Chemical characterization of waxes - SurfGz.com Characterization of Waxes.pdf · 3/22 FAMOUS GREEN...
Transcript of Chemical characterization of waxes - SurfGz.com Characterization of Waxes.pdf · 3/22 FAMOUS GREEN...
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1/22
Chemical characterization of waxes
Ref : CR08235002
Date : April 4th, 2011
Introduction :
RESCOLL has carried out a chemical screening of several waxes available on the
market in order to verify the accordance between real composition of the
products and the claims written on the different packages. In a few words, are
the so called “bio” or “green” waxes really bio-based and petrochemical free?
6 different waxes have been studied:
MATUNAS COLD,
RAMSON COOL FORMULA,
TERRAWAX 11-17°C/52-62°F,
FAMOUS GREEN LABEL WARM,
STICKY BUMPS SOY WAX WARM,
GREENFIX COLD.
These samples have all been analyzed following a test protocol developed by
RESCOLL in order to assess the presence of petrochemical based products in the
formulations. According to this protocol, we can identify the major constituents
of the waxes (petrochemical or bio-based). However, ingredients with contents
under 5%in mass are not detected with this test method.
E046E– 18/02/11
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Analysis methodology Waxes are constituted by organic compounds (in the sense of carbon based products,
synthetic or bio-based) and mineral fillers. This last ingredients may interfere in the
characterization, thus extraction of these fillers is mandatory. So, first step of the test protocol
is separation of the mineral fillers from the organic ingredients.
Test method is constituted by several steps:
Extraction of the organic phase with cyclohexane under agitation
overnight at room temperature,
Separation between cyclohexane soluble compounds and other
constituents by centrifugation and filtration
Drying of the cyclohexane solution by solvent evaporation,
Analysis of the dried mix by Fourier Transform Infra-Red spectroscopy
(FTIR), following standard T 51-500 (1989) and Differential Scanning
Calorimetry (DSC) following standard NF EN ISO 11357-3 (1999).
Results : MATUNAS COLD
FTIR spectra and DSC thermogram of this wax are presented in Appendix 1.
The FTIR analysis shows that the analysed portion of the product contains:
mainly signals that are typical of CH2 and aliphatic CH functions,
a band corresponding to the C=O function at 1745 cm-1.
The C=O function band has a very low intensity, which indicates that the sample contains no
or very few fatty acids, constitutive compounds of vegetable waxes and oils.
This analysis underlines that major organic constituents of this wax are from petrochemical
origin, for instance paraffins and mineral oils.
RAMSOM COOL FORMULA
FTIR spectra and DSC thermogram of this wax are presented in Appendix 2.
The FTIR analysis shows that the sample only contains CH2 and aliphatic CH functions.
Bands characteristic to fatty acids are missing on the spectrum.
So, organic constituents of this wax are mainly from petrochemical origin.
TERRAWAX 11-17°C/52-62°F
FTIR spectra and DSC thermogram of this wax are presented in Appendix 3.
Results obtained for this sample are similar to those from RAMSON COOL FORMULA.
Then, organic constituents of TERRAWAX 11-17°C/52-62°F are mainly petrochemicals.
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FAMOUS GREEN LABEL WARM
FTIR spectra and DSC thermogram of this wax are presented in Appendix 4.
The FTIR spectrum of this sample contains the bands presented in the following table.
Wave number (cm-1) Mode
2916 – 2848
1737 – 1708
1463
1366
1192 – 1169
728 - 719
- CH2 aliphatic
-C=O ester / acid
d- CH2 aliphatic
- CH aliphatic
-C-O ester
- (CH2)n aliphatic n>4
This wax has a more complicated formula compared to the previous references.
The spectrum shows all the bands that are characteristic to vegetable waxes like beeswax,
coprah oil and soy butter.
However, DSC does not allow concluding on the absence of paraffin in the formula.
In order to conclude on the paraffin question, we studied the intensity of the FTIR signals. It
appears that paraffin, if present in the sample, should correspond to less than a few % in
mass.
Thus, organic constituents of this wax are mainly from natural origin.
STICKY BUMPS SOY WAX WARM
FTIR spectra and DSC thermogram of this wax are presented in Appendix 5.
The FTIR spectrum of the sample shows bands that are presented in the table below.
Wave number (cm-1) Mode
2916 – 2848
1737
1462
1376
1171 – 1113
729 - 719
- CH2 aliphatic
-C=O ester
- CH2 aliphatic
- CH aliphatic
-C-O ester
- (CH2)n aliphatic n>4
According to this spectrum, this wax contains a vegetable oil like coprah oil.
However, given the intensity of the FTIR bands at 1737 and 729cm-1 and the DSC melting
temperatures, this sample may probably contain a petrochemical based constituent like
paraffin. However, it is difficult to conclude on the presence of this paraffin on the basis of
these analyses.
Thus, organic constituents of this wax are mainly from natural origin.
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GREENFIX COLD
FTIR spectra and DSC thermogram of this wax are presented in Appendix 6
The FTIR spectrum of this sample shows bands that are presented in the following table.
