Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky,1 Linda Lopez,1 Aaron Kettle,1 Prapisala Thepsithar,2 Yi Zhang,2 Zhenpeng Zhang,2 and Rong Yan2 1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
2 Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent Extraction
All trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method
• Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
3Thermo Scientific Poster Note • PN71099_SBFC_2014_E_04/14S
All trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method
• Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
All trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method
• Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
4 Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionAll trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method
• Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
5Thermo Scientific Poster Note • PN71099_SBFC_2014_E_04/14S
All trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method • Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
6 Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent Extraction
All trademarks are the property of Thermo Fisher Scientific and its subsidiaries.
This information is not intended to encourage use of these products in any manners that might infringe the intellectual property rights of others.
Development of Jatropha Oil Extraction From Biodiesel Feedstocks Using Accelerated Solvent ExtractionPeter Bodsky1, Linda Lopez1, Aaron Kettle1
, Prapisala Thepsithar2, Yi Zhang2, Zhenpeng Zhang2, and Rong Yan2
1Thermo Fisher Scientific, Sunnyvale, CA; 2Nanyang Technological University, Singapore, Singapore
The Dionex ASE 150 system gives comparable results to those obtained from the conventional Soxhlet method, in a much faster time and with less solvent usage. In addition, the repeatability of the test results was very good. Moreover, the Dionex ASE 150 system can be effectively used when the sample portion is only 3 g. Figure 2 compares the percentage of oil extracted from 4 g of jatropha seeds using the EN method and 5 g and 3g, respectively, of seeds using the Dionex ASE 150 system method. The highest percentage of oil was extracted from the 3 g sample using the Dionex ASE 150 method; approximately 49.5 ±2.6% weight oil/weight kernel (n =3). Although the standard deviation is slightly higher than that of the results obtained from EN ISO 659:1998 and the Dionex ASE 150 system when using 5g of sample, they are considered as being consistent with those results.
ConclusionThe accelerated solvent extraction method significantly streamlines sample preparation. From this assessment, the Dionex ASE 150 / 350 system permits a very effective method for oil extraction for the determination of the oil content in jatropha seeds. The test results are very consistent with the results obtained from the European Norm. The results obtained from the Dionex ASE 150 / 350 system demonstrate excellent accuracy and precision, and it can be used for the determination of oil content when only a limited amount of sample is available. It should also be emphasized that the oil extraction method using the Dionex ASE 150 / 350 system requires less than one hour to complete, as compared to ten hours consumed by the Soxhlet extraction method, permitting a fully automated extraction process that can be performed in minutes for fast and easy extraction with low solvent consumption.
References1. Raynie, D. Innovations in Sample Preparation; Poster: Presented at Minnesota
Chromatography Forum, Minneapolis, MN, May 7, 2008.2. Ghirlanda, S.; Henderson, S.; Carlson, R.; Richter, B.; and Cavalli, S.; Advances in
Automated Sample Preparation Presentation, GeoSciences 2008. [Online] http://www.dionex.com/en-us/webdocs/67793-LPN_2042-01_ASE_Sample%20Prep_note.pdf (accessed April 7, 2014)
Acknowledgements of Original WorkThepsitha, Prapisala R.; Zhang, Yi; Zhang, Zhenpeng; Yan, Rong; Institute ofEnvironmental Science and Engineering, Nanyang Technological University, InnovationCentre, 18 Nanyang Drive, Singapore 63772
FIGURE 2: Percentages of oil extracted using the European Norm Soxhlet methodand a Dionex ASE 150 system at 80 and 100 °C.
PO71099_E 04/14S
Procedure1. Grind the sample into a particle size specified earlier using a mechanical grinder. 2. Place a cellulose disk at the bottom of the extraction cell (10 mL or 34 mL cells). Fill
the cell with 3 to 5 g of sample. 3. Add Thermo Scientific™ Dionex™ ASE™ prep DE Dispersant (ASE Prep DE) on top
of the sample and leave the head space of the cell around 1/5 of the cell length. Place another cellulose disk on top of the Dionex ASE Prep DE and assemble the extraction cell. Place the extraction cell into the Dionex ASE 150 system.
4. Set the method conditions on the Dionex ASE 150 system and start the extraction.5. Upon the completion of extraction, transfer the extracts to a round bottom flask and
attach the flask to the evaporation apparatus. Weigh the extracted oil and calculate the percentage of oil content using the following equation:
%Oil content = (weight of extracted oil (g) ÷ weight of sample (g)) × 100
Experimental Equipment• Dionex ASE 150 / 350 Accelerated Solvent Extraction system equipped with 10 or
34 mL cells (see Figure 2 for alternative cell sizes).
