas atmosphere
N 2 , air each 30 ml/min
Tab. 1: testing conditions
Fig. 1: characteristic temperature profile
page - 2 -
*The samples were ramped from room temperature in 10mins to the required testing temperature in
nitrogen atmosphere (non-oxidative condition). The sample was kept for 3mins at the isothermal testing
temperature in nitrogen before the reaction gas atmosphere was switched to synthetic air (oxidative
condition).
f) Type of the instrument
The instrument used for the tests is a basic instrument configuration manufactured by ACL Instruments
AG, the instruments identification number is 205 (http://www.aclinstruments.com/en/productsbenefits/instruments/basic-configuration/). The characteristics of the instrument are :
-
photon counting mode
-
photon detection limit ~0.5 count/s
-
dynamic of the detection unit: > 6 decades
-
temperature tolerance: ±0.02K
prior to the experimental work, the temperature control of the oven compartment was calibrated to the
use of the above specified glass crucibles.
g) data analysis procedure
The acquired CL intensity (counts/s) were normed to the sample mass (counts/mg/s). The visualisation
and analysis of the OIT event was processed with the software tool Calisto Processing V. 1,084
(http://www.akts.com/tga-dsc-dta-tma-ftir-ms-analysis-software/download-calisto-processingsoftware.html).
h) Amount of experiments and statistical analysis
Each testing condition (time/temperature profile) was performed within this test serie once (n = 1). No
replicate tests were performed.
page - 3 -
Fig. 2: CL data acquired at isothermal temperature profiles ranging 105..150°C, ðT = 5K, in synthetic air.
The data acquired in the range 70..100°C are not depicted. Obviously the B100 sample undergoes a multi-step
oxidation (presence of multiple oxidation reaction Stepps which are at least partially overlaid).
i) Oxidation Induction Time Values
The resulting OIT values are given in the following tab (no. 2):
T (°C)
160
155
150
145
140
135
130
125
120
115
110
105
100
95
90
85
80
75
70
1/T (1/K)
0.00230867
0.00233563
0.00236323
0.00239149
0.00242043
0.00245008
0.00248047
0.00251162
0.00254356
0.00257632
0.00260994
0.00264445
0.00267989
0.00271628
0.00275368
0.00279213
0.00283166
0.00287233
0.00291418
1000/T (1000/K)
2.31
2.34
2.36
2.39
2.42
2.45
2.48
2.51
2.54
2.58
2.61
2.64
2.68
2.72
2.75
2.79
2.83
2.87
2.91
OIT1
0:00:00
0:26:31
0:42:03
1:02:02
2:14:44
4:19:44
7:30:00
10:24:14
25:31:39
OIT 2
0:27:03
0:32:07
0:41:13
0:52:55
1:02:45
1:10:50
1:22:33
1:51:47
2:22:08
3:22:21
4:05:54
6:16:47
8:44:55
12:15:58
18:21:47
26:57:02
35:23:12
54:24:32
78:27:44
Ln[OIT1]
-3.99462
-3.53354
-3.14473
-2.36910
-1.71274
-1.16315
-0.83587
0.06170247
Ln[OIT2]
-3.97471
-3.80302
-3.55356
-3.30368
-3.13324
-3.01207
-2.85899
-2.55584
-2.31563
-1.96240
-1.76747
-1.34073
-1.00916
-0.67121
-0.26771
0.11595
0.38828
0.81847
1.18456
Tab. 2: OIT values (format hh:mm:ss). The OIT1 (minor oxidation step) occurs spontaneously at temperature profiles above 105°C, the OIT2 represents the onset of the major oxidation reaction step.
page - 4 -
j) Incidents, which may influenced the results
No incidents are known/were reported which may influence the results.
k) Modification of the norm DIN E 51835-1:2011-01
-
use of synthetic air in place of pure oxygen (O 2 )
-
gas flow of 30ml/min in place of 50ml/min
-
use of saucer-shaped glass crucibles in place of concave aluminium crucibles
-
no use of heat conductive medium
-
sample volume of 20uL in place of 5uL
l) Date of the tests
The tests were performed in Juli and August 2011.
m) Arrhenius-Analysis and -Diagram
160
155
150
145
140
135
130
125
120
115
110
105
100
95
90
85
80
75
70
1/T (1/K)
0.00230867
0.00233563
0.00236323
0.00239149
0.00242043
0.00245008
0.00248047
0.00251162
0.00254356
0.00257632
0.00260994
0.00264445
0.00267989
0.00271628
0.00275368
0.00279213
0.00283166
0.00287233
0.00291418
1000/T (1000/K)
2.31
2.34
2.36
2.39
2.42
2.45
2.48
2.51
2.54
2.58
2.61
2.64
2.68
2.72
2.75
2.79
2.83
2.87
2.91
OIT1
OIT 2
0:00:00
0:26:31
0:42:03
1:02:02
2:14:44
4:19:44
7:30:00
10:24:14
25:31:39
Ln[OIT1]
0:27:03
0:32:07
0:41:13
0:52:55
1:02:45
1:10:50
1:22:33
1:51:47
2:22:08
3:22:21
4:05:54
6:16:47
8:44:55
12:15:58
18:21:47
26:57:02
35:23:12
54:24:32
78:27:44
-3.99462
-3.53354
-3.14473
-2.36910
-1.71274
-1.16315
-0.83587
0.06170247
Ln[OIT2]
-3.97471
-3.80302
-3.55356
-3.30368
-3.13324
-3.01207
-2.85899
-2.55584
-2.31563
-1.96240
-1.76747
-1.34073
-1.00916
-0.67121
-0.26771
0.11595
0.38828
0.81847
1.18456
2
1
0
Ln[OIT (h)]
T (°C)
-1
-2
-3
(major) OIT 2
(minor) OIT 1
-4
-5
-6
2.30
2.50
2.70
2.90
1'000/T (1'000/K)
Tab. 3: Arrhenius-parameterisation
Fig. 3: Arrhenius-Diagram with linear regression lines
The green linear regression lines represent Arrhenius behaviour conform to the norm.
n) Energy of Activation for the OIT-Events according to Arrhenius
The following tab. (no. 4) gives the energies of activation for the two OIT-events analysed. Please mind
that the given values are only applicable fort he OIT event (not for the whole oxidation reaction progress).
temperature range
linear regression line
coeff. of correlation R 2
Energy of activation (kJ/mol)
(minor) OIT 1
70..160°C
y = 14.898x - 43.451
0.993
122.9
(major) OIT 2
70..160°C
y = 10.12x - 28.237
0.999
84.1
Tab. 4: Activation energy parameters. The correlation coefficients of both OIT events are conform to the
norm DIN E 51835-1:2011-01 and therefore acceptable.
page - 5 -
Remarks
The given test report is a sample report for public dissemination. Nevertheless the content and the results of this document are the sole and exclusive property of ACL Instruments AG.
If you want to present and/or publish and/or disseminate the given sample test report and/or parts of it,
you require the written authorisation from ACL Instruments AG.
Do you have question regarding the given sample test report or do you have questions regarding your
specific samples? ACL Instruments AG provides advice! We are an independent service provider to help
and support you!
Kerzers, 22. September 2011
ACL Instruments
Fabian Käser
Managing Director
page - 6 -