Wave number (cm-1) Mode
2917 – 2852
1730
1497
1461
1377
1235 -1169 – 1104
884 – 822
719
- CH2 aliphatic
-C=O ester
- C=C aromatic
- CH2 aliphatic
- CH aliphatic
-C-O ester
- CH aromatic
- (CH2)n aliphatic n>4
The bands characteristic to aromatic functions seem to indicate the presence of modified
rosin.
The ratio between heights of the peaks at 2917 and 1730 cm-1 indicates the presence of
vegetable waxes (beeswax for instance).
Then, identified constituents of this wax are exclusively from natural origin.
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Conclusions The following table summarizes the results obtained for the 6 tested waxes.
Wax Identified constituents
MATUNAS COLD Mainly waxes and oils from petrochemical
origin
RAMSON COOL FORMULA Mainly waxes and oils from petrochemical
origin
TERRAWAX 11-17°C/52-62°F Mainly waxes and oils from petrochemical
origin
FAMOUS GREEN LABEL WARM Mainly waxes and oils from natural origin
STICKY BUMPS SOY WAX WARM Mainly waxe and oils from natural origin.
Probably very low % of petrochemical waxes
GREENFIX COLD Waxes and oils from natural origin
exclusively
Modified rosin (natural origin)
6/22
Appendix 1: FTIR spectra and DSC thermograms of MATUNAS COLD
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6349.003
Analyst: Admin
Description: RC/08235/MATUNAS ORGANIC COLD
Date Created: fri dec 03 08:54:15 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 03/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2954
2915
2848
1795
1743
1389
872
729
712
661
625
534
496
470
456
1230
1176
1089
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6381.003
Analyst: Admin
Description: RC/08235/Extrait Cyclo MATUNAS ORGANICS COLD
Date Created: tue dec 14 16:23:16 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 14/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2916
2848
1745
1462
1366
1229
729
719
7/22
53.23°C
41.65°C85.17J/g
-1.2
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/MATUNASSize: 9.5400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_MATUNAS.001Operator: BLRun Date: 12-Jan-2011 00:44Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
47.36°C
50.54°C81.26J/g
36.49°C
-0.2
0.0
0.2
0.4
0.6
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/MATUNASSize: 9.5400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_MATUNAS.001Operator: BLRun Date: 12-Jan-2011 00:44Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
8/22
50.93°C
34.17°C84.66J/g
40.78°C
-1.2
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/MATUNASSize: 9.5400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_MATUNAS.001Operator: BLRun Date: 12-Jan-2011 00:44Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
9/22
Appendix 2: FTIR spectra and DSC thermograms DSC of RAMSON COOL FORMULA
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6350.003
Analyst: Admin
Description: RC/08235/RAMSOM COOL
Date Created: fri dec 03 08:57:51 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 03/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2915
2848
1415
1230
874
729
718
627
534
495
469
1794
2949
710
659
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6382.003
Analyst: Admin
Description: RC/08235/Extrait Cyclo RAMSOM COOL
Date Created: tue dec 14 16:14:13 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 14/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2915
2848
1462
1366
1230
729
719
10/22
54.24°C
43.39°C81.87J/g
-1.3
-1.1
-0.9
-0.7
-0.5
-0.3
-0.1
0.1
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/RAMSONSize: 7.9400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_RAMSON.001Operator: BLRun Date: 11-Jan-2011 22:34Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
49.47°C
52.36°C87.09J/g
38.00°C
-0.2
0.0
0.2
0.4
0.6
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/RAMSONSize: 7.9400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_RAMSON.001Operator: BLRun Date: 11-Jan-2011 22:34Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
11/22
52.10°C
34.07°C84.06J/g
-1.2
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/RAMSONSize: 7.9400 mgMethod: ISO 11357
DSCFile: C:...\RC\2008\08235\RC_08235_RAMSON.001Operator: BLRun Date: 11-Jan-2011 22:34Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
12/22
Appendix 3: FTIR spectra and DSC thermograms of TERRAWAX 11-17°C/52-62°F
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6348.003
Analyst: Admin
Description: RC/08235/TERRA WAX 11-17
Date Created: fri dec 03 08:48:45 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 03/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2954
2915
2848
1407
873
729
712 625
534
496
470
663
1794
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6380 .003
Analyst: Admin
Description: RC/08235/Extrait Cyclo TERRA WAX 11-17
Date Created: tue dec 14 16:20:09 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 14/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2953
2915
2848
1462
1366
1230
803
729
719
13/22
52.32°C
45.57°C68.72J/g
41.29°C
-1.2
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/TERRA WAXSize: 7.1800 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_TERRA WAX.001Operator: BLRun Date: 12-Jan-2011 05:04Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