• Thermo Fisher Scientific vials for extraction collection (60 mL)
• Analytical balance
Solvent• Analytical grade n-hexane (or light petroleum ether especially composed of
hydrocarbons with 6 carbon atoms)
Extraction Method
• Oven temperature: 80 ºC
• Pressure: 10 Mpa (1500 psi)
• Oven heat-up time: 10 min
• Static time: 10 min
• Flush volume: 60%
• Purge time: 60 s
• Solvent: n-hexane
• Static cycles: 3
Comparisons of EN ISO 659:1998 and Dionex ASE 150 System Methods
EN ISO 659:1998 (Soxhlet)
Dionex ASE 150System
Sample Size 10 gground seeds
3-5 g ground seeds
Solvent n-Hexane n-Hexane
Total Volume of Solvent Used
~150 mL ~60 mL
1st Extraction 4 hrs, heat and grind
10 min heat, 10 minstatic time, 1 min
purge2nd Extraction 2 hrs, heat and
grind10 min static time,
1 min purge3rd Extraction 4 hrs 10 min static time,
1 min purgeTotal Extraction Time
10 hrs < 60 min
TABLE 1: Comparison of EN ISO 659:1998 and Dionex ASE 150 System Methods EN ISO 659:1998 (Soxhlet) Dionex ASE 150 system
FIGURE 3: Percentages of oil extracted using the EN Soxhlet method with a 4 gsample size, a Dionex ASE 150 system with a 5 g sample size, and a Dionex ASE 150 system with a 3 g sample size.
FIGURE 1: The Dionex ASE 150 / 350 Accelerated Solvent Extractor Systems.
FIGURE 2: Stainless-steel Dionex ASE 150 / 350 extraction cells, available in cell sizes of 1, 5, 10, 22, 34, 66, and 100 mL.
Sample PreparationThe moisture content of all samples should be less than 10% (w/w). If it is greater than 10%, it should be reduced to less than 10% (w/w) by drying the sample in an oven with a constant temperature not greater than 80 ºC. It is also important that the particle size of all samples should be approximately 2 mm, and not greater than 5 mm. The samples should be ground using a mechanical mill without heating or a change in moisture and oil content. It is essential that the oil extractions are carried out within 30 min of grinding, especially if the free fatty acid content of the extracted oil is to be determined.
Results and DiscussionAccuracy and ReproducibilityThe extraction was carried out on jatropha seeds using both European Norm (EN ISO 659:1998) and Dionex ASE 150 system methods. To compare the performance of the Dionex ASE system relative to that of conventional Soxhlet extraction methods, the weight percent of oil in the seeds was determined using the two methods, and summarized in Table 1.
Figure 1 compares the percentage of oil extracted from the jatropha seeds using conventional Soxhlet and Dionex ASE 150 system methods. The percentage of oil extracted from the jatropha seeds using the EN ISO 659:1998 Soxhlet extraction method was 47.2 ± 0.7% weight oil/weight kernel (n =4) with a total extraction time of 10 h. Two different extractions were performed using the Dionex ASE 150 system, operated at 80 and 100 °C, respectively. The percentage of oil extracted at 80 °C was approximately 48.5 ± 1.3% weight oil/weight kernel (n = 3), and approximately 50.6 ± 0.5% weight oil/ weight kernel (n = 3) when extracted at 100 °C. Total extraction time for each Dionex ASE 150 system method was < 60 min.
IntroductionThe determination of oil content in biodiesel feed stocks can be performed using several methods, including mechanical press, solvent extraction, and nuclear magnetic resonance (NMR). For the feedstock quality control in terms of oil content, it is important that the applied method is universally accepted so as to obtain results that can be compared with those reported from alternate sources. The European Norm (EN) has specified two methods for the determination of oil content in oil seed crops: conventional Soxhlet extraction and NMR imaging. However, these methods have several disadvantages. Both methods are time, labor, and cost intensive, and both require highly skilled labor and a significant amount of sample. These methods are also unfriendly to the environment as Soxhlet extraction requires large volumes of solvent and NMR uses highly toxic solvents.
The Thermo Scientific™ Dionex™ ASE™ 150 Accelerated Solvent Extractor system has great potential to overcome these constraints. Furthermore, it also has a high potential for oil-content testing of third generation biodiesel feed stocks (e.g., micro algae).
In this poster we present the extraction of oil from jatropha seeds in compliance with accuracy and reproducibility requirements described in the EN method. Oil extraction using a Dionex ASE 150 system requires only one to one-and-a-half hours, as compared to nine hours consumed by the Soxhlet extraction. In this research, the effects of the Dionex ASE 150 system conditions on the percentage of oil extracted, the optimum conditions for oilseed extraction, and the minimum amount of oilseeds required per test are also investigated.
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PN71099_E 04/14S
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