50.82°C
53.93°C61.76J/g
36.74°C
-0.2
0.0
0.2
0.4
0.6
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/TERRA WAXSize: 7.1800 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_TERRA WAX.001Operator: BLRun Date: 12-Jan-2011 05:04Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
14/22
53.42°C
42.10°C57.61J/g
40.53°C
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/TERRA WAXSize: 7.1800 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_TERRA WAX.001Operator: BLRun Date: 12-Jan-2011 05:04Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
15/22
Appendix 4: FTIR Spectra and DSC thermograms of FAMOUS GREEN LABEL WARM
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6468.003
Analyst: Admin
Description: RC/08235/FAMOUS Warm
Date Created: tue jan 25 08:10:49 2011
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 25/01/11
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2916
2849
1795
1736
1407
1195
1174
872
848
730
712
623
531
494
470
960
1115
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6469.003
Analyst: Admin
Description: RC/08235/FAMOUS Warm - extrait Cyclohexane
Date Created: tue jan 25 08:13:37 2011
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 25/01/11
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2916
2848
1737
1463
1366
1169
1113
965
719
1708
1192
728
16/22
60.31°C
38.03°C66.29J/g
48.87°C
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/FAMOUS WARMSize: 9.9700 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_FAMOUS WARM.001Operator: BLRun Date: 25-Jan-2011 07:24Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
53.54°C
58.49°C65.93J/g
25.12°C
48.11°C
-0.1
0.0
0.1
0.2
0.3
0.4
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/FAMOUS WARMSize: 9.9700 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_FAMOUS WARM.001Operator: BLRun Date: 25-Jan-2011 07:24Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
17/22
59.65°C
26.04°C56.60J/g
42.80°C
51.14°C
-0.8
-0.6
-0.4
-0.2
0.0
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/FAMOUS WARMSize: 9.9700 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_FAMOUS WARM.001Operator: BLRun Date: 25-Jan-2011 07:24Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
18/22
Appendix 5: FTIR Spectra and DSC thermograms DSC of STICKY BUMPS SOY WAX
WARM
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6351.003
Analyst: Admin
Description: RC/08235/STICKY BUMPS SOY WAX WARM
Date Created: fri dec 03 09:01:17 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 03/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2916
2848
1737
1413
1195
1172
873
730
718
622
534
493
467
641955
1794
2949
RESCOLL
Golden Gate
Opérateur : BL
Spectrum Pathname: C:\pel_data\spectra\6383.003
Analyst: Admin
Description: RC/08235/Extrait Cyclo STICKY BUMPS SOY WAX WARM
Date Created: tue dec 14 16:16:36 2010
Accumulations: 16
Resolution: 4 cm-1
IR Accessory:
Date: 14/12/10
4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 450.0
0.0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100.0
cm-1
%T
2916
2848
1737
1462
1376
1171
1113
861
729
719
19/22
59.28°C
57.85°C113.6J/g
22.34°C
-2.5
-2.0
-1.5
-1.0
-0.5
0.0
0.5
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/STICKY BUMPSize: 5.3300 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_STICKY BUMP.001Operator: BLRun Date: 12-Jan-2011 02:54Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
54.12°C
57.16°C108.4J/g
0.35°C
47.35°C
-0.2
0.0
0.2
0.4
0.6
0.8
1.0
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/STICKY BUMPSize: 5.3300 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_STICKY BUMP.001Operator: BLRun Date: 12-Jan-2011 02:54Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
20/22
55.74°C
42.96°C101.8J/g
22.34°C
49.12°C
-2.0
-1.5
-1.0
-0.5
0.0
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200
Temperature (°C)
Sample: RC/08235/STICKY BUMPSize: 5.3300 mgMethod: ISO 11357
DSCFile: C:...\08235\RC_08235_STICKY BUMP.001Operator: BLRun Date: 12-Jan-2011 02:54Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
21/22
Appendix 6: FTIR Spectra and DSC thermograms of GREENFIX COLD
62.80°C
54.63°C58.97J/g
3.51°C
45.67°C
-1.0
-0.8
-0.6
-0.4
-0.2
0.0
0.2
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200 250
Temperature (°C)
Sample: RC_08235_GREEN FIXSize: 9.6500 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_GREEN FIX.001Operator: BLRun Date: 14-Mar-2011 18:02Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
22/22
56.55°C
59.01°C55.25J/g
47.15°C
-12.11°C
-0.2
0.0
0.2
0.4
0.6
0.8
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200 250
Temperature (°C)
Sample: RC_08235_GREEN FIXSize: 9.6500 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_GREEN FIX.001Operator: BLRun Date: 14-Mar-2011 18:02Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments
60.10°C
43.88°C55.27J/g
1.75°C
47.44°C
-0.8
-0.6
-0.4
-0.2
0.0
He
at
Flo
w (
W/g
)
-100 -50 0 50 100 150 200 250
Temperature (°C)
Sample: RC_08235_GREEN FIXSize: 9.6500 mgMethod: ISO 11357
DSCFile: C:...\2008\08235\RC_08235_GREEN FIX.001Operator: BLRun Date: 14-Mar-2011 18:02Instrument: DSC Q2000 V24.8 Build 120
Exo Up Universal V4.7A TA Instruments